The Challenges of AnalyticalMethod Validation forHallucinogens and DesignerStimulants in BiologicalSamples Using LC-TOFBar...
Goals•The Need:•Accurate, sensitive, versatile tools.•Identification•Detection•Routine analysis•Novel, complex, esoteric a...
NMS Labs Center for InnovationCrim. Blood UrineJWH-018JWH-073~35 Cpds.TimeCP47,497HU210JWH-018JWH-073JWH-019JWH-250JWH-081...
NMS Labs Center for InnovationCrim. Blood/urineMDMAMDAMDEATFMPPBZPDBZP5-MeO-DIPT…~30 Cpds.Timeatropinebenzylpiperazinedext...
The ScopeBath Salts and Stimulant Designer Drugs – Expanded43 Compounds• Classical StimulantsAmphetamine, Methamphetamine,...
The ScopeBath Salts and Stimulant Designer Drugs – Expanded43 Compounds (Continued)• 2C Series – Stimulants with Hallucino...
The TechnologyPerformance Checklist: High Sensitivity High Performance High Resolution Mass Accuracy (>5ppm) User Frie...
The TechnologyLiquid Chromatography-Time of Flight MassSpectrometry (LCTOF/LCQTOF)• Agilent 1200 HPLC system• Agilent 6230...
The TechnologyLiquid Chromatography-Time of Flight MassSpectrometry (LCTOF/LCQTOF)• Agilent 1200 HPLC system• Agilent 6230...
Time of Flight (TOF)6200/6500 Series Time of Flight Mass Spectrometry(LCTOF/LCQTOF)
AnalysisLiquid Chromatography-Time of Flight MassSpectrometry (LCTOF/LCQTOF) - Control
•A sample is considered positive if the followingare true:The area is greater than or equal to 25% of theaverage area of ...
AnalysisLiquid Chromatography-Time of Flight MassSpectrometry (LCTOF/LCQTOF) - Control
AnalysisLiquid Chromatography-Time of Flight MassSpectrometry (LCTOF/LCQTOF)
AnalysisLiquid Chromatography-Time of Flight MassSpectrometry (LCTOF/LCQTOF) - Control
AnalysisLiquid Chromatography-Time of Flight MassSpectrometry (LCTOF/LCQTOF) – Case 1
AnalysisLiquid Chromatography-Time of Flight MassSpectrometry (LCTOF/LCQTOF) – Case 1
AnalysisLiquid Chromatography-Time of Flight MassSpectrometry (LCTOF/LCQTOF) – Case 1
AnalysisLiquid Chromatography-Time of Flight MassSpectrometry (LCTOF/LCQTOF) – Case 1
AnalysisLiquid Chromatography-Time of Flight MassSpectrometry (LCTOF/LCQTOF) – Case 1
AnalysisLiquid Chromatography-Time of Flight MassSpectrometry (LCTOF/LCQTOF) – Case 1
AnalysisLiquid Chromatography-Time of Flight MassSpectrometry (LCTOF/LCQTOF) – Case 1
AnalysisLiquid Chromatography-Time of Flight MassSpectrometry (LCTOF/LCQTOF) – Case 1Criterion ValueMass Defect 161.46ppmR...
AnalysisLiquid Chromatography-Time of Flight MassSpectrometry (LCTOF/LCQTOF) – Case 2
AnalysisLiquid Chromatography-Time of Flight MassSpectrometry (LCTOF/LCQTOF) – Case 2
AnalysisLiquid Chromatography-Time of Flight MassSpectrometry (LCTOF/LCQTOF) – Case 2
AnalysisLiquid Chromatography-Time of Flight MassSpectrometry (LCTOF/LCQTOF) – Case 2MDMAC11H15NO2193.2423MethedroneC11H15...
AnalysisLiquid Chromatography-Time of Flight MassSpectrometry (LCTOF/LCQTOF) – Case 2MDMAC11H15NO2193.2423MethedroneC11H15...
Qualitative Validation Assay Validation Cut-off Verification Sensitivity and Specificity Interfering Substances Carry...
Time of Flight8756B/U Bath Salts and StimulantsDesigner Drugs – Expanded8085B/U Drug Impaired Driving/DREToxicology Bath S...
Designer Drugs TrendsNMS Labs Designer Drugs Trends ReportAugust 2012http://www.nmslabs.com/services-forensic-designer-dru...
Compare and ContrastLCMSMS LCTOF LCQTOFTarget CompoundAnalysisComprehensiveScreeningTarget CompoundanalysisMust set up sca...
•NMS Labs• Alex Maggitti• Sherri Kacinko• Matthew McMullin• Fran Diamond•Agilent• Tom Gluodenis• Jay Levine• Mary Cuddrye•...
The Challenges of Analytical Method Validation for Hallucinogens and Designer Stimulants in Biological Samples Using LC-TOF
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The Challenges of Analytical Method Validation for Hallucinogens and Designer Stimulants in Biological Samples Using LC-TOF

