CSIR-NISTADS- STAPP/Adulteration
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CSIR–National Institute of Science,
Technology and Development Studies
S&T applications to peoples’ problems
(STAPP)
Adulteration Detection and Prevention
Problem Identification with Socio-Economic Impacts
Technology Landscaping
o Technology Outlook
R&D Ecosystem
Strategy and Roadmap
Towards Efficient, Cost-Effective and Solution-centric R&D systems
July 2017
NISTADS Tracks in Policy Research: NISTADS/STAPP/Adulteration/2017-1
P Goswami
Praveen Sharma
May 2017
CSIR-NISTADS- STAPP/Adulteration
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Project Information
Project Team:
Nodal Officer : Dr. P. Goswami
Principal Investigator : Dr. Praveen Sharma
Funding Agency: CSIR
Project Type: Translation Research for Policy Advocacy
Publication Type: Interim Report
Circulation: Limited
Corresponding Author: P Goswami; [email protected]
Acknowledgements:
This Policy Advocacy benefitted from comments from a variety of sources, especially from CSIR
laboratories; notable contributions came from CSIR-CFTRI and CSIR-IGIB. The analyses presented
are based on mostly secondary sources (websites); while we have made sincere efforts to refer to all
these sources, it is possible we have missed some. Finally, the critical comments on our earlier drafts
from several reviewers are gratefully acknowledged.
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s&t applications to peoples’ problems (stapp): an outline
The Prime Minister of India had on several occasions emphasized the need for addressing problems faced
by the people of India through applications of science and technology. This assumes significance as it
calls for a systematic identification, and prioritization, of peoples’ problems that can be potentially solved
through applications of existing S&T solutions, or with appropriate innovation and value addition. Thus the
initiative for design of research and development for Applications of S&T to Peoples’ Problems (STAPP)
was taken up at CSIR-NISTADS.
The conventional discipline-centric R&D can be said to be the cutting edge that drives our progress and
guides our civilization. However, an additional, parallel effort is needed to systematically and effectively
translate the results of scientific inquiry to solutions to peoples’ problems and drive development. STAPP
is aimed at enabling this task through systematic identification of S&T solutions.
The seemingly obvious and simple-looking task of STAPP, however, turns out to be a huge challenge as
one begins to analyse the question in detail. In the first place, STAPP calls for a paradigm shift in our
design of our R&D programmes; it necessitates identification and prioritization of problem to be addressed
through socio-economic impact analysis and technology landscaping as the first step. Further, to keep
pace with the evolution of the problem as well as the S&T solutions, the effort has to be supported by a
sustained R&D effort and technology outlook,
The basic approach, and the departure from the conventional approach lies in STAPP is in its focus on
the solution to an overall problem, rather than only on any specific cause of the problem. For example,
while drought may be a major cause for water scarcity, the focus in STAPP would be on ensuring water
availability and accessibility in a sustainable manner. A major challenge in achieving this is technology
integration in an effective R&D ecosystem,
STAPP needs a carefully identified and comprehensive R&D ecosystem to address a societal problem.
For example, an acute problem faced by the people of India is adulteration in many products: food, milk,
drugs, fuel and so on. It therefore requires a complete R&D ecosystem (and, of course, delivery
mechanism) to address the problem of adulteration; segmental R&D cannot provide a solution to the
people. A first requirement therefore is to examine the components and the connectivity of such an R&D
ecosystem, and then proceed to create it. It is in this sense that the STAPP approach is problem-based,
and not discipline or theme based.
The CSIR-NISTADS effort on S&T Applications for Peoples’ Problems (STAPP) identifies 125 such
peoples’ problems grouped into 25 broad topics where S&T can provide effective solutions, contributing
to rapid and disruptive socio-economic transformation of India. The identification is made objective as far
as possible, using traceable parameters like the number of persons affected, geographical coverage,
socio-economic strata and the severity; however, there is need for more extensive data and deeper
analysis in the process of identification and prioritization.
STAPP also attempts to provide a global technology landscaping and technology outlook for addressing
a problem. The technology landscaping and outlook, while not exhaustive, are expected to provide inputs
for the design of a comprehensive R&D ecosystem leveraging new techniques and tools. Based on the
analysis, a roadmap is suggested for applying science and technology to the identified peoples’ problems
in a cost-effective and implementable manner.
It is expected that the challenges thrown by STAPP will open new and promising areas of innovation.
STAPP is thus meant to supplement and complement, and strengthen our conventional science and
technology research, not replace it.
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S&t applications to peoples’ problems (stapp)
Broad Topics Selected as Peoples’ Problems
The list contains topics initially selected as problems faced by people of India. For each of them, some
S&T solutions are outlined based on available literature; similarly, a first-level technology outlook is
provided for R&D planning.
The purpose of listing the topics is identification and prioritization of people-centric R&D. Naturally, the
list is not exhaustive. Also, the ordering of the topics in the list doesn’t reflect prioritization.
1. Adulteration: Food, Milk, Drugs, Fuel and Material
2. Water: Accessibility, Quality, Sustainability, Equity
3. Breathable Air: Control of pollution, Management of Pollution
4. Energy: Access, Dark and Brown Hours, Affordability
5. A House for Each: Affordability, Liveability, Eco-compatibility
6. Dignified Old Age: Adult Care S&T solutions
7. Healthy Mother, Healthy Baby: Maternity and Birth
8. Nutrition: Balance, Deficiency monitoring
9. Sanitation: Affordability, affluence, Maintenance
10. Lifting of Poverty Line: Minimum Income, Creating Employment
11. Disease and Healthcare: Access, Diagnosis, Affordability, Prevention, Awareness
12. Mental Health: Awareness, Diagnosis, Treatment, Prevention
13. Employment: Skill empowerment, Skill upgradation, Self-employment, Placement
14. Waste-Free Environment: Less-waste products, Degradable waste, waste processing
15. Climate Change: Technology adaptation, Mitigation Technology, Resilience
16. Documentation and Record: Digital records, Accessibility, Operability, Security
17. Social Equity and Inclusiveness: Resource Policy, Employment Planning
18. Rural-Urban Divide: Road Connectivity, e-connectivity, Cultural Connectivity
19. Mass Employment: SME Empowerment, Resource and Material
20. Regional Equity: Local skill, local employment, local resource mapping
21. Sustainable Development: Acceptable Good Practices, Resource Planning, Products
22. Vulnerability to Disasters: Warning, Preparedness, Resilience, Prevention
23. A Secure Society: Social Unrest, Terrorism, Access to Law Enforcement
24. Cyber Safety: Privacy, Fraud, Harassment
25. Digital Literacy: Uniform literacy, access and dissemination
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s&t applications to peoples’ problems (stapp)
Adulteration: Food, Milk, Drugs, Fuel and Material
Summary
Adulteration has emerged as a foremost problem for the Indian people. Adulteration is found in essentially
all sectors, from food to milk to drugs to fuel and material. Major food adulteration and contamination events
occur with alarming regularity and are known to be episodic, with the question being not if but when another
large-scale safety/integrity incident will occur. Indeed, the challenges of maintaining quality in food, drugs and
other sectors are now internationally recognised. Adulteration, therefore, is a major societal problem; science
and technology solutions are needed to address this problem.
Within the philosophy and the scope of solution-centric R&D Design for Application of S&T to Peoples’
Problems (STAPP), the present report documents the nature and the magnitude of the problem of
adulteration and possible S&T interventions. Here adulteration is viewed as a general problem, affecting
food, milk, drugs, fuel and material due to bad practices by suppliers/vendors; detection and at-source
prevention are, therefore, some of the S&T and policy interventions required.
The Report first provides a macro-level socio-economic impact assessment of adulteration in the five
sectors; these assessments are based on secondary data available in the form of reports prepared by
various agencies. Next, the Report provides, in the form of Technology Landscaping, a broad survey of
various technologies available and in practice for adulteration detection. Similarly, new techniques
developed specifically for detection and analysis are always emerging. As some of the standard
assessment techniques become smaller, lighter and cheaper, the boundary between field and laboratory
testing is blurring. The section on Technology Outlook outlines some recent developments.
Navigating the technological landscape is a formidable challenge, especially in low- and middle-income
countries. At the same time, offenders develop new ways of circumventing the detection techniques. There
is thus need for dedicated and sustained R&D efforts in adulteration detection.
In terms of technology development, the cost of development is the main barrier to having robust,
sustainable, easy-to-use, and inexpensive detection technologies available in the field. It is likely that
public funding for development would direct academic interest and attention to this important problem.
In terms of an R&D system for adulteration detection, it is found that there are basically a few core
technologies/methods involved. It would be therefore cost-effective and efficient to develop an Integrated
R&D Eco-system for Adulteration Detection (IREAD). Such a system should have multi-disciplinary
expertise; adulteration detection draws from physics, chemistry, biology, material, computer science, and
a range of engineering disciplines. There is considerable scope for innovative in adulteration detection;
for example, the Minilab, a useful kit, can test only 63 drugs.
A Roadmap is suggested to establish IREAD for sustained developments in adulteration detection by
pooling existing expertise (scientists on deputation) and infrastructure to create a world class facility at
very little additional cost. There are agencies like CSIR where expertise and infrastructure may already
exist in a distributed manner; an outline of CSIR's footprint in prevention/detection of adulteration is
included to indicate feasibility of the proposed strategy.
It is argued that the establishment of an Integrated R&D Ecosystem for Adulteration Detection (IREAD)
would address a major Peoples’ Problem and contribute to a Swasth Bharat.
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Problem Definition: Macro Socio-Economic Analysis
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Food Adulteration
Food adulteration happens to be a major health hazard for people in day-to-day life. Adulteration of food
stuff leads to a number of harmful effects on the digestive system, even cancerous and life threatening in
some cases. Food Safety and Standards Act, 2006 is the consolidation of laws relating to food and to
establish the Food Safety and Standards Authority of India (FSSAI) for laying down science based
standards for articles of food and to regulate their manufacture, storage, distribution, sale and import, to
ensure availability of safe and wholesome food for human consumption and related matters.
Table 1: Broad Socio-Economic Impact of Food Adulteration
Social Strata
Affected
Number of People
Affected
Geographical Coverage Technology Solutions
Affects all
irrespective of
age/economic/ social
status
People of India In 2014-15 survey, food
adulteration found in all
samples from all states/union
territories, except for
Mizoram where testing
facility is not available.
Demarcation of High Risk Zones for
Food Adulteration.
Portable food adulterant testing kits /
Spot testing through Mobile Food
Testing Vans.
Telephonic / Online Complaint
Mechanism through Food Safety
Helpline by FSSAI.
As per FSSAI Report, there has been a surge in cases of food adulterations during 2011-2015 (Table 1). In
2014-2015 report, food adulteration was found in all samples from all states and union territories, except
for Mizoram where testing facility was not available.
