Detection and Validated Quantification of 11 Sedative-Hypnotics in Human Plasma by UPLC-MS/MS Method / 医药导报

ABSTRACT

Objective To develop a rapid ultra high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/ MS) for determination of 11 sedative-hypnotics in human plasma. Methods The plasma samples were extracted with dichloromethanen-hexaneacetoacetate (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 composed 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 (MRM) via electrospray ionization (ESI) source in positive mode. Results Good linear relation was obtained over the investigated concentration range, with all correlation coefficients higher than 0.99. The limit of detection was 200 pg?mL-1 for dexzopiclone,and 10- 20 pg?mL-1 for other sedative-hypnotics. The intra- and inter-day RSD of 11 sedative-hypnotics were no more than 15.0%. The recoveries were in the range of 72.3%-108.0%, and the matrix effects were approximately 0.86- 1. 12. Conclusion The method is rapid, sensitive and reliable, and suitable for the simultaneous determination of 11 sedative-hypnotics in human plasma.