2.1 Le Blanc

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  • 1. ISBM,ManchesterUK,9th 11th September 2013 HOW CONFIDENT ARE WE? Alain LeBlanc Special projects manager, support services and external quality assessment Centredetoxicologie duQubec(CTQ) INSPQ,Qubec,Canada Pierre Dumas Research & Development division
  • 2. TheINSPQisaprovincialgovernmentbodycreatedtoimprove thecoordination,developmentanduseofexpertiseinpublichealth Amongitsexpertise,theCentredetoxicologie duQubec(CTQ) offersanalyticalsupportinclinical,environmentalandoccupationalhealth www.inspq.qc.ca/ctq
  • 3. QUEBEC MINISTRY OF HEALTH AND WEALTHFARE (MSSS) INSTITUT NATIONAL DE SANT PUBLIQUE DU QUBEC (INSPQ) ENVIRONMENTAL HEALTH AND TOXICOLOGY DEPT. (DSET) CENTREDETOXICOLOGIEDUQUBEC(CTQ) ClaudeThellen QUALITYMANAGEMENT SergineLapointe TOXICOLOGY LABORATORYBRANCH NormandFleury SPECIALPROJECTS,SUPPORT SERVICESandEQASSECTOR AlainLeBlanc RESEARCH PierreAyotte METHOD DEVELOPMENT PatrickBlanger CLINICAL ORGANICS MichelLefebvre Eric Gaudreau METALS CiprianMihai Cirtiu PROJECT MANAGEMENT andSUPPORT SERVICES EXTERNAL QUALITY ASSESSMENT SCHEMES
  • 4. Tomake scientists,researchers and epidemiologists aware ofdaytoday issuesthat laboratories encounter when confronted with testing newenvironmental contaminants Triclosan
  • 5. Todevelop reliable,robust andaccurate analytical methods Toassuretracability ofthemetrology Toassuretracability ofthedata Toassurethecomparability oftheanalytical results Todevelop andmaintain competence ofstaff
  • 6. Sample collection,integrity andstorage Timeofcollection(spot/24hrs;daytoday variability) Handling(freeze/thaw) Stability (+>5yrs) Homogeneity:free/conjugated species Contamination(collectionprocess,container,) Sampling container(adsorptionontoplastics)/Tubes Arewe surewe aremeasuring therightbiomarker?intherightmatrix? Shippingconsiderations (overnight,deep freeze) Analytical innovation Keep costs down;compromisewith multianalyte methods Tendtoless invasivematrices,butarethey therightones?
  • 7. Analytical standards Availability ofconjugated analytes Accuracy (certificates,multiplesources) Impactonbiomonitoring data(cycletocycle) Availability ofappropriate internal standards 13Clabeled andunlabeled analogs areusually notavailable at thesame time Customsynthesis (TRC,CANSYN,CHIRON,CIL,etc) Highcost,timetodelivery,lottolot,purity (UV,NMR,IRandMSspectra) Analytical methods Classical versusexperimental protocols Sensitivity (LODs)andspecificity Reportablelimits (nointernationalconsensus;study comparisons) Laboratory contamination(ex:BPA,Triclosan,Parabens,BDEs,)
  • 8. Analytical instrumentation Comparability Reference materials Availability (certified?) Appropriateness (same matrix?)commutability Internal RM2nd sourceofstandard!! External quality assessment schemes Howtocomparestudy results? Collaborationamong reference labs orresearch centers Tohelpreduce vulnerability
  • 9. SAMPLEINTEGRITYANDSTORAGE
