液相色谱-串联质谱法快速测定人血浆中布洛芬

 目的建立快速、灵敏的液相色谱-串联质谱(LC-MS/MS)方法测定人血浆中布洛芬。方法血浆样品经液-液萃取后,以乙腈-甲醇-5 mmol·L^-1醋酸铵-甲酸(450∶450∶100∶0.062 5)作为流动相,采用Zorbax Eclipse XDB-C₁₈柱分离,通过电喷雾电离源以多反应监测(MRM)方式进行负离子检测。用于定量分析的离子反应分别为m/z205→m/z161(布洛芬)和m/z229→m/z185(内标,萘普生)。结果人血浆中布洛芬测定的线性范围为50.0～25 000μg·L^-1,定量下限为50.0μg·L^-1,日内、日间精密度(RSD)均小于8.5%,准确度(RE)在±2.5%以内,每个样品测试时间仅为4.0 min。结论pH值是影响布洛芬色谱行为和质谱响应的主要因素,优化后的方法具有快速、灵敏等特点,适用于布洛伪麻片中布洛芬的生物利用度和生物等效性研究。

Rapid Determination of Ibuprofen in Human Plasma by Liquid Chromatography-Tandem Mass Spectrometry Method

OBJECTIVE To developed a simple,sensitive and rapid liquid chromatography-tandem mass spectrometric method for the determination of ibuprofen in human plasma.METHODS Ibuprofen and the internal standard,naproxen,were processed from plasma by liquid-liquid extraction with n-hexane,and then chromatographed on a Zorbax Eclipse XDB-C₁₈ column(4.6 mm×150 mm,5 μm),using acetonitrile-methanol-5 mmol·L^-1 ammonium acetate-formic acid(450∶450∶100∶0.062 5) as the mobile phase.An API 4000 tandem mass spectrometer equipped with Turbo Ionspray ionization source was used as detector and was operated in the negative ion mode.Multiple reaction monitoring(MRM) with the precursor to product ion combinations of m/z 205→161 and m/z 229→185 were used to quantify ibuprofen and naproxen(IS),respectively.RESULTS The linear range of the calibration curve for ibuprofen was 50.0-25 000 μg·L^-1.The limit of quantification was 50.0 μg·L^-1 by using 25 μL plasma sample.Each sample was assayed within 4.0 min.CONCLUSION The method was proved to be rapid,sensitive and suitable for bioavailability and bioequivalence investigations of ibuprofen formulations.