Abstract:
OBJECTIVE To develop a rapid UPLC-MS/MS method for the determination of 8 kinds of benzodiazepines and 3 kinds of non-benzodiazepines in human urine. METHODS The urine samples were extracted with dichloromethane∶ n-hexane∶acetoacetate(5∶4∶1). The separation was performed on a Waters ACQUITY UPLC HSS T3 column(2.1 mm×100 mm, 1.8 μm) using the mobile phase of acetonitrile-0.1% ammonium solution at a flow rate of 0.2 mL·min
-1 in gradient elution mode. The detection was performed on a triple quadrupole tandem mass spectrometer by multiple reaction monitoring via electrospray ionization source in positive mode. RESULTS Good linear relation was obtained over the investigated concentration range, with all correlation coefficients >0.99. The limit detection was 0.5 ng·mL
-1 for dexzopiclone and 0.01-0.02 ng·mL
-1 for other sedativehypnotics. The intra- and inter-day RSDs were <15%(n=5). The recoveries were in 68.8%-115.0%. The matrix effects were approximately 0.85-1.14. CONCLUSION This method is rapid, sensitive, reliable, and suitable for the simultaneous determination of 8 kinds of benzodiazepines, zolpidam, zaleplone and dexzopiclone in human urine.