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LC-MS/MS法测定人血清中氟比洛芬含量

LC-MS/MS determination of flurbiprofen in human serum
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摘要 目的:建立液相色谱-串联质谱法(LC—MS/MS)测定人血清中氟比洛芬的含量。方法:血清经甲醇直接沉淀法去除蛋白质后,以液相色谱分离、电喷雾离子化串联质谱进行检测,氟比洛芬和消炎痛(内标)的 MRM 扫描离子通道 m/z 分别为243.3→198.8,356.3→312.0。二者的保留时间分别为0.9 min,1.6 min。采用 API3000串联质谱仪及 Shimadzu 系列液相色谱仪,Gemini C_(18)柱(50 mm×2.1 mm,5μm),流动相为乙腈-水(18:82,用氨水调 pH 为8.0),流速为0.3 mL·min^(-1),进样体积为3 μL,每个样品的分析时间为3 min。结果:氟比洛芬在0.05~50μg·mL^(-1)范围内线性关系良好(r=0.9995),日内、日间RSD 分别为4.1%~5.5%及4.2%~6.8%,准确度为99.6%~109.5%。结论:本法样品预处理简便快速,检测准确灵敏专一,适用于氟比洛芬药物动力学和生物利用度的研究。 Objective:To establish a liquid chromatography- tandem mass spectrometry( LC -MS/MS)method for the determination of flurbiprofen in human serum. Method: The serum samples were precipitated with methanol. The drug was determinated by LC -MS/MS using electrospray ionization. Flurbiprofen and its internal standard (IS)indomethacin were detected on multiple reaction monitoring (MRM) by the transitions from the precursor to the product ion (m/z 243.3/198.8 and m/z 356.3/312.0). The retention time of these two analytes were 0. 9 min and 1.6 min. An API3000 tandem mass spectrometer and an Shimadzu liquid chromatograph were used for all analyses. The analytical column was a Gemini C18 column (50 mm × 2. 1 mm,5 μm). The mobile phase, acetonitrile - water ( 18: 82) , was used at a flow rate of 0. 3 mL · min^-1. The injection volume was 3 μL and the total run time was 3.0 min. Results : Calibration curve had good linearity in the range of 0.05 - 50 μg·mL^ -1 ( r = 0. 9995 ). The intra - and inter- day precision(RSD) were all less than 15% and the accuracy was within 99.6 -101.5%. Conclusion:The established LC - MS/MS method is shown to be sensitive, accurate and simple for the determination of flurbiprofen in human serum. It is suitable for the pharnlacokinetics and bioavailability study of flurbiprofen.
出处 《药物分析杂志》 CAS CSCD 北大核心 2008年第8期1248-1251,共4页 Chinese Journal of Pharmaceutical Analysis
关键词 氟比落芬 液相色谱-串联质谱 血药浓度 含量测定 flurbiprofen LC - MS/MS drug blood concentration determination
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参考文献8

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