Liquid Chromatography Mass Spectrometry SSI-LCMS-8 LCMS-8 Drugs of Abuse: Analytes with Polarity Switching LCMS-8 Summary Seventy six analytes and their internal standards are described below. Multiple drug classes (barbituates, opiates, amphetamines, tricyclic antidepressants, synthetic cannabinoids, cannabinoids, club drugs, bath salts and hypnotics) were analyzed in a five minute polarity switching LCMS-8 method. Method A total of analytes and internal standards were analyzed from enzymatically hydrolyzed urine. The sample was diluted by a factor of six and then directly injected onto the LCMS- 8. The linear range tested for these analytes was from ng/ml. A HPLC column with a guard column was used with a binary gradient. The flow rate was. ml/min and the column temperature was C. The injection volume was µl. LCMS-8 Analysis Electrospray ionization (ESI) with polarity switching was used for ionization of each analyte. The MS temperatures and gas parameters for the LCMS-8 are listed in Table. Multiple reaction monitoring (MRM) methods were used for MS analysis. MS Parameters Nebulizing Gas Flow L/min Heating Gas Flow L/min Drying Gas Flow L/min Interface ESI Interface Temperature C DL Temperature C Heat Block Temperature C Table. LCMS-8 mass spectrometer interface parameters.
SSI-LCMS-8................. min Figure. Representative chromatogram for all drug class analytes in under minutes. Results and Discussion A representative chromatogram of all analytes is shown in Figure. All analytes are eluted from the column in just under. minutes. Calibration curves and MS chromatograms for the low standard for oxymorphone, pentobarbital, naloxone, lorazepam, methamphetamine, THC-COOH, tepentadol, alprazolam, methaqualone, gabapentin, noroxycodone, dextrorphan, MDPV, and zolpidem are shown in Figure. These analytes represent the many drug classes that are analyzed with this method. Calibration curves demonstrate linearity over these ranges The retention time, area, linear range, calculated concentration, standard concentration (low limit) and percent accuracy for all analytes measured in this drug panel are listed in Table. The accuracy values for all analytes are between 9 and. Conclusions A polarity switching method for analytes was demonstrated for a wide array of drug classes using the ultra fast LCMS-8 triple quadrupole mass spectrometer.
SSI-LCMS-8 Oxymorphone :.>.(+) :.>98.(+). r =.99 8 Pentobarbital :.>8.(-) :.>.(-) 9 r =.999. 8.. Naloxone.........8.8 :8.>.(+) :8.>.(+)......... Conc. Ratio 9 8 r =.999.9.9........ Lorazepam 8:.8>.8(+) 8:.8>.9(+) 8 9 Conc. Ratio 8 r =.99 9 8...8.8.9.9.... Methamphetamine 8:9.9>9.9(+) 8:9.9>8.9(+) 8 9 Conc. Ratio... r =.998 -......8.8.9.9. THC-COOH 8:.>99.(+) 8:.>9.(+)........ Conc. Ratio r =.99....8.8.9.9...... Tepentadol :.>.9(+) :.>.9(+).......... Conc. Ratio r =.999... 9 8.9.9........ Alprazolam :8.9>8.(+) :8.9>.(+)........ Conc. Ratio 9 8 r =.998............. Methaqualone 9:.>.(+) 9:.>9.9(+).......... Conc. Ratio 9 8 r =.998.......... Gabapentin 8:.>.9(+) 8:.>.(+) Conc. Ratio 8 r =.99 9 8.9.9........ Noroxycodone :.>8.(+) :.>8.(+) :.>.(+) 8 9 Conc. Ratio.... r =.99 8....8.8.9.9... Dextrorphan :8.>.(+) :8.>.(+) 9 8 8 9 Conc. Ratio r =.99. 9 8 -.........8.8 MDPV :.>.8(+) :.>.(+).....8.8.9.9............... 8. 9. Conc. Ratio.......... Zolpidem Conc. Ratio r =.998 r =.99.......... Conc. Ratio 8:8.>.(+) 8:8.>.(+).9......... 8 9 Conc. Ratio Figure. Calibration curves and MS chromatograms for the low reporting limit for the representative analytes (oxymorphone, pentobarbital, naloxone, lorazepam, methamphetamine, THC- COOH, tepentadol, alprazolam methaqualone, gabapentin, noroxycodone, dextrorphan, MDPV, zolpidem).