Table 2: FSSAI Laboratory Testing Reports on Food Adulteration
Year Samples
Analysed
% adulterated/
Misbranded
No. of Cases Launched
Criminal/ Civil
Penalties in (Rs
lakhs)*
2011-12 64593 12.7 6845 -
2012-13 69949 14.8 5840 525
2013-14 72200 18.7 10235 734
2014-15 74010 19.7 10536 1093
Technological solutions for detection/prevention of food adulteration include periodic Demarcation of High
Risk Zones, Portable food adulterant testing kits / Spot testing through Mobile Food Testing Vans and Telephonic /
Online Complaint Mechanism through Food Safety Helpline by FSSAI.
References
Food Safety and Standards Authority of India - http://www.fssai.gov.in/home#
Central Agmark Laboratory Report - http://agmarknet.nic.in/adulterants.htm
FSSAI data on Food Sample Testing - http://foodsafetyhelpline.com/2015/06/56097/
FSSAI Laboratory Testing Reports on Food Adulteration -
http://old.fssai.gov.in/Portals/0/Pdf/Annual_Labs_Reports_20_07_2016.pdf
Food Testing Manual for various adulterants -
:http://old.fssai.gov.in/Portals/0/Pdf/Final_test_manual_part_I(16-08-2012).pdf
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Milk Adulteration
As a primary source of nutrition for infants, growing children as well as the elderly, adulteration of milk is
particularly dangerous. As per the Economic Survey 2015-16, India ranks first in milk production,
accounting for 18.5% of world production, attaining yearly output of 146.3 million tonnes during 2014-15
as related to 137.69 million tonnes during 2013-14. The per capita availability of milk in India has
increased from 176 grams per day in 1990-91 to 322 grams per day by 2014-15. It is more than the world
average of 294 grams per day during 2013. This represents a sustained growth in availability of milk and
milk products for the growing population Dairying has become an important secondary source of income
for millions of rural households engaged in agriculture.
Milk is subject to adulteration; numerous studies and other evidences have demonstrated milk adulteration in
many countries, notwithstanding the prevailing inspection practises. Moreover, there are very few accounts in
the literature concerning the validation of the classical qualitative methods generally employed to detect milk
fraud and those practises as described in the legislation (Gondim et 2015: Gondim et 2016).
Socio-Economic Impact: Milk adulteration affects many strata of the society in a variety of ways. The
National Survey on Milk Adulteration 2011 (snap shot survey) was conducted by the FSSAI of India to
ascertain the quality of milk and identify different type of adulteration in the liquid milk throughout the
country. The parameters that analysed were Fat (%), SNF (%), Neutralizers, Acidity, Hydrogen Peroxide,
Sugar, Starch, Glucose, Urea, Salt, Detergent, Skimmed milk powder and vegetable fat to ascertain the
presence of adulterant. The deviations were found highest for fat (%) and SNF (%) (solids-non-fat) in 574
(46.8%) samples of the total non–conformity. The second highest parameter of non-conformity was the
Skim Milk Powder (SMP) in 548 samples (44.69%) which
included presence of glucose in 477 samples.
The survey indicated that addition of water to milk is most
common adulterant. Added water not only reduces the
nutritional value of milk but contaminated water may also pose
health risk to the consumers. Also, powdered milk is
reconstituted to meet the demand of milk supply. The study
exposed the occurrence of detergent in some samples which has
health hazards and indicates lack of hygiene and sanitation in the milk handling. In urban parts of the
country, nearly 70% of samples were found to be contaminated, while 31% contamination has been
reported in samples from rural areas. Samples taken from two states - Goa and Puducherry were not
contaminated.
References
The Food Safety and Standards Act, 2006
Milk and Milk Products Regulations, 1992
National Survey on Milk Adulteration –
http://www.indiaenvironmentportal.org.in/content/345963/national-survey-on-adulteration-of-milk-an-
overview/
Hon’ble Supream Court Judgement dated 05th August 2016 –
http://www.indiaenvironmentportal.org.in/files/adulterated%20milk%20Supreme%20Court%20Judgement.
Methods of detecting Milk Adulteration – http://old.fssai.gov.in/Portals/0/Pdf/Adulteration(26.02.14).pdf
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Drug Adulteration
Drug Adulteration is the practice of substituting original drug partially or wholly with other similar looking
substances having inferior chemical or therapeutic properties and rendering it to be injurious to health. In
addition to the adulteration of drugs, the problem of spurious or imitation drugs also exists in India.
Spurious or imitation drug products are drug formulations manufactured concealing the true identity of the
product and made to resemble another drug, especially some popular brand, to deceive the buyer and cash
on the popularity of the original product.
The Drugs and Cosmetics Act, 1940 is the nodal law that regulates the import, manufacture and distribution
of drugs in India. The primary objective of the act is to ensure that the drugs and cosmetics sold in India
are safe, effective and conform to state quality standards. The Drugs and Cosmetics (Amendment) Act,
2008 provides deterrent penalties for offences relating to manufacture of spurious or adulterated drugs.
Socio-Economic Impact: The Ministry of Health and Family Welfare, Government of India, had carried
out a National Survey of the extent of Problems of ‘Spurious and Not of Standard Quality (NSQ) Drugs’
(2014-16). A source wise distribution of samples and survey outcomes are depicted in diagram below. As
such, the percentage of NSQ Drugs in India has been found to be 3.94% and that of spurious drugs 0.0276%.
Drug adulteration is a growing problem for the people of India.
References
The Drugs and Cosmetic Act, 1940
The Drugs and Cosmetic (Amendment) Act, 1940
National Survey of the extent of Problems of ‘Spurious and Not of Standard Quality Drugs’ (2014-16) -
http://pib.nic.in/newsite/PrintRelease.aspx?relid=158639
National Survey of the extent of Problems of ‘Spurious and Not of Standard Quality Drugs’ (2014-16)
Report - http://www.mohfw.gov.in/index1.php?lang=1&level=2&sublinkid=6386&lid=4186
Total Samples Tested - 47012
Spurious -13 NSQ - 1850
Samples from Retail Outlets -
33656
Spurious - 8 NSQ - 1850
Samples from Govt. Outlets -
8369
Spurious - 5 NSQ - 839
Samples from Ports - 4987
Spurious - 0 NSQ - 0
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Fuel Adulteration
Adulteration of the transport fuels at the point of sale and during transportation has become an acute
problem in the country. Transport fuels are often adulterated with other cheaper or by-product or waste
hydrocarbon stream for monetary gains. For example, gasoline (petrol) is believed to be widely adulterated
with naphtha, natural gas liquids, kerosene, waste solvents, by-product petroleum stream, etc. With large
number of adulterants available in the market, both indigenous and imported, the magnitude of the problem
of fuel adulteration has grown into alarming proportions in the past few years. Transport fuels are often
adulterated with cheaper/ by-product/waste hydrocarbon stream. For example, gasoline (petrol) is believed
to be widely adulterated with naphtha, natural gas liquids, kerosene, waste solvents, by-product petroleum
stream, etc. With large number of adulterants available in the market, both indigenous and imported, the
magnitude of the problem has grown to alarming levels in the past few years.
The Motor Spirit and High Speed Diesel (Regulation of Supply, Distribution and Prevention of
Malpractices) Order, 2005 issued by the Central Government under Essential Commodities Act, 1955
provides for punitive action against malpractices such as adulteration. Provisions are also available in the
contractual documents and administrative guidelines to prevent and punish malpractices.
Socio-Economic Impact: According to the Ministry of Petroleum & Natural Gas (Govt. of India), the Oil
Marketing Companies (OMCs) namely, Indian Oil Corporation Limited (IOCL), Bharat Petroleum
Corporation Limited (BPCL) and Hindustan Petroleum Corporation Limited (HPCL) have detected
malpractices including under-measurement and adulteration at their retail outlets in the country during
2011-14. OMCs have terminated 160 retail outlets for such irregularities during the period in proven cases
under Marketing Discipline Guidelines (MDG)/Dealership Agreement. OMC wise details of irregularities
in cases of under-measurement and adulterated samples found at Retail Outlets in all the states are presented
in Table 1. OMC wise details of retail outlets terminated are presented in Table 2.
There are 1.1 crore registered Cars/Jeeps/Taxis owned by 4.7% households and 5.2 crore scooters/ motor
cycle /moped owned by 21% households as of 2011*
Table 2– OMC wise Irregularities and Adulterated Samples
BPCL HPCL IOCL Total Samples
Under
Measurement
Adulterated
samples
Under
Measuremen
t
Adulterated
samples
Under
Measuremen
t
Adulterated
samples
Under
Measuremen
t
Adulterated
samples
586 102 1178 23 1752 70 3516 195
A report by Center for Science and Environment (CSE) has pointed out that availability of wide variety of
low priced fuels and solvents in the market are an immediate enticement to adulteration as depicted in
Figure 1. High taxes on petrol makes it vulnerable to adulteration with cheap solvents and naphtha. Diesel
is easily mixed with subsidized kerosene and cheaper LDO.
References
Numbers of registered vehicles in India - http://censusindia.gov.in/2011-
Common/NSDI/Houses_Household.pdf
Ministry of Petroleum & Natural Gas Report on Adulteration of Petrol/Diesel -
http://pib.nic.in/newsite/PrintRelease.aspx?relid=123774
Control of Fuel Adulteration initiatives - http://cpcb.nic.in/upload/NewItems/NewItem_157_VPC_REPORT.pdf
Statistics for Fuel Adulteration - http://www.downtoearth.org.in/coverage/dirty-fuel-13661
IIP Research work - http://www.iip.res.in/details.php?pgID=sb_61
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Material Adulteration
In India, manufacturers are legally required to give material information about the quality and constituents
of the product they market, and adhere to the laws and standards enforced strictly by public authorities, but
it is generally not followed. Also, the producers suppress the information about the quality, purity, standard
or performance of the product. Manufacturers adulterate their products or use substandard raw materials
for production of the goods for earning more profits and thus violating the consumer rights and other laws.
Socio-Economic Impact: Under the Bureau of Indian Standards Act, 1986, the Bureau ensures
development of the activities of standardisation, marking and quality certification of goods. It has many
standards for the various technical divisions including many products and materials related to various fields
like - Electronics And Information Technology, Electrotechnical, Chemicals, Civil and Mechanical
Engineering, Medical Equipment and Hospitals, Metallurgy and Production etc.
Manufacturers are legally required to give material information about the quality and constituents of the
product they market, and adhere to the laws and standards enforced strictly by public authorities, but it is
generally not followed. Producers quash the information about the quality, purity, standard or performance
of the material. Manufacturers adulterate their products or use substandard raw materials for production of
the goods for earning more profits and thus violating the consumer rights and other laws.
