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目的建立液相色谱-串联质谱(LC-MS/MS)测定兔血浆中B07的浓度。方法血浆样品经碱化沉淀蛋白后,用甲基叔丁基醚液-液萃取,以乙腈(含0.2%乙酸)-40 mmol·L~(-1)乙酸铵(含0.2%乙酸)水溶液(80∶20)为流动相,采用Waters Symmetry C18(4.6 mm×150 mm,5μm)柱分离;采用电喷雾电离源,以多反应监测(MRM)方式进行正离子检测,用于定量分析的离子对B07为529.3→335.4,内标卡马西平为237.1→194.1。结果测定血浆中B07线性范围为0.31~310 ng·mL~(-1),r>0.99。日内和日间精密度小于15%,提取回收率均大于75%。结论该法选择性强、灵敏度高、重现性好,能够快速、准确测定兔血浆中B07浓度。
Objective To establish a liquid chromatography-tandem mass spectrometry (LC-MS / MS) for the determination of B07 in rabbit plasma. Methods The plasma samples were alkalinized to precipitate proteins and then extracted with methyl tert-butyl ether by liquid-liquid extraction. The samples were eluted with acetonitrile (containing 0.2% acetic acid) and 40 mmol·L -1 ammonium acetate (containing 0.2% acetic acid) 80:20) as the mobile phase and separated by a Waters Symmetry C18 column (4.6 mm × 150 mm, 5 μm). The positive ion was detected by multiple reaction monitoring (MRM) using electrospray ionization source. The ion pair for quantitative analysis B07 was 529.3 → 335.4, and the internal standard carbamazepine was 237.1 → 194.1. Results The linear range of B07 in plasma was 0.31 ~ 310 ng · mL ~ (-1), r> 0.99. The intra- and inter-day precision was less than 15% and the extraction recovery was over 75%. Conclusion The method is selective, sensitive and reproducible. It can rapidly and accurately determine the B07 concentration in rabbit plasma.