Emerging approaches of Analytical and Sensory Quality … AIDA 5... · 2017. 10. 10. · Disclaimer...

Binod K MaitinIndependent Technical Consultant

Emerging approaches of Analytical and Sensory Quality

Assessment of Spirits Beverages

Technical Seminar Bangalore, October 5-6, 2017

Disclaimer : This presentation is intended only for knowledge dissemination by Binod K Maitin . Reproduction in any form is prohibited.

Knowledge for Innovation & Excellence

Contents

Critical Quality Imperatives

Emerging Instrumental Analytical Techniques

Emerging Sensory Techniques



Quality Control and consistency

Process Improvement & optimisation

Assessing product shelf life

Flavour Profiling

Product Authenticity & counterfeit protection

Trouble shooting & Problem solving

Precision & Accuracy of the reported values

Supply Chain Improvement

Regulatory compliance

Consumer Driven New Product Development

Critical Quality Imperatives




Optical Methods

• UV-VIS - Authenticity Analysis

• Fluorescence - Adulterant Analysis

• NIR – Alcohol Analysis

Trace Metal Analysis Techniques

Other Emerging Techniques

Instrumental Sensory Techniques

• Olfactory – GC/MS

• E-nose




Rapid

Better accuracy and higher Precision

More Specific and Lower MDL

Computer Aided “ Intelligent ” Instruments

• Excellent Data Management Capabilities

• Faster Unattended Automated Analysis

• Adaptability for in-line Process Analysis



Optical Methods UV -VIS NIR FLUORESCENCE



Reference : A.G. Mignani et al. / Sensors and Actuators B 171– 172 (2012) 458– 462

PCA & Pattern Recognition Software



Ocean Optics Spirit Sampler – UV Vis



Ocean Optics Spirit Sampler – UV Vis



• Highly accurate measurement of the alcohol content of your spirits in the concentration range 35 to 65 %vol

• Alcohol content of liqueurs in the concentration range of 15–40 %vol (in combination with MCP 100 circular polarimeter)

• Optional pH, color and turbidity measurement

• For spirits such as whisky, cognac, brandy, vodka, gin, tequila and rum

• For liqueurs based on saccharose or invert sugar

• Accurate, fully automatic thermostatting via an integrated solid-state thermostat

NIR based Alcolyzer for Alcohol analysis

Alcolyzer Spirits measures the NIR spectrum of the

sample in the range of the 2nd overtone of the C-H

stretching vibration near 1200 nm. It utilizes the

symmetrical vibration of the methyl group because

its pronounced and distinct shape is little

influenced by the matrix.



Fluorescence Spectroscopy of Spirits

Reference : Jana Sádecká et al (2016). Fluorescence Spectroscopy for the Analysis of Spirit Drinks, Applications of Molecular Spectroscopy to

Current Research in the Chemical and Biological Sciences, Dr. Mark Stauffer (Ed)

Spirits contains intrinsic fluorophoresFluorescence spectroscopy allows the determination of some compounds at

concentration as low as 0.1–1 μg/L often without sample preparation. Total Luminescense Spectra (TLS) and total

synchronous fluorescence spectrum (TSFS) of Brandy and Vodka are shown.

Perkin–Elmer LS 50 Luminescence Spectrometer

equipped with the Xenon lamp used for right

angle and front face geometry




Complies with any regulatory requirements.Leachng of Lead &

Arsenic concentration from poor-quality copper distillation vessels

Cadmium from decorative crystal containers

Control of heavy metal content as levels of trace elements can also

significantly affect the taste of the Spirits

Fingerprint of the metal concentration






Other Emerging Techniques

Site-specific Natural Isotope Fractionation - Nuclear Magnetic Resonance

(SNIF – NMR) –

Distinguishes natural and synthetic origins with great specificity.

Detects isotopic ratios of deuterium and hydrogen (D/H) on multiple

sites in a molecule.

Specific Natural Isotope Profile by Isotope Ratio Mass Spectrometry (SNIP –

IRMS)

Based on multi isotopic fingerprinting in which 13C/12C isotope ratios

values are measured on several components of the same product and

make use of the intermolecular isotope correlations between these

components to assess its authenticity.

