High-performance liquid chromatography-atmospheric pressure chemical ionisation-mass spectrometry determination of zaleplon in human plasma.
作者： Beibei Zhang , Zunjian Zhang , Yuan Tian , Fengguo Xu , Yun Chen
DOI: 10.1016/J.JPBA.2005.06.031
关键词:
摘要: Abstract A sensitive and specific liquid chromatography–atmospheric pressure chemical ionisation-mass spectrometry (LC–APCI-MS) method has been developed validated for the identification quantification of zaleplon in human plasma using estazolam as an internal standard (IS). After addition 2.0 M sodium hydroxide solution, samples were extracted with ethyl acetate then organic layer was evaporated to dryness. The reconstituted solution residue injected onto a prepacked Shim-pack VP-ODS C 18 (250 mm × 2.0 mm i.d.) column chromatographed mobile phase comprised methanol:water (70:30) at flow-rate 0.2 ml/min. Detection performed on single quadrupole mass spectrometer by selected ion monitoring (SIM) mode via atmospheric ionization (APCI) source. mean curve linear ( r = 0.9991) over concentration range 0.2–100 ng/ml had good back-calculated accuracy precision. intra-day inter-day precisions within 10% relative deviation ranged from 85% 115%. limit detection 0.1 ng/ml. LC–APCI-MS used successfully study pharmacokinetic, bioavailability bioequivalence adult volunteers.
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