References
BIS Act 2016
http://www.bis.org.in/bs/BIS_Act_2016.pdf
BIS Hallmark for Jewellery
http://www.bis.org.in/cert/hallbiscert.htm
Consumer Handbook, 2015 by Department of Consumer Affairs
http://consumerhelpline.gov.in/Consumer_Handbook.pdf
CBRI Research works
http://cbri.res.in/rd/rd-programs/supra-institutional-network-project/
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Technology Landscaping for
Adulteration Detection
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The ever increasing scale and complexity of food supply networks has made them significantly vulnerable to
adulteration and contamination, and potentially dysfunctional. This has made the task of deciding which
analytical methods are more suitable to collect and analyse (bio) chemical data within complex food supply
chains, at targeted points of vulnerability, much more challenging.
Technology Characterization: Those working within and associated with the food industry strive for user-
friendly methods to detect food fraud and contamination, and fast and high screening methods for the analysis
of food in general (Ellis et al 2015). In addition to being robust and reproducible, these methods need to be
portable and ideally handheld and/or remote sensor devices. They can be then taken to points of vulnerability
along complex food supply networks. A minimum amount of background training is needed to acquire
information rich data speedily (Accum 1820).
Mass spectrometry: Mass spectrometry (MS) is a powerful technology with many advantages and few current
limitations for applications within the food supply chain. It provides abundant structural information and the
precise molecular weight of the compound under investigation. The analytical methods like MS offer high
chemical specificity and sensitivity for example, enabling the accurate identification and quantification of known
analytes within complex food matrices at very minute level concentrations. These methods are considered to be
the gold standard within many industries including the agri-food as well as the pharmaceutical, petrochemical,
and defence industries. However, MS is a sophisticated analytical technique that requires extensive training
and expertise to use.
Some forms of MS can be considered as fingerprinting techniques (Ellis et al 2015) as they involve the direct
introduction of samples into the mass spectrometer without prior chromatographic separation. Some recent
examples of MS fingerprinting techniques include direct infusion/injection mass spectrometry (DIMS) for the
characterization of the foodborne pathogen Campylobacter jejuni (Howlett et al 2004) desorption electrospray
ionisation (DESI) for the analysis of melamine migration into foods from melamine tableware (Mattarozzi et al
2012), matrix-assisted laser desorption (MALDI) MS for detection of hazelnut oil in extra virgin olive oil 1%
level (Calvano et al 2012). They are used for direct analysis in real-time (DART) MS for direct cleansing of
fruit and vegetables for the detection of pesticides (Crawford and Musselman 2012) amongst many others.
Whilst the MS methods are all relatively bulky and hence confined to conventional laboratories, there is
enormous potential for these techniques outside the lab and in the food supply chain. Significant and progressive
steps in portability and miniaturization have been achieved with reductions in size to less than 4 kg by Ouyang
and Cooks (2009).
MS methods are usually coupled with chromatographic techniques. The chromatography column chemistry
needs to be carefully chosen in order to separate out the complex components of food adequately and thus comes
with an additional analytical cost as well as being relatively slow
The development of entirely self-sustained, integrated, and truly handheld MS sensors may hopefully be
equipped in future. Yet this could still be possible with simplified user interfaces, perhaps with the same MS core
but with any number of interchangeable sample cartridges for a number of on-site applications (Zhou et al
2014). Such innovations would have place for the true democratisation of MS methods in becoming universal
techniques able to be routinely used by non-specialists within a wide range of applications outside of laboratories,
such as food supply chains.
Infrared Spectroscopy: Methods for Food chain detection: Molecular vibration and rotation energies in
the infrared regions of the electro-magnetic spectrum may be observed with near-infrared or Raman
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spectrometers. These methods are relatively straightforward to use and moderately expensive, and routine
comparative applications do not require extensive training.
Fourier Transform Infrared (FT-IR) Spectroscopy: Infra-red (IR) spectroscopies include; along with near
infrared (NIR), they provide rapid, high-throughput at/in/on-line screening technology. The potential of FT-IR
spectroscopy for food analysis has been recognised for quite some time. The methods involve measuring the
absorption of an IR beam within a sample, with every sample having its own unique spectral fingerprint (Ellis
and Goodacre 2006). Rodriguez and Allendorf (2011) present in their work, a review of FT-IR for rapid
authentication and detection of food adulteration.
Unlike MS methods, on/at-line NIR instrumentation has been used within the food processing industry for a long
time, mainly for the monitoring and control of product and process quality (Ellis et al 2012; Downey et al 1997).
The range of FT-IR applications are significantly wide-ranging and contain the rapid detection of food spoilage
bacteria at ambient temperatures in meat (Alexandrakis, Downey and Scannell 2012; Ellis, Broadhurst and
Goodacre 2004; Ellis et al 2002; Ellis and Goodacre 2001). Others include the checking of bacterial interactions
in milk (Nicolaou and Goodacre 2011) while others relate to speciation in meat and dairy products (Ellis et al
2005; Nicolaou, Xu and R. Goodacre 2010).
Raman spectroscopy: Raman spectroscopy is another vibrational technique, which has to a large degree been
made portable by many manufacturers (vide infra); it has high potential for use within food supply chains. While
IR spectroscopy measures the absorption of energy, Raman spectroscopy contains the measurement of
the exchange of energy with EM radiation of a specific wavelength, typically provided by a monochromatic
light. The measurement in the shift of the incident laser light (the Raman shift) observed is also known as
the inelastic light scattering effect. IR and Raman spectroscopy are complementary due to the selection rules,
whereby molecules are either IR or Raman active. Molecules are infrared active only if the vibration induced by
infrared light causes a change in the dipole moment; in contrast, Raman spectroscopy detects changes in the
polarizability of molecules. Consequently there exist rules of mutual exclusion - the two approaches can deliver
complementary (bio) chemical information, with bands in Raman typically being much sharper and therefore
more characteristic than in the IR.
In terms of food analysis, Raman spectroscopy offers further distinctive benefits to IR spectroscopy, with
water being a weak Raman scatterer for example, which is always an advantage when the huge bulk of foods or
feed contain water in one form or the other. It is also a confocal method in the sense that it measures precisely at
the point where the laser is focused on a sample, eliminating any out-of-focus signal. This is highly significant
as it means that as long as the material the laser is passing through is transparent to laser light, conventional
Raman spectroscopy can readily analyse samples through glass or plastic bottles/bags and other forms of
transparent packaging, focusing directly on the contents inside including liquids and gather a (bio) chemical
fingerprint quickly; this reduces the need to remove the sample, which becomes significant if the sample is highly
hazardous. Therefore, Raman gives the user some advantages over the infrared methods.
Hyperspectral Imaging: Use of NIR hyperspectral imaging for process control, food safety and quality has
been well recognised. It has been accompanied by the application of chemometrics for data pre-treatment and
analysis (Cheng and Sun 2015; Esquerre et al 2012) and multivariate screening and modelling (Lopez et al
2014). Other applications include test of melamine adulteration of soya bean meal (Haughey et al 2013; Haughey
et al 2015) and non-targeted analysis of adulteration of milk powders (Botros et al 2013).
Micro-Electrical-Mechanical-Systems (MEMS): There are developments in the miniaturization of these
approaches using handheld micro-electrical-mechanical-systems (MEMS) based NIR online in abattoirs. While
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NIR technology is still refining and is very suitable technology within the agri-food sector for rapid, bulk and
high-throughput screening (Zamora et al 2012). Santos et al (2013), FT-IR is more sensitive and possibly more
apt to the detection of low-level compounds within complex food matrices and subtle differences between
samples from analogous backgrounds.
The suitability and utility of portable/handheld FT-IR spectroscopy within the food supply chain has become
increasingly evident. In addition to the relatively stable and restricted laboratory setting, portable and handheld
spectroscopy has already proven effective in the more challenging and lively surroundings of the food supply
chain. A considerable body of work by Saona and co-workers (2011) has shown the utility and efficacy of
portable and handheld FT-IR for a range of food-based applications, including monitoring oxidative stability
(Allendorf, Subramanian and Saona; 2012) as well as measuring trans-fat content in edible oils (Birkel and
Saona, 2011). Thus handheld FT-IR can be a simple and quick substitute to MS for on-site analysis of
acrylamides in potato chips (Ayvaz and Saona, 2015), and in situ discernment and confirmation of
conventionally produced and organic butter (Pujolras et al 2015).
Nuclear Magnetic Resonance (NMR): This spectroscopy method analyzes the interaction of nuclei with
EM radiation in magnetic fields. Like Raman and NIR spectrometry, it is a non-destructive, reliable
technique, applicable to nuclei that have a non-zero spin, such as those in hydrogen and carbon-13 that
yields quantitative data with little sample preparation.
However, NMR instruments are expensive and require stable electrical power supplies, controlled
temperatures, and skilled analysts for their operation. Integrating the area under each absorption peak can
provide detailed information about molecular composition and structure; the area under each peak
corresponds to the number of nuclei (in protons or carbon-13 atoms) contributing to that particular signal.
Many common chemical contaminants produce characteristic absorption peaks (Gottlieb et al 1997).
In NMR analysis, all of the compounds in that contain the nucleus under analysis will contribute to the
spectrum. This can produce ambiguous spectra that may contain overlapping signals, so chemists typically
isolate the components before analyzing them with NMR. However, newer, more sophisticated NMR
technologies may be capable of separating drug components and producing clearer signals. Diffusion-
ordered proton-NMR spectroscopy, for example, can identify the various types of ingredients in a mixture
by taking advantage of differences in molecular mass (Martino et al 2010). The downside to this type of
technique is that it is not quantitative, like normal NMR is, but, by using the two techniques together, a
fuller, clearer molecular picture can be developed. Using these methods, scientists have successfully
differentiated between many authentic and falsified versions of antimalarials, erectile dysfunction drugs,
and antidepressants (Martino et al 2010).
X-ray diffraction and X-ray fluorescence are other techniques that can give substantial information about
drug contents. X-ray diffraction can be used to analyze active ingredients and excipients, while X-ray
fluorescence is used for elemental analyses that can often distinguish real from falsified drugs (Kaur et al.,
2010; Martino et al 2010).
Challenges in Detection of Drug Adulteration: A full evaluation of drug quality requires a range of
qualitative and quantitative testing to verify the identities and amounts of active ingredients, check for
impurities, and ensure acceptable disintegration, dissolution, stability over time, and sterility (USP, 2007).
Identifying falsified and substandard drugs does not always follow the same process as a rigorous quality
evaluation. A few simple tests can identify a product with no active ingredient or one made under gross
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manufacturing negligence. More sophisticated adulterations resist easy detection. Appearance, content, and
therapeutic effect can all be considered in classifying falsified drugs.
Offenders in the business of making falsified drugs can buy crude active ingredients, chemicals that have
not undergone the appropriate purification steps required to meet pharmacopeial standards or
manufacturer's dossier requirements, for example. The drugs made from such chemicals would pass most
tests. Only highly sophisticated and expensive assays could detect trace contaminates.