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The Challenges of Analytical Method Validation for Hallucinogens and Designer Stimulants in Biological Samples Using LC-TOF

Hosted by Agilent Technologies on October 8, 2012

Presented by Barry K Logan, Ph.D., NMS Labs National Director, Forensic Services

Published in: Health & Medicine, Technology
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  • The Challenges of Analytical Method Validation for Hallucinogens and Designer Stimulants in Biological Samples Using LC-TOF

    1. 1. The Challenges of AnalyticalMethod Validation forHallucinogens and DesignerStimulants in BiologicalSamples Using LC-TOFBarry K Logan, Ph.D.,NMS Labs National Director, Forensic Services
    2. 2. Goals•The Need:•Accurate, sensitive, versatile tools.•Identification•Detection•Routine analysis•Novel, complex, esoteric and designer drugs and otheranalytes in a variety of matrices and sample types.•The solution:•LCMS/MS•LCTOF, LCQTOF
    3. 3. NMS Labs Center for InnovationCrim. Blood UrineJWH-018JWH-073~35 Cpds.TimeCP47,497HU210JWH-018JWH-073JWH-019JWH-250JWH-081JWH-122JWH-200JWH-210AM-2201AM-694RCS-4RCS-8DEA schedulingProfessional activitiesClient EnquiriesCrim. CaseworkAcademic collaborationInternational contactsVendor activityJWH-018 metsJWH-073 metsJWH-019 metJWH-250 metAM-2201 metJWH-018 metsJWH-073 metsCP47,497 (C8)~17 Cpds.CP47,497 (C7)HU-210Internet purchasesWeb IntelligenceCustomer Feedback~42 Cpds.JWH-203JWH-022AM-2233AM-1248XLR-11UR-144AKB-48A720,296RCS-4 metJWH-122 metJWH-210 metJWH-081 metJWH-200 metJWH-250 metJWH-210 metJWH-081 metJWH-122 metJWH-398 metSyntheticCannabinoids
    4. 4. NMS Labs Center for InnovationCrim. Blood/urineMDMAMDAMDEATFMPPBZPDBZP5-MeO-DIPT…~30 Cpds.TimeatropinebenzylpiperazinedextromethorphandimethyltryptamineketamineMDAMDMAmescalinephencyclidinescopolamine2C-B2C-B-FLY2C-T-75-MeO-DIPTAMTBDBMBDBMephedroneLSDbufoteninpsilocinsalvinorin Asalvinorin BTFMPPDEA schedulingProfessional activitiesClient EnquiriesCrim. CaseworkAcademic collaborationInternational contactsVendor activity~10 Cpds.Internet purchasesWeb IntelligenceCustomer Feedback~70 Cpds.Blood/urineExpanded…MDPVMethyloneAmphetaminem-CPPO-desmethyltramadolDMAA3,4-DMMC4-MECPentylone2C-C2C-E2C-I2C-P2C-T-2Bromo-Dragon Fly5-MeO-DALTBuphedroneEthylonePetedronePhenazepam….StimulantsandHallucinogens
    5. 5. The ScopeBath Salts and Stimulant Designer Drugs – Expanded43 Compounds• Classical StimulantsAmphetamine, Methamphetamine, MDMA, MDEA, DOM,DOB, PMA, Cocaine, Benzoylecgonine• CathinonesCathinone, Mephedrone, Buphedrone, Methylone, Ethylone,Butylone, Pentylone, Mmethcathinone, Methedrone,Naphyrone, 3-FMC, 4-FMC, 4-MEC, 3,4-DMMC,
    6. 6. The ScopeBath Salts and Stimulant Designer Drugs – Expanded43 Compounds (Continued)• 2C Series – Stimulants with Hallucinogenic Properties2C-B, 2C-C, 2C-E, 2C-H, 2C-I, 2C-N, 2C-P, 2C-T-2, 2C-T-7• BenzylpiperazinesBZP, TFMPP, DBZP, MBZP, m-CPP• OthersPhenazepam, Mitragynine, 7-OH Mitragynine,O-desmethyltramadol, DMAA
    7. 7. The TechnologyPerformance Checklist: High Sensitivity High Performance High Resolution Mass Accuracy (>5ppm) User Friendly and Adaptable Data Reduction Tools Versatility Stable Performance Robust Design Technical Support Value/ROI
    8. 8. The TechnologyLiquid Chromatography-Time of Flight MassSpectrometry (LCTOF/LCQTOF)• Agilent 1200 HPLC system• Agilent 6230 with Jet Stream Technology• Mass Hunter Software
    9. 9. The TechnologyLiquid Chromatography-Time of Flight MassSpectrometry (LCTOF/LCQTOF)• Agilent 1200 HPLC system• Agilent 6230 with Jet Stream Technology• Agilent 6530 QTOF• Mass Hunter Software
    10. 10. Time of Flight (TOF)6200/6500 Series Time of Flight Mass Spectrometry(LCTOF/LCQTOF)