SSI-LCMS-8 Name Ret. Time Area Linear Range Calculated Conc. Std. Conc (Low limit) Accuracy Lisdexamfetamine., - 9. 9. Morphine.9 9, -.9 9.9 Oxymorphone.9, - 9. 98. Noroxycodone.9,99 -. 9.9 Hydromorphone.9,89 -.. Pregabalin. 9, - 98.8 98.8 Gabapentin.8 8, - 9. 9. Amphetamine.88 88, - 9.8 98.8 -MAM.98,98 -.. Naloxone.9, - 98. 98. Methylhexanamine.99 8,9-9. 98.8 Codeine., -.9 Phentermine.,,98-9. 98. Methamphetamine. 8, - 8. 9.9 Norhydrocodone.,9-9.8 99. O-desmethyltramadol. 9, - 9. 98. Methylone.9,9-9. 9. Oxycodone. 8, -. 9. -methylephedrine.,9 -.8. Hydrocodone., -..8 MDMA.,8-8.8 9. Diethylpropion.,88 -.9 9.8 MDEA. 89, - 9.9 99.9 Tapentadol.,9 -.98 99.9 Norfentanyl., -.. Dextrorphan., -.. Tramadol.9, -.. Benzoylecgonine.,9 -.. Methylphenidate., - 9. 99 Normeperidine.8,8 -.9 98.8 Meperidine.,9 -.. Meprobamate.,88-9. 99. Zopiclone.,89-9. 9. Phenobarbital.8,9 -.8. MDPV.8,8 - -aminoclonazepam.8, - 9.9 99.9 Norbuprenorphine.899, -.. Butalbital.9, - 9. 9 Table. Results for the low reporting level for all analytes measured. Included in the table are retention time, area, linear range, calculated concetration, standard conc. and percent accuracy.
SSI-LCMS-8 Name Ret. Time Area Linear Range Calculated Conc. Std. Conc (Low limit) Accuracy Pentobarbital., - 99.88 99.9 Amobarbital.,8-9.8 9.8 Zolpidem.8 89, -.. Fentanyl. 89,9 -.. Secobarbital.9,9-99. 99. Buprenorphine. 9, -.. Carisoprodol. 9,9-9. 99. Flurazepam.,98-9.9 99.9 Phencyclidine.9,8 -.8 9.9 Propoxyphene.8, - 9.9 99.8 Desipramine.,8-9. 98.8 Imipramine. 8,89-9. 98. Sufentanil.8,9-9. 9. Mitragynine. 9, -.. Cyclobenzaprine. 9,8 -.. Nortriptyline. 98, -.89.8 EDDP.9, - 8.9 9 Amitriptyline.8, -.. N-desmethylflunitrazepam., - 8. 9. Lorazepam.8,9 -.. Chlordiazepoxide.8,8 -.9. Oxazepam.89, - 9. 98 Clonazepam.88 9, -..8 Methadone.9, -.8. Midazolam.989, - 9.9 99.9 Desalkylflurazepam.99 9,8-8.9 9. Methaqualone.8 8,9 -. Zaleplon., - 9.8 98. Nordiazepam.8, -.. Flunitrazepam.98, -..8 Temazepam.9 9, - 8. 9. Triazolam., -.. Alprazolam. 9, - 9. 99. Diazepam.9 8,99-9.9 99.8 JWH-8 Pentanoic Acid.,8 -.. JWH- Butanoic Acid., -.. THC-COOH., -.9. XLR-.88 8,8 -.. Table (continued). Results for the low reporting level for all analytes measured. Included in the table are retention time, area, linear range, calculated concetration, standard conc. and percent accuracy.
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