Detection, Screening, and Analytical Techniques: The main techniques for pharmaceutical analysis are:
visual inspection of product and packaging; tests for physical properties such as disintegration, reflectance
spectroscopy, and refractive index; chemical tests including colorimetry and dissolution; chromatography;
spectroscopic techniques; and mass and Raman spectrometry. Within each of these categories, some
technologies are appropriate for use in the field with minimal training, while others require sophisticated
lab equipment and a high level of technical expertise.
Visual Inspection and Package Technologies: An expert can identify some drug quality problems by
sight. Therefore, visual inspection of a product and its packaging by someone who knows the properties of
the authentic drug or is able to compare the sample to the authentic product is the standard first step in any
drug quality analysis (Martino et al 2010). The Global Pharma Health Fund's Minilab toolkit promotes
visual inspection as the first step to identifying falsified and substandard drugs but admits that this is
challenging even for experts (Jähnke et al 2008; Sherma, 2007).
The printing on a fake Cialis blister pack is less crisp at 32× magnification. SOURCE: Lim, 2012.
Falsified drugs packaging may have missing or misplaced expiry
dates, lack instructions or manufacturing information, not have a
batch number, or differ from the genuine packaging in many other
ways. Sometimes poorly written instructions and spelling errors
expose fake medicines; poor-quality inks may dissolve in water
(Kaur et al 2010). Similarly, the drugs may be the wrong color, size,
or shape, have the wrong markings on them, have a different
coating or texture, or be otherwise different from what is expected (Kaur et al 2010).
Physical and Bulk Property Testing: Active ingredients are the most expensive component of drugs;
dilute or impure active ingredients can translate into vastly increased profits for an unscrupulous
manufacturer. Some tests that rely on pH and other bulk properties can help identify active ingredients.
Bulk properties, also called intensive properties, are properties that do not depend on the amount of the
chemical sampled. Density, solubility, reflectance spectra, refractive indices, and optical rotation are
examples of bulk properties (Brown et al 2011). The malaria drug artesunate, for example, has some
distinctive physical properties: It yields characteristic crystals when precipitated from water, and its extract
acidifies water (Deisingh 2005; Newton et al 2006). These properties can be used to differentiate some
genuine and false antimalarials.
The refractive index, can be used to measure the purity of liquids and is able to detect materials separated
by liquid chromatography. Field inspectors can use handheld refractometers to measure the refractive index
and use it as a quantitative test for some active ingredients (Kaur et al 2010).
Colorimetry and Other Chemical Testing: A variety of simple chemical reactions can test for the
presence of active ingredients. Colorimetry is one such technique. It relies on chemicals that undergo color
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changes when reacted with certain compounds to provide qualitative data about a drug's identity.
Colorimetry protocols exist for the active ingredients in many essential drugs. Green and colleagues
explored the practical use of refractive index to measure the amount of active ingredients selectively
dissolved in certain solvents (Green et al 2007). They found that while the refractive index can measure
the amount of an unknown active ingredient, colorimetry can be used to help confirm its presence (Green
et al 2007). Fast Red TR dye tests for the active ingredient in some antimalarials by turning yellow in the
presence of artesunate (Green et al 2001). In addition to verifying the presence of an active ingredient,
colorimetry can serve as a semi-quantitative technique to provide information about tablet potency; a more
drastic color change or deeper color generally indicates a larger amount of ingredient. More precise
colorimetric testing is possible with a handheld photometer, a spectroscopic device that measures
absorbance of light through a substance (Newton et al 2006). Colorimetry gives limited information and
destroys the sample under investigation, but it is invaluable to field inspectors because it is an inexpensive
technique that requires very little training.
Mass Spectrometry in Detection of Drug Adulteration: Mass spectrometer can identify many active
ingredients and excipients, as well as some impurities (Kaur et al 2010; Martino et al 2010). This technique
successfully detected falsified halofantrine syrup, an antimalarial, in West Africa that instead contained a
sulphonamide antibiotic (Wolff et al 2003). When mass spectrometers were bulky, their worth was hard to
appreciate in poor countries, but newer, portable machines can take this sophisticated technology into the
field (Yang et al 2008). However, mass spectrometers need a steady electrical power source, which may
be problematic to attain in some developing countries.
Other kinds of mass spectrometry are direct ionization, tandem, time-of-flight, secondary ion, and
electrospray ionization [ESI]. They can be used alone and in combination with other analyses to detect
illegitimate drugs (Deisingh, 2005; Martino et al 2010; Wolff et al 2003). Direct ionization MS is a
relatively new class of mass spectrometric analysis that does not require lengthy sample preparation. Other
techniques, such as direct analysis in real time (DART) mass spec and desorption ESI mass spec, can
identify correct and incorrect active ingredients and some excipients. Desorption ESI mass spec in
particular provides information about tablet surface homogeneity and the distribution of active ingredients
and excipients in or on the surface of a tablet (Martino et al., 2010). For example, an artesunate sample
with homogeneous surface distribution of lactose and paracetamol, a fever reducer, is illegitimate; an
authentic, good-quality sample should have homogeneous distribution of artesunate and scattered
distribution of lactose (Martino et al., 2010).
The most sophisticated drug copies may resist identification with any technology other than mass
spectrometry. Among these are very close analogues of genuine active ingredients. These analogues can
be so chemically and structurally similar that they behave the same under nearly any analysis. Mass
spectrometry's ability to precisely measure molecular weight and compare fragmentation patterns can help
distinguish between compounds that differ by only one or two atoms. For example, the erectile dysfunction
drug Cialis is often copied with varying degrees of sophistication (Putze et al 2012; Trefi et al 2008). U.S.
Food and Drug Administration (FDA) forensic chemists have discovered several analogues of the active
ingredient, tadalafil, in so-called herbal remedies (Gamble et al 2008).
IR Spectroscopy- Applications in Drugs adulteration detection: The infrared (IR) range of the EM
spectrum can be divided into three sub regions: the near-infrared (NIR) mid-infrared (MIR), and far-
infrared (FIR). Molecular vibration and rotation energies in the infrared regions of the EM spectrum may
be observed with NIR or Raman spectrometers. These methods are relatively straightforward to use and
moderately expensive, and routine comparative applications do not require extensive training. Chemists
analyze the absorption peaks in these spectra primarily to identify molecular functional groups; most active
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pharmaceutical ingredients and some organic excipients and impurities have characteristic spectral peaks
or spectral fingerprints that can be used to help identify them
Various spectra produced using the techniques elucidate different aspects of drug composition;
characteristic absorption or emission peaks correspond to aspects of chemical composition and molecular
structure. A chemist can extract detailed chemical and structural information from a spectrum, and an
inspector with minimal training can also identify falsified and substandard medicines by comparing the
drug spectra to reference materials in drug spectra databases (Kaur et al 2010). The World Health
Organisation (WHO) maintains a digital form of the International Pharmacopoeia with drug quality
determination protocols for various common medicines (WHO 2011). This guide includes a reference
infrared spectrum for each drug.
Of the three sub regions of the EM radiation, MIR range is more discerning and commonly used region
(Deisingh, 2005). There are several ways to collect infrared spectra, each having advantages and
disadvantages. Attenuated total reflectance and FT-IR is particularly useful for drug quality analyses
because it does not require sample preparation, does not destroy the sample, and provides information about
the distribution of active ingredients and excipients on the surface of tablets (Martino et al 2010). Proper
application of FT-IR can distinguish between some types of real and falsified packaging.
Raman Spectroscopy Raman spectroscopy can readily identify many active ingredients and give further
information about excipients, as well as the relative concentration of active ingredients to excipients
(Deisingh, 2005). These ratios can be key to detecting falsified and substandard drugs, because criminal
manufacturers often take care to use the correct amount of active ingredient but may not be as exacting
about the excipients, which may vary even among genuine manufacturers (Deisingh, 2005; Nyadong et al
2009). For example, artesunate tablets may contain either of the highly similar
sugars lactose or sucrose, depending on the manufacturer (Nyadong et al 2009).
Raman can distinguish between these, and a Raman spectrum of Cialis identifies
both the active ingredient, tadalafil, and the primary excipient, lactose (Lim,
2012). Raman spectroscopy is particularly useful for detecting inorganic
substances in drugs, such as titanium dioxide, a common component of tablet
coatings (Witkowski, 2005).
Data Analytics: Detection technologies provide both qualitative and quantitative
data about drugs. Qualitative methods provide information about a drug's identity,
such as its active ingredient, color, or labeling. Quantitative techniques provide
data on a drug's content and how that content will be absorbed in the body.
Qualitative assays may be used to quickly detect the least sophisticated falsified
drugs, such as those with the wrong or no active ingredient. Quantitative
deficiencies, such as an unacceptable level of impurities or an unacceptably low
or high dosage of active ingredient, are more common among substandard drugs.
Tests for drug quality use both qualitative data (e.g., the identity of ingredients, the presence and nature of
any packaging and inserts, the presence or absence of impurities, and any data referring to the drug's
appearance); quantitative data include the amount of an ingredient present, tablet hardness, the rate and
extent of disintegration and dissolution, and levels of impurities.
A few studies involving portable Raman spectroscopy have included the screening of melamine adulteration in
milk powder (Cheng et al 2010) and infant formula, lactose, whey protein, wheat bran and wheat gluten and
povidone (Mecker et al 2012). Portable Raman devices have been employed to detect organophosphate and
organothiophosphate pesticides phorate and fenthion on apple skins (Li et al 2014), fungicide and parasiticide
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thiabendazole applied on citrus fruits and bananas (Muller et al 2014), vegetable and essential oils (Jentzsch and
Ciobota 2014). There are studies also for detection of marker compounds for illegal alcoholic beverages
(Kwiatkowski et al 2014). In addition few research studies relate to detection and discrimination of pathogenic
bacteria on food crops in the field (Wu et al 2013), detection of offal adulteration in beef (Zhao, Downey and
O'Donnell 2015); and one relates to identification of rapid meat spoilage (Sowoidnich et al 2012).
Chromatography: Chromatography is the most common analytical method used in drug evaluations
(Martino et al 2010). It separates mixtures into their constituent parts based on a variety of chemical and
physical properties. It can be used to separate drug ingredients for further testing and, when used with
appropriate detectors, provides both qualitative and quantitative information about active ingredients and
impurities (Kaale et al 2011). Chromatographic techniques range from basic techniques, such as thin layer
chromatography (TLC) with visual inspection, to more specialized laboratory methods, such as high-
performance liquid chromatography (HPLC) coupled with mass spectrometry.
TLC is a planar chromatographic technique that is ideal for field drug testing (Martino et al., 2010). In TLC
comparisons, authentic samples travel the same distance on a TLC plate and yield main spots of highly
similar shapes, colors, intensities, and sizes as reference standards. The distance the sample travels is
associated with its identity; the intensity of the spot correlates with the amount of the drug present. High
concentrations of impurities may be visible on a TLC plate as well (Kaur et al 2010). In a convenience
sample of tuberculosis drugs in Botswana, TLC indicated 31 percent of the samples tested were substandard
(Kenyon et al 1999). In China, researchers used TLC to distinguish between authentic and falsified versions
of several antibiotics (Hu et al 2005).