    11. 11. AnalysisLiquid Chromatography-Time of Flight MassSpectrometry (LCTOF/LCQTOF) - Control
    12. 12. •A sample is considered positive if the followingare true:The area is greater than or equal to 25% of theaverage area of the responses for the two decisionpoint cut off calibrators (10ng/mL).The retention times are within +/- 0.02 min of theaverage retention time of the decision point cut offcalibrators.The Mass Accuracy is within +/- 30ppmEstablishing Acceptance Criteria
    13. 13. AnalysisLiquid Chromatography-Time of Flight MassSpectrometry (LCTOF/LCQTOF) - Control
    14. 14. AnalysisLiquid Chromatography-Time of Flight MassSpectrometry (LCTOF/LCQTOF)
    15. 15. AnalysisLiquid Chromatography-Time of Flight MassSpectrometry (LCTOF/LCQTOF) - Control
    16. 16. AnalysisLiquid Chromatography-Time of Flight MassSpectrometry (LCTOF/LCQTOF) – Case 1
    17. 17. AnalysisLiquid Chromatography-Time of Flight MassSpectrometry (LCTOF/LCQTOF) – Case 1
    18. 18. AnalysisLiquid Chromatography-Time of Flight MassSpectrometry (LCTOF/LCQTOF) – Case 1
    19. 19. AnalysisLiquid Chromatography-Time of Flight MassSpectrometry (LCTOF/LCQTOF) – Case 1
    20. 20. AnalysisLiquid Chromatography-Time of Flight MassSpectrometry (LCTOF/LCQTOF) – Case 1
    21. 21. AnalysisLiquid Chromatography-Time of Flight MassSpectrometry (LCTOF/LCQTOF) – Case 1
    22. 22. AnalysisLiquid Chromatography-Time of Flight MassSpectrometry (LCTOF/LCQTOF) – Case 1
    23. 23. AnalysisLiquid Chromatography-Time of Flight MassSpectrometry (LCTOF/LCQTOF) – Case 1Criterion ValueMass Defect 161.46ppmRT Diff 0.016minApparentConc.36ng/mLNot Confirmed X
    24. 24. AnalysisLiquid Chromatography-Time of Flight MassSpectrometry (LCTOF/LCQTOF) – Case 2
    25. 25. AnalysisLiquid Chromatography-Time of Flight MassSpectrometry (LCTOF/LCQTOF) – Case 2
    26. 26. AnalysisLiquid Chromatography-Time of Flight MassSpectrometry (LCTOF/LCQTOF) – Case 2
    27. 27. AnalysisLiquid Chromatography-Time of Flight MassSpectrometry (LCTOF/LCQTOF) – Case 2MDMAC11H15NO2193.2423MethedroneC11H15NO2193.2423
    28. 28. AnalysisLiquid Chromatography-Time of Flight MassSpectrometry (LCTOF/LCQTOF) – Case 2MDMAC11H15NO2193.2423MethedroneC11H15NO2193.2423Confirmedby GCMS √
    29. 29. Qualitative Validation Assay Validation Cut-off Verification Sensitivity and Specificity Interfering Substances Carryover Matrix Matching Stability
    30. 30. Time of Flight8756B/U Bath Salts and StimulantsDesigner Drugs – Expanded8085B/U Drug Impaired Driving/DREToxicology Bath Salts Add-On• Test design based on:• 43 compounds• Regular updates based on trends• Compounds found in “bath salts” casework• Federally Scheduled Drugs• Covers additional drugs scheduled in manystates• Drugs emerging in Europe
    31. 31. Designer Drugs TrendsNMS Labs Designer Drugs Trends ReportAugust 2012http://www.nmslabs.com/services-forensic-designer-drug-trends
    32. 32. Compare and ContrastLCMSMS LCTOF LCQTOFTarget CompoundAnalysisComprehensiveScreeningTarget CompoundanalysisMust set up scanninggroupsAcquire all data andquery database laterAcquires more limiteddata in QTOF modeWYSIWYG Post hoc identification Post hoc identificationCompound specifictransitionsMolecular formulainformationMolecular formulainformation forfragmentsLimited structuralconfirmationNo structuralinformationLimited StructuralinformationMay differentiateisobarsTOF does notdifferentiate isobarsMay differentiateisobarsLower Cost Higher cost Even higher cost
    33. 33. •NMS Labs• Alex Maggitti• Sherri Kacinko• Matthew McMullin• Fran Diamond•Agilent• Tom Gluodenis• Jay Levine• Mary Cuddrye• John HughesAcknowledgements

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