  • 10. Sample Temperature Tracking Chart Freeze/thaw 30 Temperature C 20 10 0 -10 -20 -30 Sample handling: Chronological events (worst case scenario)
  • 11. Freeze/Thaw StabilityoftotalBPAinurine(14samples) 125 120 115 +10% 105 % BPA 110 +5% 100 -5% 95 90 -10% 85 80 cycle 0 cycle 1 cycle 2 cycle 3 cycle 4
  • 12. Freeze/Thaw StabilityofconjugatedBPAinurine(14samples) 100 %Conjugated BPA 98 96 94 92 90 88 cycle 0 cycle 1 cycle 2 cycle 3 cycle 4
  • 13. %Recovery inurine TipR50%ACN FreeTriclosan canbe rapidlyadsorbedonto plastictipsaccordingto typeofmaterialand%of acetonitrile inspike solution. Timeresidenceinthe pipettetipscanincrease thedegreeofadsorption. 100 TipR5%ACN 97 TipR0%ACN 95 TipB50%ACN 101 TipB5%ACN 91 TipB0%ACN 90 TipY50%ACN1Min 98 TipY5%ACN1Min TipY0%ACN1Min 82 75 TipY50%ACN 103 TipY5%ACN TipY0%ACN 93 86
  • 14. InternalQCfrom unspiked urine. Endogenousconjugated formoftrichlorophenol 18.7 Concentration (ug/L) 17.7 16.7 15.7 14.7 13.7 Goodstability 12.7 49 76 3 8 49 17 2 59 7 00 48 47 48 42 2 7 83 1 25 46 45 46 66 6 1 45 08 5 49 44 43 91 0 11.7 # squence 7.250 ExternalQCmadefrom spikedurineusingfree trichlorophenol 5.250 4.250 Poorstability 3.250 2.250 # squence 3 49 76 8 49 17 2 59 48 48 00 7 2 47 42 7 46 83 1 46 25 6 45 66 1 08 45 49 44 91 0 5 1.250 43 Concentration (ug/L) 6.250
  • 15. ANALYTICALSTANDARDS
  • 16. Supplier MMP MEP MiBP MnBP MCHP MBzP MEHP MEHHP MEOHP MECPP MOP MCPP MNP CIL2006 25% 2% 47% 1% 63% 29% 11% 7% 12% 22% 39% CIL2009 9% Certified solutions CIL2010 11% 5% 13% 12% 76% 14% 21% 4% 3% 2% 70% 16% 3% 9% 0% 11% 7% 3% 11% 19% 9% 2% 3% 78% 10% 3% Accustandard 26% 31% 19% 4% 27% Accustandard 8% 7% 5% 2% 27% Aldrich 9% 6% 5% Chiron Chiron 21% 0% Neat standards DrEhrenstorfer 13% 2% 29% CanSyn 9% 5% 4% 1% 6% 1% 8% 6% 4% 1% 10% 7% 3% CIL 0% 0% 0% 0% 0% 0% 0% 0% 0% 0% 0% 0% 0% TRC 7% 3% 4% 6% 10% 2% 11% 9% 9% 70% 12% 2% 6% Langlois E., LeBlanc A., Simard Y., Thellen C. Accuracy investigation of phthalate metabolite standards Journal of Analytical Toxicology, 2012 ; 36 :270-279
  • 17. BPA Triclosan compoundssynthesized at CHUL BPA13C12 andTCS13C12 were obtained from CambridgeIsotopeLaboratories
  • 18. ANALYTICALMETHODS
  • 19. CadmiuminurinebyICPMS MoOinterference correctedVSuncorrected Meanconcentrationcanbe biasedby30%withindividual errorgreaterthan200% Comparabilitybetweenstudies isstronglyrelatedtolaboratory methodologies Moinsample Moincalibrationcurve 30 21 Cd nmol/L Laboratories CV% 35 25 32 20 15 10 23 9.5 78 5 130 0 0 50 100 150 200 Ratioconc.Mo/Cd 250 300
  • 20. Cadmium Urine (nmol/L) QMEQAS 2011-2 Lab B Lab A
  • 21. X1.6 ComparingUnitedStatesandCanadianpopulationexposuresfromNationalBiomonitoring Surveys:Bisphenol Aintakeasacasestudy JudyS.LaKind,Johanne Levesque,PierreDumas,ShirleyBryan,JanineClarkeandDanielQ.Naiman JournalofExposureScienceandEnvironmentalEpidemiology(2012)22,219226
  • 22. X1.6
  • 23. QC Low QC High Target value 2.90 0.23 10.17 0.58 CTQ 1 2.98 10.6 CTQ 2 2.82 10.2
  • 24. NCI PCB153(1g/L)+PCB132(0.3g/L) Completeoverlap ofboth congeners EI
  • 25.