TLC is an uncomplicated assay useful in developing countries because it yields “versatile and robust”
results at a low cost (Kaale et al 2011). Compared to other chromatographic techniques, TLC requires
significantly less equipment and expertise. Modern instrumental TLC applications give quantitative
assessments similar to those obtained with other instrumental chromatography procedures.
The main drawbacks to TLC are its limited semi-quantitative data (when used with visual detection) and
the need for accurate technique (Kaale et al 2011). TLC solvents are often toxic or flammable, so these
chemicals may be difficult to transport for field use. Additionally, TLC delivers partial information about
a drug's identity; two samples that travel unlike distances are definitely not the same substance, but two
different substances could appear identical using any chromatography technique if they are chemically
similar enough. Accurately estimating the amount of drug on a TLC plate can be difficult without
experience (Kaale et al 2011).
Advanced chromatography techniques: Chromatographic techniques range from basic techniques, such
as thin layer chromatography (TLC) with visual inspection, to more specialized laboratory methods, such
as high-performance liquid chromatography (HPLC) coupled with mass spectrometry. HPLC is a more
selective technique and, when coupled with sensitive detectors, is generally regarded as the definitive
technique for drug content analysis (Martino et al 2010). Depending on the associated detection technology,
it can be expensive and require skilled operators and expensive, often scarce, solvents. The systems also
require reliable electrical power, which can be an obstacle in developing countries.
An HPLC chromatogram can clearly distinguish between the antimalarial chloroquine, mefloquine, and
quinine. Although the drugs are chemically similar, mefloquine is significantly more expensive, and the
cheaper drugs are sometimes sold labelled as mefloquine (Gaudiano et al 2006). HPLC can identify and
measure active ingredients and many impurities, but may not detect excipients that are not soluble in the
mobile phase.
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Diode array detection is now standard with many HPLC assays and can be used to confirm the presence
of active ingredients. It is a type of UV spectroscopy that is particularly useful because it can operate at
varying wavelengths, allowing it to be fine-tuned for analyses, and can help detect the presence of several
components hidden in a single HPLC peak (Kazakevich and McNair 1996). Another study settled an HPLC
with diode array detection method to detect and quantify eight antidepressants for use in cases of suspected
poisonings (Titier et al 2003). The main advantages of the method were its speed, ease of use, and accuracy.
Gas chromatography, the most powerful chromatographic technology, provides similar information as
the other chromatography systems. However, it may only be used for separation of volatile materials, such
as residual solvents, undeclared ingredients, and any volatile impurities. This technique can only be used
when the compounds of interest are gaseous in the analytical temperature range and do not degrade at or
before the assay's minimum temperature. For example, artemisinin derivatives for treating malaria are too
unstable for gas chromatography (Martino et al 2010).
Unlike TLC, advanced chromatography techniques require considerable investment; the equipment needed
is expensive to buy and maintain (Kaale et al 2011). These tests can only be done in central laboratories,
and countries most affected by falsified and substandard drugs have limited access to such facilities (IOM,
2012). HPLC and gas chromatography are time-consuming, especially considering the time spent preparing
the samples for analysis. The return on the time investment is mixed, as chromatography separates a
minimum number of components present in a sample. A peak assumed to represent one compound may be
hiding several other compounds.
Whilst the Raman effect is an inherently weaker process than IR, and the equipment more expensive, the
materials used to construct Raman devices are slowly becoming inexpensive. Also, the detection responses in
Raman devices are faster as compared to infrared techniques, and indeed the detectors are charge-coupled devices
(CCDs) like those set up in digital cameras and consequently within every smart phone and home.
Milk Adulteration detection: Several techniques have been developed for detection of adulteration in milk.
Once again these techniques are based on colorimetry and spectroscopy. Wu et (2015) use ELISA approach for
the detection of Salmonella spp. in milk samples. Lang, Pang and He (2015) developed a method integrating
two gold nanoparticle (Au NP) based techniques, colorimetric and surface enhanced Raman spectroscopic
(SERS) analyses, for rapid screening and validation of melamine in milk. The colorimetric method utilizes the
color transformation of gold nanoparticle from red to blue or purple on interaction with melamine and was used
for rapid screening. However, the colorimetric method presents false positive and inaccurate quantitative signals
in the presence of interfering compounds. To overcome these limitations the SERS method was employed as a
rapid validation tool. The SERS method can directly utilize Au NPs from the colorimetric method. For the
optimization of combining two methods, three sizes (15, 30, and 50 nm) of Au NPs were evaluated, and the 30
nm Au NPs were determined to be the best size for both colorimetric and SERS methods based on limits of
detection and quantification capability of melamine. By using the developed colorimetric–SERS method, Lang
and colleagues (2015) have been able to rapidly screen and validate melamine in milk, as low as 0.25 ppm, within
20 minutes. Integrating colorimetric and SERS methods exploits the advantages of both methods, and provides
a more rapid, accurate, and cost-effective way for monitoring melamine contamination in large amounts of food
products.
In a study by Gondim et al (2015), a novel validation approach has been applied on classical qualitative methods
related to the detection of the density restoratives starch, chlorides and sucrose in raw milk, considering the
official and modified versions. The study also estimated the rates, unreliability regions, detection limits,
accordance, concordance, selectivity and robustness. In related further work Gondim et al (2017) develop a
MIR-SIMCA strategy to detect the presence of milk adulteration. They use mid-infrared spectroscopy
(MIR) and soft independent modelling of class analogy technique to detect adulterants in milk. Models
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were set with low target levels of adulterations including formaldehyde, hydrogen peroxide, bicarbonate,
carbonate, chloride, citrate, hydroxide, hypochlorite, starch, sucrose and water. In the first step, a one-class
model was developed with unadulterated samples, providing 93.1% sensitivity. Four poorly assigned
adulterants were thrown away for the subsequent step. Afterwards a multi-class model was applied taking
unadulterated and formaldehyde-, hydrogen peroxide-, citrate-, hydroxide- and starch-adulterated samples,
that provided 82% correct groupings, 17% inconclusive classifications along with 1% misclassifications.
The strategy put forward by Gondim and colleagues (2017) might be efficient as a screening tactic as it
would decrease the number of samples subjected to confirmatory analysis, time, costs and errors.
Paper spray (Wang et al 2010; Liu et al 2014) is a recently developed ambient ionization source, and has
demonstrated its promise in direct analysis of complex samples with high quantitation capacity but with
simple procedures for operation. Wang et al (2015) have done a study related to quantitative analysis of
pesticides in milk. They developed a silica coated paper using a facile vacuum filtration method. Different
from the commercially available grade SG81 paper, the developed paper was evenly covered by a layer of
silica particles on the top side of the paper substrate. To study the effects of the preparation parameters on
the performance of the resulting paper, the types and amounts of adhesive agents including soluble starch,
modified corn starch and cassava starch were inspected as well as the concentration of the coated silica
particles. More notably, the as-prepared silica coated paper was successfully employed as a substrate for
paper spray mass spectrometry, and a systematic comparison was carried out between it and the uncoated
filter paper and grade SG81 paper in quantitative analysis of pesticides in milk (Zhang et al 2012). The
results of study done by Wang and colleagues show that using the as-prepared paper, the target analytes in
the complex matrix are more favorably retained at the top side of the paper rather than penetration through
the paper substrate compared to uncoated filter paper and SG81 paper (Wang et al 2015).
Fuel adulteration detection: To check fuel adulteration effectively, it is necessary to monitor the fuel
quality at the distribution point itself. The equipment for this purpose should be handy and the measurement
method should be quick, capable of providing test result within a very short time. It should also be
preferably economic (as a large number of such units would need to be simultaneously deployed) and easy
to use.
There are many methods to detect adulteration in fuel like density measurement method, fibre grating
sensor technology, emission testing, filter paper method (Felix, Udaykiran and Ganesan 2015). Density
measurement method can’t be executed inside automobiles because of many reasons like densities of
adulterated and unadulterated fuels are nearly same and also density can only be measured for a liquid that
is stagnant which is impossible to achieve inside a vehicle due to engine vibrations and other factors. The
sensor grating method uses laser transmitter and receiver which are too costly for just an add-on to an
automobile. The emission testing equipment is too bulky to be fitted inside an automobile. The study by
Felix and colleagues (2015) presents a low cost adulteration detection system that can be installed in an
automobile. In this method, the fuel is heated to a temperature to the boiling point of petrol or kerosene. In
case of diesel fuel, it is heated to a temperature equal to the boiling point of kerosene and in case of petrol
fuel, it is heated to a temperature that of petrol. In this way, one of the constituents gets evaporated and the
other is left in the sample. From this the amount of adulteration in the fuel can be detected. The amount of
the left out sample after heating the adulterated fuel is detected by using two different methods. The first
method uses IR sensors and the second method uses camera based Imaging system for level detection.
Coupling a gas chromatogram to a mass spectrometer is not possible when one is using a flame ionisation
detector which destroys everything passing through it. When the detector is showing a peak, some of what
is passing through the detector at that time can be diverted to a mass spectrometer. There it will give a
fragmentation pattern which can be compared against a computer database of known patterns. That means
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that the identity of a large number of compounds can be detected without the need to identify their retention
times.
The study by Samal (2016) analyses Gasoline by Gas liquid chromatography (GLC) and compares with
the simulated samples of adulterated Gasoline. Recognized quantities of kerosene are mixed with petrol
and 10%, 5% and 2% adulterated petrol sample are arranged. The samples are inserted into GC column
and the chromatograms are obtained. The observation is that the adulteration of Kerosene in Gasoline can
be detected at a minimum level of 2%, without any sample preparation. The method used by Samal (2016)
has been found to be sensitive, specific to kerosene adulteration, rapid and economical for analysis of
adulterated sample of petrol.
A combined density and viscosity measurement is a good way to determine the % adulteration in a sample.
As the aim is to keep the device as handy as possible, the use of a miniaturized sensor becomes imperative.
MEMS-based AT-cut Quartz BAW (Bulk Acoustic Wave) Resonator proves to be the ideal choice for this
purpose. Dwivedi and Dey (2013) discuss the use of a microacoustic sensor, with integrated temperature
control, to be utilized as a combined density and viscosity sensor incorporated in the device for detecting
adulteration.
Roy (1999) developed a simple, intrinsic intensity modulated fibre optic sensor for determining adulteration
of petrol and diesel by kerosene. The sensor is useful due to its simple construction, operation, safety with
inflammable fuels and the possibility of making it compact and portable for on-road measurements. Fibre
grating sensor technology has also been used by Mishra et al (2008) for detection of fuel adulteration.
A method for detection of adulteration of biodiesel by soybean oil using UV-VIS spectrophotometer has
been proposed by (David et al 2014). The observation of adulteration of diesel has been observed by using
kinetic viscosity and opacity value as test parameters (Yadav et al 2005). A field survey of excessive
crankcase dilution of lubricating oil in petrol driven vehicle has done by Ehsan et al (2010). An approach
to automatic fuel adulteration detection and reporting system has been proposed by Felix et al (2015).
