Urinary Drug Confirmation of Selected Analytes

Transcription

1 Liquid Chromatography Mass Spectrometry SSI-LCMS- Urinary Drug Confirmation of Selected Analytes LCMS-8 Summary: Forty analytes, and the associated internal standards for each, are included in this urinary drug confirmation panel. Method: A Restek Ultra Biphenyl mm x mm, um particle column is used in these analyses. Mobile phase A is Ammonium Formate in LCMS grade water and mobile phase B is Methanol with Ammonium Formate. Samples are prepared by making a four-fold dilution with % mobile phase A followed by glucuronidase enzymatic hydrolysis. Transfer the top ul to an autosampler vial and inject ul into the LCMS for analysis. Analyses from each sample are replicated using iterations. Figure : LC-MS drug panel MS chromatogram at. ppb min

2 SSI-LCMS- High Panel Analytes Type Transition Reference Ion Polarity Range Curve Fit Type R Amphetamine D IST.9> ppb Amphetamine Target 6.>9. 6.> ppb Linear.998 MDMA D IST 98.9> ppb MDMA Target 9.>6. 9.> ppb Linear.999 Normeperidine D IST 7.9> ppb Normeperidine Target.9>6..9> ppb Linear.999 Doxepine D IST 8.> ppb Doxepin Target 8.>7. 8.> ppb Linear.999 Desipramine D IST 7.>7. 7.> ppb Desipramine Target 67.>. 67.> ppb Linear.999 Cyclobenzaprine D IST 79.> ppb Cyclobenzaprine Target 76.>. 76.> ppb Linear.999 Hydromorphone D6 IST 9.>8. 9.> ppb Hydromorphone Target 86.>8. 86.> ppb Linear.999 Gabapentin D IST 8.9>6. 8.9> ppb Gabapentin Target 7.9>. 7.9> ppb Linear.998 Codeine D6 IST 6.> ppb Codeine Target.>.9.> ppb Linear.999 Norhydrocodone D IST 89.>. 89.> ppb Norhydrocodone Target 86.> > ppb Linear.999 Methamphetamine D IST 6.>97. 6.> ppb Methamphetamine Target.>9..> ppb Linear.996 O-Desmethyltramadol D6 IST 6.> ppb O-Desmethyltramadol Target.>8..> ppb Linear.999 Methylone D IST.9> ppb Methylone Target 7.9>6. 7.9> ppb Linear.997 MDEA D6 IST.> ppb MDEA Target 8.>. 8.> ppb Linear.999 Benzoylecgonine D IST 9.9> ppb Benzoylecgonine Target 9.>68. 9.> ppb Linear.997 Methylphenidate D9 IST.> ppb Methylphenidate Target.9>6..9> ppb Linear.996 Ritalinic acid D IST.> ppb Ritalinic acid Target.>8..> ppb Linear.997 Flurazepam Target 88.>. 88.> ppb Linear.998 Imipramine D IST 8.> ppb Imipramine Target 8.>8. 8.> ppb Linear.999 EDDP-D IST 8.> ppb EDDP Target 78.>9. 78.> ppb Linear.999 Midazolam Target 6.>9. 6.> ppb Linear.998 Table : MS characterization of high response panel analytes

3 SSI-LCMS- High Panel Analytes Type Transition Reference Ion Polarity Range Curve Fit Type R Oxazepam D IST 9.9> ppb Oxazepam Target 87.>.9 87.> ppb Linear.99 Methadone D IST.> ppb Methadone Target.>6..> ppb Linear.999 Nordiazepam D IST 76.>. 76.> ppb Nordiazepam Target 7.>9.9 7.> ppb Linear.999 Flunitrazepam D7 IST.>7..> ppb Flunitrazepam Target.>68..> ppb Linear.999 Hydrocodone D6 IST 6.> ppb Hydrocodone Target.>98.9.> ppb Linear.999 Alprazolam D IST.> ppb Alprazolam Target 9.>. 9.> ppb Linear.99 Tapentadol D IST.> ppb Tapentadol Target.>..> ppb Linear.999 Tramadol D IST 68.> ppb Tramadol Target 6.>8. 6.> ppb Linear.999 Meperidine D IST.> ppb Meperidine Target 8.>. 8.> ppb Linear.999 PCP D IST 9.> ppb PCP Target.>86..> ppb Linear.999 Nortriptyline D IST 67.>. 67.> ppb Nortriptyline Target 6.>. 6.> ppb Linear.998 Amitriptyline D IST 8.>. 8.> ppb Amitriptyline Target 78.>. 78.> ppb Linear.999 Clomparimine D IST 8.> ppb Clomipramine Target.>8..> ppb Linear.999 Temazepam D IST.9> ppb Temazepam Target.8>..8> ppb Linear.999 Diazepam D IST 9.>98. 9.> ppb Diazepam Target 8.>. 8.> ppb Linear.999 Mephedrone D IST 8.> ppb Mephedrone Target 78.>6. 78.> ppb Linear.997 Hydrocodone D6 IST 6.> ppb Hydrocodone Target.>98.9.> ppb Linear.999 Fentanyl D IST.> ppb Fentanyl Target 7.>. 7.> ppb Linear.997 Merperidine D IST.> ppb Merperidine Target 8.>. 8.> ppb Linear.999 Table (Continued): MS characterization of high response panel analytes

4 >6.(+) 6.>9.(+) SSI-LCMS- 7 Hydromorphone Conc. Ratio Amphetamine Temazepam Methylone MDMA 86.>8.(+) 86.>7.(+) Conc. Ratio Conc. Ratio Conc. Ratio Conc. Ratio.8>8.(+).8>.(+) 7.9>89.9(+) 7.9>6.(+) 9.>.(+) 9.>6.(+) Curve Curve Curve Curve Curve Figure : curves with statistical data for representative high panel analytes. Inset spectra show MS signals at. ppb for each analyte..6

5 SSI-LCMS Nordiazepam Conc. Ratio Normeperidine Conc. Ratio Desipramine PCP Cyclobenzaprine 7.>6.9(+) 7.>9.9(+) 7.9>.(+).9>6.(+) 67.>7.(+) 67.>.(+) Conc. Ratio Conc. Ratio Conc. Ratio.>9.(+).>86.(+) 76.>.(+) 76.>.(+) Curve Curve Curve Concentrations (ppb) Point Area %RSD Accuracy Curve Curve Concentrations (ppb) Point Area %RSD Accuracy Figure (Continued): curves with statistical data for representative high panel analytes. Inset spectra show MS signals at. ppb for each analyte..

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