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,5 μm)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 devolop a liquid chromatographic-tandem mass spectrometric (LC-MS/MS) method for the determination of B07 in rabbit plasma.METHODS Analytes were separated from plasma by a combination of alkalinized protein precipitation and liquid-liquid extraction with methyl tert-butyl ether. Chromatographic separation was performed on a Waters Symmetry C₁₈ (4.6 mm×150 mm, 5 μm)column with the mobile phase consisted of acetonitrile (containing 0.2% acetic acid ) -40 mmol·L^-1 ammonium acetate (containing 0.2% acetic acid) in water (80∶20). A tandem mass spectrometer equipped with electrospray ionization source was used as detector and operated in the positive ion mode. Quantification was performed using multiple reaction monitoring (MRM) of the transitions m/z 529.3→335.4 and m/z 237.1→194.1 for B07 and carbamazepine (internal standard), respectively.RESULTS The method showed a good linearity in a concentration range of 0.31-310 ng·mL^-1for B07 was more than 0.99. The intra- and inter-day precision was less than 15% and the absolute recovery was above 75%.CONCLUSION This method was selective and rapid, sensitive for investigating blood drug concentrations in rabbit.