Obeidat et al (2014) employ the excitation emission matrices fluorescence spectroscopy and multiway
principal component analysis to classify several petroleum products (gasoline, diesel, and kerosene) and
some organic solvents (hexane, paint thinner). The study considered 60 samples in all including the
petroleum and organic samples. The same protocol was also used successfully for uncovering the
adulteration detection of gasoline with less expensive petroleum or organic substances of different
compositions. The methodology was also used to uncover the adulteration of diesel with kerosene.
Mendes and Barbeira (2013) have shown that the use of distillation curves combined with PCA (Principal
Component Analysis) and PLS-DA (Partial Least Squares Discriminant Analysis) provides a model with
enough sensitivity to discriminate adulterated and unadulterated gasoline samples, as well as, the
determination of the solvent used in adulteration with minimum percentage of 97% accuracy.
It is observed that there are usually, many commonalities among the principles and the methods of detection
of adulteration in fuel and other products.
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Technology Outlook
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Advances in science and technology have opened up many new avenues for adulteration detection. These
methods are not only powerful but are also relatively expensive; forensic chemistry techniques can now
give information on the unique fingerprints manufacturers leave on their products. Such an analysis can
give authorities the evidence necessary to tie falsified drugs to particular sources; however, such sensitivity
is still expensive. Forensic chemistry assays are not practical for routine product quality market surveillance
and may be out of reach entirely in many of the low- and middle-income countries most affected by the
problem (Fernandez et al 2008; Power, 2008). There exists a need of inexpensive and sustainable detection
technologies to be used for routine product quality assessments in all markets.
As offenders become more sophisticated, there will be an increased need for expensive technologies
to detect falsified medicines.
There are several categories of techniques to analyze pharmaceuticals. They include visual inspection
of product and packaging; tests for physical properties such as disintegration, reflectance
spectroscopy, and refractive index; chemical tests including colorimetry and dissolution;
chromatography; spectroscopic techniques; and mass spectrometry.
Novel technologies are constantly being developed to detect falsified and substandard medicines.
Improved colorimetric–SERS method has been used (Lang and others, 2015) to rapidly screen and validate
melamine in milk, as low as 0.25 ppm, within 20 minutes. Integrating colorimetric and SERS methods
exploits the advantages of both methods, and provides a more rapid, accurate, and cost-effective way for
monitoring melamine contamination in large amounts of food products.
It is felt that, along with the many other methods currently in development, mobile handheld (as well as static,
benchtop, fixed at-line) spectroscopy, will play a far greater role within the area of food and feed fraud detection,
and indeed food analysis/screening in general, within increasingly complex and globalized food supply chains.
It is believed that ever expanding portfolio of sensor platforms and technologies and future pervasive, predictive
computation will together take on the role of a technology-based capable guardian for food systems (Hollis-Peel
and Welsh 2014; Cohen and Felson 1979). Able to increase the resilience of food systems, and reduce the areas
of vulnerability within complex food supply chains significantly, as well as the space within which the
opportunities for food crime currently exist. As food fraud has repeatedly been shown to be a problem of systems,
and it therefore requires systems level solutions and thinking (Capra and Luisi 2014), holism, as opposed to one-
eyed reductionism.
Innovative technologies to detect falsified and substandard drugs are constantly emerging. Many of the
most promising examples draw from a range of scientific disciplines. A team of researchers from U.S.
Pharmacopeia and Boston University is developing another new technology called PharmaCheck. It uses
microfluidics, the control of fluids at a sub-millimeter scale, for rapid field drug testing (EurekAlert 2012).
PharmaCheck, which will weigh less than 10 pounds and fit in a shoebox, promises to greatly reduce the
need for confirmatory laboratory testing (Barlow 2012; Gaffney 2012).
Combined NIR/FT-IR methods: Evaluation and direct comparison of both NIR and MIR methods show that
NIR and MIR spectroscopy have their own advantages and limitations. FT-IR is more sensitive to vibrations
from liquid, bound and atmospheric water than NIR, which can be overcome to some extent via the use of very
narrow path lengths or attenuated total reflectance (ATR) (Hashim et al 2010; Koca et al 2010 ). On the contrary
NIR, while not as sensitive to water as FT-IR is able to infiltrate much deeper into the surface of samples.
However, the ability to combine these methods into one component, ideally handheld, can be a very valuable
tool for many applications across the food supply chain.
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Lab-based benchtop combined MIR/NIR spectroscopy permits to select of the most suitable range to choose as
per context, what is fit-for-purpose, allowing for a wider and more varied range of samples to analyse quickly
using a single instrument. It is only a matter of time before such benchtop innovations are significantly reduced
in size and available on/at-line, and handheld combination single package MIR/NIR instruments can be used
within the food supply chain. These would be simple to use, truly democratised analytical technology much
closer to development and commercialisation than handheld MS for use in the food supply chain, with the ability
to switch to reduced wavenumber ranges when and if required and generate highly reproducible and easily
interpretable data.
Spatially Offset Raman spectroscopy (SORS): Another recent and rousing innovation and variant of Raman
spectroscopy is (Matousek et al 2005a). With SORS, Raman spectra are collected from locations within a
sample at depth that are spatially separate from the point at which the sample is illuminated by the laser on the
sample's surface. SORS can be undertaken in seconds, by shining a laser light onto a surface/container and
detecting the Raman signal at the point of excitation and one or more offset positions, the resultant spectra
subtracted using a scaled subtraction, which produce two spectra representing the surface and subsurface of
samples (Matousek et al 2005b). Consequently, SORS enables the user to isolate and retrieve chemically rich
spectral information from distinct layers, substructures, and indeed through other barriers, which would not be
accessible even via conventional Raman spectroscopy, or indeed, any of the other techniques (handheld or
otherwise) mentioned thus far. When commenting from the perspective of its potential use for food product
analysis, the ability of SORS to penetrate through barriers/packaging and retrieve chemically rich information is
especially pertinent and it appears to be a readily transferable technology, and one may even suggest it has the
potential to be a highly disruptive technology.
Food-related SORS applications to date include one to demonstrate the potential utility of subsurface detection
of lycopene and product quality through the pericarp of tomato fruit (Qin, Chao and Kim 2011). There are studies
about the qualitative and quantitative characterization of quality parameters of salmon through the skin (Afseth
et al 2014). It can be said that there is rarity of available food-based SORS studies, nevertheless, the wide range
of applications published thus far in the other areas illustrate the specific and seemingly unique combined
capabilities of this technique. These techniques clearly demonstrate that SORS remains an exciting area, ready
for more exploration, development, and detailed investigation within the region of food authenticity, wider food
analysis in general within supply chains/networks and its use within other forms of logistic networks.
A handheld Raman spectrometer: Few blister packs, capsule materials, and tablet coatings can obstruct
with Raman scattering rendering them problematic to read (Martino et al 2010). If the drug ingredients
yield fluorescence, they interfere with Raman signals, particularly those read with handheld Raman
spectrometers. Though far more widely available and useful for field inspections, these portable devices
have less tolerance for fluorescence than their full-sized equivalents. This is especially problematic in
screening antimalarials, as artesunate is somewhat fluorescent (Martino et al 2010). But some investigators
maintain that the fluorescence of genuine artesunate can serve as a tool to distinguish between good- and
poor-quality samples, as those without sufficient active ingredient will not produce as much fluorescence
(Ricci et al 2008). Ricci and colleagues found that fluorescence interfered more with their readings on the
handheld scanner, but it ultimately produced as reliable results as the Fourier-transformed Raman scanner
(Ricci et al 2008).
It is worth noting that handheld combined FT-IR/Raman spectrometers are already commercially available, in
addition to a wide-range of the other handheld spectroscopy devices.
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A commercially available handheld Raman spectrometer
(CBEx 1064, Snowy Range Instruments, Laramie, USA) and
a range of Raman spectra developed from this scheme
either directly through plastic packaging, commercial glass
and plastic bottles, or from vials. These are from several
sample types commonly associated with food fraud, and
include extra virgin olive oil, honey, red wine, beef, whisky,
and saffron.
NIR and Raman spectroscopy: Recent developments of portable NIR and Raman spectrometers have led
to an increase in the use of these techniques for drug quality analysis (Fernandez et al 2011). These two
methods are non-destructive, quick, and no sample preparation is needed. The radiation can pass through
samples in blister packs (Kaur et al 2010; Martino et al 2010).
NIR is better suited than MIR method to quantitative analysis of drug contents. Computer modelling can
produce limited quantitative characterization from all vibrational spectroscopy, but NIR and UV-visible
spectroscopy yield more reliable quantitative data (Hsu, 1997). NIR can identify active ingredients and is
particularly useful for detecting incorrect concentrations of excipients, a common inconsistency in falsified
and substandard drugs (Deisingh, 2005).
NIR spectra of two different compounds are often only slightly different, and accurately interpreting results
may require significant training (Martino et al., 2010). Portable, battery-powered NIR spectrometers are a
more accessible alternative to traditional spectrometers (Dowell et al 2008). Bate and colleagues compared
the effectiveness of a handheld model to TLC and disintegration tests and found that the handheld
spectrometer detected significantly more poor-quality antimalarial drugs and antibiotics than the other tests
(Bate et al 2009a). The model they used weighed 4 pounds and contained a battery that could operate for
10 hours after a full charge, making it a powerful field tool (Bate et al 2009a).
Combining Techniques: Combining analytical techniques is a challenge both in the field and in the
laboratory. It is difficult to determine which tests can be combined to allow inspectors to use the minimum
number of different techniques. It is usually best to work through tests beginning with the easiest or least
expensive ones and to only move on to the more expensive or difficult tests if the sample passes the earlier
ones. For example, a drug that fails an identity test does not need to be tested for the amount of incorrect
active ingredient. This is the basis of the minimum testing scheme used by the Pharmaceutical Security
Institute (USP, 2007).
The question remains as to how to use analytical methods in parts of the world with limited laboratory
capacity and trained chemists. Reliable reference materials to test samples against are often scarce in poor
countries (Fernandez et al., 2011). Manufacturers are reluctant to release reference standards when they
fear the information could be used to make an illegitimate drug.
Although any one test may suffice to label a drug substandard or falsified, no single analytical technique
provides enough information to confirm that a drug is genuine. Similarly, while colorimetry and TLC are
field techniques for testing for the presence of a particular ingredient, knowing a sample's full content
requires more testing. Spectroscopic techniques are useful for identifying active ingredients but cannot rule
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out the presence of countless possible impurities. Chromatographic techniques may suggest that the drug
contains sufficient active ingredient, but they do not provide any information about how much of that active
ingredient will reach the patient. Time and budget allowing, the best understanding of drug quality comes
from the several complementary experiments.