SNIF- NMR and SNIP – IRMS are rapid and extremely sensitive techniques that

may become useful in authenticity assessment



• Olfactometry – GC/GCMS

• Electronic Nose ( E-Nose)

Instrumental Sensory Techniques



Olfactometry – GC/GCMS

GCMS- Olfactometer with ODP and Sampling Accessories

Photo: GERSTEL GmbH & Co.KG

Isolation procedures for volatile odour active compounds, Head space (HS), Solid Phase Micro

Extraction (SPME), and Liquid–Liquid Extraction (LLE), are frequently used for spirits beverages.



Electronic Nose ( E-Nose)

Heracles II Dual Flash Gas Chromatography E-Nose. Photo: Alpha MOS



Electronic Nose ( E-Nose) contd. An artificial olfaction technology emerged as a powerful tool for fast sensory quality

evaluation of spirit beverages.

Considered most potential complimentary techniques commonly employed analysis

of volatiles and non-volatiles

The new generation Alpha MOS : HERACLES II Electronic Nose provides fast and

efficient fingerprint signature analysis of the product. Uses technology of dual

fast/flash gas chromatography to detect the chemical compounds responsible for the

taste and aroma characteristics of products. Ultrafast GC analysis facilitates high

analysis throughput at the production plant.

AroChemBase library includes nearly 84,000 compounds with their Kovats index,

chemical data and, for around 2,000 of these molecules provide information on the

related sensory attributes and human odour detection thresholds.

Intelligent chemometrics and other software makes the technique very useful



Emerging Sensory Methods & Tools

Retronasal Tasting

Temporal Dominance of Sensation (TDS)

Rapid Sensory Profiling for consumer research

Training & Proficiency



19

Sensory Evaluation

“ A scientific discipline used to evoke, measure,

analyze and interpret those responses to products

that are perceived by the senses of sight, smell,

touch, taste and hearing”

Stone, H and Sidel, JL. 1993. Sensory Evaluation Practices. 2nd ed. Academic Press: San Diego.

All senses are important when eating or drinking but of all the five senses,

sense of smell that is plumbed into our memory through the limbic

system in our brain and has direct access to our world of feelings…



Molecules released into the air inside our mouths as we chew and swallow travel up

through the retronasal passage into the nose, then move up and contact the olfactory

epithelium. Flavor is the combination of true taste (sweet, salty, sour, bitter) and

retronasal olfaction

Taste versus Flavor



Orthonasal and Retronasal tasting



Examples of GMP Compliant safe to taste Sensory References

Acetaldehyde Pungent, Solvent, Green Apple Skin, Leafy, Grassy, Cardboard

Earthy Dusty, Chalky

Isovaleric Cheesy, Sweaty, Rancid

Butyric Baby Vomit, Rancid, Cheesy, Putrid

Ethyl Acetate Fruity, Nail Enamel, Solvent, Acetone, Paint, Glue

Mercaptan Sulphury, Drain, Gas, Butane-like

Brett-Barnyard Band-aid, Medicinal, Sweaty Horses

Ethyl Butyrate Tropical Fruits, Pineapple, Banana, Mango

Metallic Metal, Iron Rust, Blood-like

Diacetyl Buttery, Butterscotch, Creamy, Toffee

H2S Sulphury, Rotten Egg

Musty Corky, Musty, Dampness

DMS Sweetcorn, Cooked Cabbage, Tomato, Shellfish, Oyster-like

Isoamyl Acetate Fruity, Banana

Plastic Styrene, Acrylic, Solvent

Dry Hay / Plastic Hay-like, Straw, Husky

Iso Amyl Alcohol Fusel Oil, Fruity, Banana, Estery



Temporal Dominance of Sensation (TDS)

Data provides a sequence of dominant sensations over time



Expert & Consumer Sensory Panel

In the sensory theory:

• Experts panels are used for the products’ description

• Consumers should only be used for the hedonic task

• They lack two essentials qualities for profiling (consensus & reproducibility)

• There are strong halo effects

In the sensory practice:

Consumers are sometimes used for both tasks it has been proven

that consumers’ description show the required qualities (consensus

and reproducible)



Traditional Descriptive Analysis

•Complete Sensory Lexicon Complete Sensory

•Panel Consensus Fingerprint

Quick Analysis Robust Data

Easy & Quick to interpret

Reliable & Actionable Results

Screened & Trained Assessors Expensive

Require On-going Training

Time Consuming



Rapid Profiling Techniques

- Additional consumer testing focuses on evaluating overall liking

on hedonic scale followed by QDA by trained sensory panel.

