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  • Inside this Issue

    February 2010 Issue 41

    Agilent ICP-MS Journal

    2 Improving Data Quality in ICP-MS with Qualifier Ions

    3 Pharma Labs Embrace ICP-MS Ahead of New US Pharmacopeia Standards

    4-5 High Throughput Analysis of Lead in Whole Blood using ICP-MS with ISIS-DS

    6 User article: Simultaneous Speciation Analysis of Fe, Zn, S and P using the 7500ce with O2 Cell Gas

    7 Call For Papers for 2nd Edition of Agilent's Speciation Handbook, 20% Price Decrease for 7500 ICP-MS Supplies

    8 Reflections on the Winter Plasma Conference 2010, Two New 7700 ICP-MS Recorded Webinars, Conferences, New ICP-MS Publications

  • 2 Agilent ICP-MS Journal February 2010 - Issue 41 www.agilent.com/chem/icpms

    Using Qualifier Ionsin ICP-MS to ValidateDataEd McCurdyICP-MS Product Marketing, Agilent Technologies

    The Agilent 7700x ICP-MS incorporatesa 3rd generation Collision/ReactionCell (CRC) which operates effectivelyin helium (He) mode. In contrast toreactive cell gases, which work onlyfor specific reactive interferences,He mode is universal, as it effectivelyfilters out all polyatomic ions regardless of their reactivity. Thebenefits of He mode for multi elementanalysis of complex, variable andunknown sample matrices have beenwell documented, but He mode has afurther important benefit. He modesimultaneously removes all polyatomicinterferences from all isotopes of eachanalyte, thereby making secondaryions (isotopes) available for manyanalytes.

    The use of qualifier ions to confirmthe identity of a target analyte iscommon practice in organic massspectrometry, where the mass of thetarget ion does not provide unequivocalanalyte identification. ICP-MS spectraare comparatively simple, whichmeans that primary or preferred isotopes give much more certainidentification of the target analyte;however, quantification of many elements can be affected by the presence of matrix-based polyatomicinterferences. By quantifying an element independently using boththe primary and secondary isotopes,the results can be compared; goodagreement validates the data, indicatingthat the reported concentration wasnot affected by any interference.

    Comparison of Results for IsotopePairsIn the data presented here, ten complexsynthetic sample matrices were analyzed on the 7700x, using He,reaction (H2) and no gas modes. Ineach matrix, the relative % difference(RPD) was calculated, to comparethe results from the primary andqualifier isotopes of several analytes;good agreement (i.e. a RPD close tozero) indicates effective removal ofinterferences from both isotopes.

    Figure 1 shows excellent agreementbetween the 65Cu/63Cu results in He Figure 2. Comparison of 53Cr/52Cr results in 3 modes and 10 matrices

    Figure 1. Comparison of 65Cu/63Cu results in 3 modes and 10 matrices

    mode (green bars) in all matrices (allHe mode results were

  • www.agilent.com/chem/icpms 3Agilent ICP-MS Journal February 2010 - Issue 41

    Pharma LabsEmbrace ICP-MSAhead of New USPharmacopeiaStandardsJrme Darrouzs and Amir LibaICP-MS Product Specialists, Agilent Technologies

    Pharmaceutical companies will soon beusing instrument-based methodologyto control elemental impurities in theirproducts, rather than the outdatedwet-chemistry based colorimetrictest (USP) that is the currentstandard method recommended bythe US Pharmacopeia (USP).

    USP is a non-profit, non-governmentalagency that sets standards for pharmaceutical manufacturers andbuyers to follow; these standards arethen enforced by the US Food &Drug Administration (FDA). USP isfully committed to advancing thecurrent standards that governmetals in pharma products so thatwidely agreed upon safe limits forkey metal impurities are properlymeasured, thereby protecting publichealth. To achieve this goal, USP hasdrafted a new performance-basedmethod, USP (target analytes andlimits) and USP (procedures)for determining elemental impuritiesin pharmaceutical materials.

    The revisions focus on two areas: Introducing new performance-

    based methodology to test for elemental impurities in drug substances and drug products including analysis using modern analytical technology.

    Setting limits for acceptable levelsof metal impurities.

    Current revisions are out for consultation, with comments due byApril 15, 2010. Final versions arescheduled for release by June 2010with implementation expected bySeptember 2013.

    Key Points of the New Standards Drug manufacturers will be able to

    select any analytical method or instrument, as long as they can demonstrate accuracy, sensitivity and specificity.

    Instrumental analytical techniques(e.g. ICP-MS/OES) are recommended.

    the proposed method USP (for dietary supplements) requiresspeciation measurement for As andHg if these elements are presentabove the threshold limit. ICP-MS ismuch better suited to speciationmeasurement than ICP-OES due tobetter sensitivity and interferenceremoval. Labs that want to buy asingle instrument and have to choosebetween ICP-MS and ICP-OES willfind that ICP-MS offers much greaterflexibility and performance for notmuch more investment.

    Benefits of Agilent ICP-MS for Pharma Applications High sensitivity and 9-orders

    dynamic range Excellent matrix tolerance with

    HMI (High Matrix Introduction) Potential to analyze a large

    number of samples daily Semiquantitative screening using

    helium mode to effectively removepolyatomic interferences

    Full 21 CFR Part 11 compliance with Agilent OpenLab ECM

    Tolerance to organic solvents, andease of coupling to LC and GC forspeciation studies.