Even combinations of techniques from within a class, such as spectroscopy, can be helpful. One study
illustrated how, due to differences in the ranges of their spectral regions, infrared spectroscopy may at times
be better at identifying organic substances in tablet coatings, whereas Raman spectroscopy may better
identify the inorganic components (Witkowski, 2005). Experiments that looked at the coating on Cialis
tablets found that Raman spectroscopy did not distinguish between the real coating and falsified coating,
but infrared spectroscopy did (Lim, 2012).
Chemists often pair mass spectroscopy with separation techniques, such as HPLC, to achieve a more
definitive analysis. These hyphenated techniques have broad capabilities. For example, liquid
chromatography-mass spectrometry is a highly reliable separation technique, but does not directly provide
quantitative data about the amount of active ingredient present; analysts must compare results to standards
to determine content (Kaur et al 2010). A type of combined gas chromatography and mass spec (GC-MS)
can provide information missing in HPLC-MS analysis. A study found that automated equilibrium
headspace sampling with capillary gas chromatography provides information about volatile impurities, but
adding mass spec analysis provides extra qualitative information about the identity of any impurities
present (Mulligan et al 1996).
Technologies for field detection of falsified and substandard drugs in developing countries must be
portable, relatively simple to use, sturdy, and inexpensive to buy, use, and maintain. They must also provide
reliable, useful data. Field techniques (including visual inspection, colorimetry, disintegration tests, TLC,
and handheld spectrometry) can detect many falsified and substandard drugs. These techniques are durable,
fast, relatively inexpensive, and fairly easy to use, making them attractive to regulators interested in
monitoring drug quality. Package verification technologies can also aid in field detection of falsified drugs,
although these methods are useful more to the patient at the point of use than to the regulator. The Chinese
drug regulatory authority uses mobile labs for drug surveillance (Jin, 2007).
Although fairly inexpensive TLC and disintegration testing are useful field techniques, according to a
study, they are less reliable than handheld spectrometric devices (Bate et al 2009a). Of 78 samples tested
in one study, 17 passed both TLC and disintegration tests but did not pass either Raman or near-infrared
spectroscopic analysis (Bate et al 2009a). Field tests are no substitute for definitive laboratory techniques
and cannot test all aspects of a product's quality, including its drug content, impurity profile, and dissolution
profile.
Noting the cost of laboratory pharmaceutical testing and the dearth of qualified laboratories in developing
countries, the German Pharma Health Fund (now known as the Global Pharma Health Fund) developed the
Minilab, a portable quality-analysis laboratory (Jähnke et al, 2001; Kaale et al, 2011). During a November
2012 Minilab training session in Angola, trainees tested an illegal shipment of various pharmaceuticals
seized by customs officials along the African coast (Minilab Saves Lives, 2012; World Customs
Organization, 2012). Using the TLC and visual inspection techniques, they identified many drugs with no
or little active ingredient (Minilab Saves Lives, 2012). Merck S.A. in Portugal provided 10 Minilabs to
Angola, which has no drug testing labs (Minilab Saves Lives, 2012). Other similar field kits also exist,
such as the Thermo Scientific FirstDefender and TruDefender field laboratory devices used by the
Singaporean regulatory authority (Lim, 2012).
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In addition to the advantages of portable/handheld spectrometers being taken out into the supply chain,
optics/photonic technologies in general also readily lend themselves to be utilized as fixed/embedded on/at-line
technologies. Therefore, one must not overlook ongoing technological developments within the whole suite of
optical technologies, and the future potential of these within food supply chains, such as the use of vertical-cavity
surface emitting lasers (VCSELs) as minute low-power light sources( Mora et al 2015), UV-Vis (Souto et al
2010), and blue LED ( Ghate et al 2015). With further innovation and future developments in sensor technologies
and computing, such as wired or wireless connectivity (i.e. Wi-Fi, Bluetooth) and/or remote access capability
(Evans et al 2014) built into the portable and handheld devices, these rapid methods could be networked and thus
used to detect trends in the food market and thus could very easily sit within the umbrella of the Internet of Things
(IoT). This, like cloud computing, will not be one but rather a series of paradigms and platforms which are set to
explode and impact on all our lives within the next decade (Atzori and Morabito 2010; Gubbi et al 2013;
Miorandi et al 2012).
Internet of Things (IoT): It is worth mentioning that the first use of the term the ‘Internet of Things’ (by the
British technology pioneer Kevin Ashton) was for its direct application to supply chains (Ashton 2009). IoT is
comprised of networks of interconnected communicating sensor/actuating physical objects (Things) able to
identify each other, and generate, analyse, share and act upon information across common operating platforms
and applications. Currently, at the forefront of IoT sensor technologies are radio frequency identification (RFID)
tags/togs/labels, characterized by unique identifiers which can be passive, semi-passive and active, as small as
an adhesive sticker, and used to monitor objects in real-time (Atzori and Morabito 2010) e.g., to track luggage at
airports. Within food supply chains RFID approaches can be used to monitor product quality in terms of expiry
dates on perishable goods (Dada and Thiesse 2008), determine the probability of goods such as RFID-tagged oils
as being counterfeit using mathematical algorithms (Dada and Magerkurth 2008), establish traceability systems
(Zhang and Chen 2014) enable low cost and ultra-low power food logistics (Zou and Chen ), low-cost chipless short
range ID and temperature/humidity monitoring (Feng et al 2015), and the detection of food freshness and bacterial
growth (Potyrailo et al 2012).
However, as the IoT continues to evolve it will be comprised of many more sensor modalities and innovations
in addition to RFID and become fully formed via a much larger analytical sensor (Ilic, Staake and Fleisch
2009), biosensor (Zhao et al 2015 ; McGrath, Elliott and Fodey 2012 ) and computational toolbox (Chen 2015;
Wu, Weng and Liao 2014). These will include machine-to-machine communicating fixed/embedded as well as
portable/handheld sensor devices with direct human input. These people-centric sensing platforms are able to
acquire rapid, timely, and context specific data associated with predicted or anticipated events, compared to data
from fixed sensor networks alone (Gubbi et al 2013) and particularly so when in the hands of operatives with
experience of supply chains and non-specialists in spectroscopy or science in general. This ability to ensure at
the developmental stage that handheld detection methods can be used by non-specialists is in itself an extremely
important part of the re and development process of these rapid devices. It forms a part of the knowledge
exchange process, is an exercise in mutual learning, and allows the translation of re into practical applications,
with positive impacts on the food supply chains and therefore society as a whole.
In addition, whilst fixed or benchtop spectroscopic devices could be based at major distribution and transport
nodes/hubs within complex food supply networks, the handheld devices can be taken to changing points of
vulnerability to fraud within these increasingly complex and dynamic networks. Points of vulnerability in food
supply networks that, in the future, may well have been automatically identified/predicted and targeted for further
investigation by pervasive and automated computational systems analysis embedded within an IoT network.
Pervasive computing in conjunction with sensor technology platforms offers considerable potential for the
improvement and efficiency of food supply chains/systems (Atzori and Morabito 2010).
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Therefore, the future analytical toolbox will also include a combination of an increasingly innovative sensor
portfolio, with methods able to track, trace and detect within food supply chains. These could include
microfluidic (Escarpa 2012; Martin, Vilela and Escarpa 2012) and nanofluidic devices such as Nanopore
(Schneider and Dekker 2012), active and intelligent packaging (Abreu, Cruz and Losada 2012) and containers
(Haass et al 2015), DNA barcoding (Parvathy et al 2014), edible tags ( Freebody 2010), 3D-printed smart caps
(Wu et al 2015) and novel adaptations to existing technologies, such as turning a handheld personal blood glucose
meter into a melamine detector for milk (Gu et al 2015). In addition to computational tools for data analysis,
simulation and fusion, as well as visualisation and interpretation of food supply chains and systems (Han et al
2015; Pang et al 2015; Shi et al 2014).
Capillary electrophoresis, a separation technique, has recently been demonstrated to be a useful tool in the
process of analyzing suspect pharmaceuticals (Marini et al 2010). Staub and colleagues developed a
capillary electrophoresis system paired with time-of-flight mass spectrometry for analyzing protein-based
drugs, such as insulin, without sample preparation (Staub et al 2010). Researchers at King's College London
and Lund University in Sweden have developed a portable nuclear quadrupole resonance (NQR) device
(Wellcome Trust 2012). Based on technology similar to NMR spectroscopy, NQR uses radiofrequencies
to provide qualitative and quantitative information about medicines and can scan them through packaging
(Wellcome Trust, 2012; Wilkinson, 2012). Unlike most other techniques, NQR can analyze large quantities
of medicine (an entire bottle or package) at one time (Barras et al 2012). Radio wave technologies similar
to those used in bomb detection are also being tailored for pharmaceutical analysis (Sprey, 2010).
Informatics: Expansion of the Raman active ingredient database would make handheld Raman
spectrometers more useful in detecting falsified drugs. All drug detection technologies would be more
powerful if there were a full authentication database with information about drug color, shape, size, weight,
Raman and near-infrared reflectance, and a TLC procedure for assay. Drug companies may balk at releasing
this information, but the committee believes that stringent regulatory agencies should require it. Sharing
all drug authentication information in a drug quality library would vastly improve the power of existing
drug detection technologies.
The Global Pharma Health Fund Minilab is a portable drug
quality analysis toolkit (Kaale et al 2011). The Minilab was
designed to help control the proliferation of substandard and
falsified drugs in countries with weak or absent regulatory
systems (Jähnke et al 2001). The Minilab relies on a
combination of accessible techniques for simple, fast, and
reliable detection of falsified and substandard drugs. The kit
includes equipment and instructions for thin layer
chromatography (TLC), chemical colorimetry, and
disintegration tests, as well as a visual inspection protocol. Testing and inspection protocols and materials
are included for more than 50 World Health Organization essential medicines, including reference
standards for 63 drug compounds (GPHF, 2012a; Kaale et al 2011). By using colorimetry and TLC, the kit
is capable of testing for the top three kinds of substandard and falsified drugs: those that contain no active
ingredient, those that contain too little active ingredient, and those that contain the wrong active ingredient
(GPHF, 2012c; Jähnke et al., 2001). Since the reliability of TLC is based in large part on the tester's level
of training, the Minilab attempts to simplify the analysis by providing reference tablets that can be used to
prepare 100 percent and 80 percent dosage strengths for comparison (Kaale et al., 2011).
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Genuine (left) and falsified (right) holograms on
artesunate blister packs found in Southeast Asia.
Source: Newton et al 2008.
Detection in Every Setting: There is a wide range of technology available to detect falsified and
substandard drugs; a good prevention strategy makes use of a wide variety of them. Some technologies,
such as scratch-off codes, can be used by the consumer. There are also package technologies manufacturers
may use to distinguish their products at the point of purchase. Making detection technology more accessible
in low- and middle-income countries is invaluable to controlling the trade in falsified and substandard
drugs. Technologies can protect consumers and also help generate accurate estimates of the magnitude of
the problem. An understanding of the technological landscape, the range and gaps in available technologies,
and the likely improvements in the near future is necessary for using technologies in developing countries.