- Newer methods are being adopted to incorporate sensory

profiles by consumers and effectively utilized for NPD.

Flash Profiling/Free Choice Profiling

Projective Mapping ( Sorting / Napping®)

Repertory Grid

-----------------------------------------------------------

Less Cost

Reduced Time

Criteria Important to the Individual Assessor



Repertory Grid

Participants are asked to describe how two products are alike or different

from the third and to score the intensity of their own constructs. Bipolar

construction allows to collect relevant and understandable information

about what consumers perceive

Flash Profile

Participants are given all the samples at a time and asked to list down the

descriptive terms which differentiate these products and then to rank the

products on all the descriptive term they found. It is an efficient and

accurate method to capture consumer’s perception

Consumer Sensory Methods



Projective Mapping (Napping)

Participants use their own criteria to position the samples according to their

perceived similarity. Then they describe the products in their own words. This

identifies the consumer’s ideal product within the defined category.

Check All That Apply (CATA)

Participants describe the samples using a set of attributes provided. They then

list descriptors they consider appropriate for their ideal product . Gives

information about attributes that are not liked by consumers.

Consumer Sensory Methods Contd.



Intensity Scale (Ideal Profiling Method)

- Participants are asked to rate the intensity of sensory

attributes using unstructured10 cm scale.

- They are then asked to rate the intensity of these

attributes for their ideal product.

- It is an alternative method when trained sensory panels

are not available.

-It is an excellent method to integrated Sensory Science

into NPD

Multivariate data analysis is proved very useful

Facilitates simultaneous measurements on many variables.

Because they analyse all variables together, multivariate

methods are inherently more difficult to understand than

univariate methods (such as ANOVA).

• Most commonly used multivariate methods of analysis include:

– Principal Components Analysis (PCA)

– Generalised Procrustes Analysis (GPA)

– Partial Least Squares Regression (PLS)

– Multiple Factor Analysis (MFA)

– Preference Mapping: etc.

• CAMO or Compusense Sensory Software are excellent tools

advance sensory practices

Statistical Data Analysis and consumer sciences



• Intensive on-site taste panel training

• Standardised & uniform training at all locations within a company

compatible to sensory panel worldwide

• 100% independent proficiency tests helps accreditation

• Blind quality Flavour Standards requiring detection and identification

• On-line software to analyse results and generate reports

• Reduce costs by appropriately training

Importance of Sensory Training & Validation



Levels of Structured training



Purposes of validation:

• Provides insight into the Quality of sensory evaluations

• Measures the effectiveness of your sensory program

• Enables focussed training more efficiently

• Determines the level of confidence in results of daily

tasting results

• Improve Quality, Shelf-life, and Consistency of products

Key importance is proficiency of the tasters



Why use proficiency tests?

• Sensory performance of the panel needs to be regularly

calibrated

• 100% independent proficiency assessments avoid biased

results

• Gain individual and collective tasting data

• Identify strengths and weaknesses

• Reduce training costs

• Improve quality and consistency



Flavor Identification Validation: Individual flavor

identification using standard terminology

Rank Rating Validation: Discrimination of different

flavor intensities and scale them accordingly

In Profile Validation: primary focus on IN or OUT /

meeting the brand‘s sensory specs– ideal for

evaluation of in-process tasters

Methods of Validation



Proficiency Testing – types of validation



Questions ?

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Emerging approaches of Analytical and Sensory Quality … AIDA 5... · 2017. 10. 10. · Disclaimer...

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