    Further Reading www.usp.org

    A list of 16 elements has been compiled, with limits based on toxicology rather than the (limited) capability of the existingUSP method.

    Compliance with the limits specified for Class 1 elemental impurities (As, Cd, Hg, Pb) is required for all drug products.

    A risk-based approach can be usedto define which other elements (Class 2 elemental impurities) should be analyzed in different sample types.

    A full description of proposed methodology is provided, including sample preparation steps, with guidance on how to evaluate analytical merit.

    Speciation of As & Hg is required if total content determined in dietary supplements* exceeds a defined limit.

    *USP is also introducing a new General Chapterrelating to dietary supplements and their ingre-dients: Elemental Contaminants in DietarySupplements (USP).

    The Role of ICP-MS in PharmaThe control of inorganic impuritieshas always been a critical issue tothe pharmaceutical industry, as eventrace levels can adversely affect drugstability and shorten the shelf life ofsome pharmaceutical products. As aresult, ICP-MS is already widelyused by the pharmaceutical industryahead of proposed changes to USPprotocols. Typical applications includequantification of metallic impuritiesand catalyst residues in in-processcontrols, raw materials, and isolatedintermediates leading up to activepharmaceutical ingredient (API).There is also a diverse range ofapplications for trace metal analysisin pharmaceutical discovery, development and commercializationprojects utilizing HPLC and GC toseparate species prior to ICP-MSanalysis.

    Advantages of ICP-MS Comparedto ICP-OES for New USP MethodsOf the two recommended techniques(ICP-OES and ICP-MS) described inthe USP methods, ICP-MS is a muchbetter fit for the application thanICP-OES. All the Class 1 elements(As, Cd, Pb and Hg) and Class 2 elements (transition metals and platinum group elements used ascatalysts) defined in the proposedmethod USP are easily measured at low concentrations byICP-MS in a single run, with superiorsensitivity to ICP-OES. In addition,

    Figure 1. Agilent 7700x ICP-MS capable of routine pharma applications, as well as moreadvanced studies for R&D facilities.

  • conditions providing a highly reproducible and accurate analysis.

    ExperimentalInstrument parameters were optimizedto normal robust plasma conditionswith oxide levels ~1% (CeO+/Ce+) Table 1.

    Table 1. 7500cx and ISIS-DS operating parameters

    Samples were supplied by theCalifornia Department of PublicHealth (CADPH) and were analyzedaccording to the CADPH methodwhich specifies a 50x dilution of thewhole blood. The high matrix toleranceof the 7500cx allows whole blood tobe analyzed routinely at a 10x dilutionand many labs take that approach.However, in compliance with theCADPH method, a 50x dilution wasapplied for this work. The samplesconsisted of the following: base blood,1 ppb spike base blood, 1 ppb CCV,CCB (diluent only), and the followingCADPH Standard Reference Materials(SRM); low blood QC (4.980.17g/dL* Pb), medium blood QC(9.660.12 g/dL Pb), and high blood QC (19.030.29 g/dL Pb) samples.These samples were analyzedrepeatedly for a total of approximately300 analyses. Calibration standardswere not matrix matched and consisted of a blank, 0.01, 0.05, 0.1, and 1 g/dL Pb, yielding an instrumentdetection limit of 3.09 x 10-4 g/dL (3.1 ppt) (Figure 1).

    Instrument Parameters No Gas Mode

    Forward power (W) 1550

    Sample depth (mm) 8

    Carrier gas (L/min) 0.85

    Makeup gas (L/min) 0.15

    Extract 1 (V) 0

    ISIS loop length (cm) 50

    ISIS loop ID (mm) 0.8

    ISIS loop volume ( L) 250

    ISIS stabilization time(sec) 20

    Sample Name Sample No. Ave Pb conc Std Dev % RSD %(n) (g/dL) Recovery

    Base Blood 52 0.004 0.0003 6.09 NA

    Base Blood Spike 45 0.097 0.0011 1.20 97%(1 ppb)

    CCB 26 0.0002 0.00010 46.5 NA

    CCV 26 0.099 0.0014 1.36 99%

    Low Blood SRM 45 4.911 0.0687 1.40 99%

    Med Blood SRM 44 9.696 0.1136 1.18 100%

    High Blood SRM 44 18.947 0.2231 1.18 100%

    4 Agilent ICP-MS Journal February 2010 - Issue 41 www.agilent.com/chem/icpmsTable 3. Whole blood sa

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Inside this Issue February 2010 – Issue 41 Agilent ICP-MS Journal 2 Improving Data Quality in ICP-MS with Qualifier Ions 3 Pharma Labs Embrace ICP-MS Ahead of New US Pharmacopeia Standards 4-5 High Throughput Analysis of Lead in Whole Blood using ICP-MS with ISIS-DS 6 User article: Simultaneous Speciation Analysis of Fe, Zn, S and P using the 7500ce with O 2 Cell Gas 7 Call For Papers for 2 nd Edition of Agilent's Speciation Handbook, 20% Price Decrease for 7500 ICP-MS Supplies 8 Reflections on the Winter Plasma Conference 2010, Two New 7700 ICP-MS Recorded Webinars, Conferences, New ICP-MS Publications
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