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R&D Ecosystem – Adulteration Detection
Narration of an R&D Ecosystem: The ecosystem for adulteration detection would involve various
components like infrastructure, equipment, experts, technicians and support staff for end-to-end and
product driven R&D on adulteration; industry and academia will be important external components.
Need for R&D Ecosystem: Given the wide variety of techniques and tools for adulteration detection, the
need for a sustained and dedicated R&D for adulteration may be questioned.
Understanding when, where, and why to use the various techniques can be difficult. The
information a technique provides, as well as its reliability, cost, required expertise, speed, and
portability make it more or less appropriate in any given situation.
There is no single analytical technique that provides enough information to confirm that a drug is
genuine, but combining techniques gives more precision.
It is often difficult to test for drug quality in low- and middle-income countries. Poor training
chemists and infrastructure are common obstacles in performing accurate drug quality testing.
Making detection technologies easily accessible in low- and middle-income countries will help
curtail the trade in falsified and substandard medicines.
Field technologies and techniques are useful for detecting most falsified and substandard drugs.
They should be easy to use and maintain, cheap, and durable.
It is clear that the spectrum of technologies and tools in adulteration detection in various sectors is relatively
small and require similar expertise/infrastructure. Essentially all the detection technologies are based on
mass spectroscopy or variants of IR or Raman spectroscopy. The other types of technologies and methods
involve chromatography and chemical analyses. However, adulteration detection is now also increasingly
dependent on sensors and emerging tools like Internet of Things and data analytics. Thus only a complete
and sustained R&D ecosystem will be able to address the problems of adulteration detection in a
comprehensive manner.
Given the financial stakes involved, the battle against adulteration is going to be an everlasting one. As the
offenders create new ways to circumvent the detection methods, there will be need for constant upgradation
of the detection methods. The goal has to make the detection process integrated to the supply chain in a
way that adulteration becomes financially and operationally unacceptable to the offenders. Technology,
along with an aware and vigilant population can achieve this.
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Adulteration Detection: Strategy and Roadmap
The Technology Landscaping and R&D Ecosystem for adulteration detection show that the detection
system depends on a few core technologies and their variants. Based on the foregoing analyses, it is
proposed that an Integrated R&D Ecosystem for Adulteration Detection (IREAD) should be established to
address the following problems
Offenders continue to develop new and more sophisticated techniques to circumvent detection; thus
there is need for continued R&D in adulteration detection
Currently, India’s adulteration detection research and development is distributed in various
institutions/university departments; these isolated efforts do not add up to complete solutions.
The costs associated with developing new detection technologies are a barrier to having robust,
sustainable, easy-to-use, and inexpensive technologies available in the field.
Therefore establishment of an Integrated R&D Ecosystem for Adulteration Detection (IREAD) would
address a major Peoples’ Problem.
IREAD Vision: To create an adulteration free India through comprehensive applications of R&D.
The primary mandate of IREAD would be the development of an effective R&D system for new
innovative detection, sampling, and analytical technologies, ranging from field and rapid screening
technology to sophisticated laboratory-based assessments.
Major Objectives of IREAD:
1. Provide complete solutions for adulteration detection and prevention from lab to field
2. Industrialisation/ Commercialisation/ Adulteration detection and prevention technologies
3. Create a comprehensive R&D Ecosystem in a cost-effective manner
4. To develop/translate/adopt new and emerging methods and technologies in adulteration detection
5. Identify organisation with existing/similar mandate/facilities/business---- augment/upgrade
Such a system will be cost-effective as it will avoid unnecessary duplication of infrastructure/equipment.
Feasibility and Implementation:
(a) There are many commonalities in the requirements of equipment/expertise for detection of adulteration
in various sectors; an integrated IREAD facility is practically implementable
(b) There are many institutions and agencies, including CSIR (Appendix A) with expertise in adulteration
detection; thus ready expertise and skill are available
(c) Agencies that already have basic expertise and infrastructures can be engaged to integrate, enhance and
catalyse adulteration detection techniques
(d) Task Teams can be formed by pooling expertise through scientists in deputation, making IREAD
financially feasible.
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Appendix A
CSIR Laboratories involved in Adulteration and Quality Control Research
Central Food Technological Research Institute (CFTRI), Mysore, Karnataka
CSIR-CFTRI has played a vital role in improving the quality of food and monitoring its safety in the
country. The lab stands out as a leading laboratory involved in all facets of scientific investigation related
to food analysis serving small, medium and large food industries, regulatory/academic organizations and
society at large. The institute leads the way in implementation of food standards in the country. Responding
to Hon’ble Supreme court of India’s request, the testing of safety parameters for 16 samples of instant
noodles was undertaken at CFTRI and scientifically backed opinion were given on the test results.
Scientific investigations carried out at the Institute thus facilitate decision making for both the industry as
well as the regulatory agencies.
CSIR-CFTRI is involved in research activities on various aspects of food quality and safety. The Institute
is committed to providing high quality analytical services and guidance to food industries and government
agencies with its sound scientific knowledge-base supported by state-of-the-art instrumentation. It offers a
wide range of science-based food analytical services to the food industries through the Customer Service
Cell for compliance under the provision of FSSA 2006, Bureau of Indian Standard (BIS), AGMARK, and
other national and international standards. The Institute is also NABL accredited for testing and analysis
of more than 250 chemical and biological samples.
Samples analysed at Referral Food Laboratory, CFTRI
S.No. Period
No. of samples analysed
Court FSSAI Port/ Customs Total
samples NC* samples
NC* samples
NC* samples
NC*
1. 2011-12 1130 601
(68%)
325 155
(52%)
498 50
(10%)
2052 806 (39%)
2. 2012-13 381 197
(69%)
312 179
(63%)
454 117
(26%)
1248 493
(40%)
3. 2013-14 161 94
(73%)
468 231
(53%)
391 55
(14%)
1109 380
(34%)
4. 2014-15 72 26
(58%)
324 162
(50%)
474 53
(11%)
890 241 (27%)
5. 2015-16 53
28
(64%)
380 165
(44%)
362 36
(10%)
870 229 (26%)
6. 2016-17 39 24
(80%)
615 300
(60%)
189 39
(21%)
843 363
(43%)
NC*: Non conforming to standards and includes substandard, misbranded and unsafe as defined under the FSSA 2006 &
Regulations 2011.
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Dairy Products
No. Year Number of
Samples
Non Conforming
1. 2011-2012 682 373(54.6%)
2. 2012-2013 255 132(51.8%)
3. 2013-2014 190 96(50%)
4. 2014-2015 120 62(51%)
5. 2015-2016 102 65(63.8%)
(*Includes Cow Milk, Buffalo Milk, Mixed Milk, Pasteurised Milk, Butter, Cheese, Curd, Ghee, Khoya, Paneer, Milk Powder,
Srikhand, Yoghurt etc.
The Institute also conducts societal outreach and public/consumer awareness programs on Food
adulteration and demonstration of simple detection methods; Health hazards of food contaminants
(Chemical and microbiological); Food laws of the country for the consumer and food establishments; Team
CSIR-CFTRI has developed an adulteration test kit to determine adulterant in commodities like milk, oil,
sweets, dhal, chilly /turmeric powder and fried items like chips and savouries.
Central Electronics and Engineering Research Institute (CEERI), Pilani, Rajasthan has developed
handheld GPS-enabled version of the recently launched Ksheer Scanner Technology to check adulteration
in milk. The device would enable to track the location of the tested sample and receive the test results
through SMS on the device.
Central Scientific Instruments Organization (CSIO), Chandigarh: The lab has wide ranging expertise
in developing sophisticated instruments and sensors.
Indian Institute of Chemical Biology (IICB), Kolkata, West Bengal is putting emphasis on quality
basic research, on projects having applied potential and is looking forward to a successful Industry-
Institute liaison towards closer partnership.
Indian Institute of Integrative Medicine (IIIM), Jammu, J&K has primary focus of research on drug
discovery from natural products (medicinal plants and microbial species).
Central Drug Research Institute (CDRI), Lucknow, Uttar Pradesh has the basic objective of
discovery and development of new drugs and contraceptive agents, and development of innovative,
economic and environment friendly process technologies for known drugs and drug intermediates.
Indian Institute of Toxicology Research (IITR), Lucknow, Uttar Pradesh aims to predict the harmful
effects of chemicals and other environmental stressors at different levels and identify key events leading
to adverse health outcomes.
Central Institute of Mining and Fuel Research (CIMFR) Dhanbad, Jharkhand deals with research on
fuel efficiency, Oxy-fuel combustion studies etc.
Indian Institute of Petroleum (IIP), Dehradun is engaged in multidisciplinary areas of research &
development including petroleum refining and value addition to refinery systems, automotive engines &
emissions, tribology, industrial and domestic combustion etc. The institute provides technical and
analytical services to petroleum refining and related industry including technology transfer for
developing novel, state-of-art technologies and products.
(Data/Information based on Institute Inputs/Public Domain)
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Cited references and related references
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Technologies Information Control & Communication, Setubal, 2008.
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Mattern and S. E. Sarma, Springer-Verlag Berlin, Berlin, 2008, vol. 4952, pp. 140–154.
3. A. Dalla Mora, D. Contini, S. Arridge, F. Martelli, A. Tosi, G. Boso, A. Farina, T. Durduran, E. Martinenghi, A.
Torricelli and A. Pifferi, Biomed. Opt. Express, 2015, 6, 1749–1760
4. A. Escarpa, Chem. Rec., 2012, 12, 72–91 .
5. A. Ilic, T. Staake and E. Fleisch, IEEE Pervasive Comput., 2009, 8, 22–29 .
6. A. Kwiatkowski, M. Czerwicka, J. Smulko and P. Stepnowski, J. Forensic Sci., 2014, 59, 1358–1363
7. A. Martin, D. Vilela and A. Escarpa, Electrophoresis, 2012, 33, 2212–2227 .
8. Alastair J. Ward, Near-Infrared Spectroscopy forDetermination of the Biochemical MethanePotential: State of the Art
Chemical Engineering and Technology. 2016, 39, No. 4, 611–619.
9. Anil Gupta and R.K. Sharma (2010). A New Method for Estimation of Automobile Fuel Adulteration, Air Pollution,
Vanda Villanyi (Ed.), InTech, DOI: 10.5772/10054. https://www.intechopen.com/books/air-pollution/a-new-method-
for-estimation-of-automobile-fuel-adulteration
10. Barlow R. BU Today. Jul 26, 2012. A new counterfeit problem: Anti-malarial drugs.
11. Barras J, Althoefer K, Rowe MD, Poplett IJ, Smith JAS. The emerging field of medicines authentication by nuclear
quadrupole resonance spectroscopy. Applied Magnetic Resonance. 2012;43(4):511–529.
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Related Further Reading
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