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老鼠血清中苯扎贝特的HPLC-MS法测定

曹慧慧,彭敬东*,张蕾   

  1. (西南大学化学化工学院,发光与实时分析教育部重点实验室 重庆 400715)
  • 收稿日期:2011-06-21 修回日期:2011-08-13 出版日期:2012-05-10 发布日期:2012-05-10
  • 通讯作者: 彭敬东,副教授; Tel:023-68254290; Fax:023-68254000; E-mail:hxpengjd@swu.edu.cn; 研究方向:高效液相色谱

Quantitative Determination of Bezafibrate in Rat Plasma Using HPLC-MS

CAO Huihui, PENG Jingdong*, ZHANG Lei   

  1. (Chemistry and Chemical Engineering,Southwest University,Education Ministry Key Laboratory on
    Luminescence and Real-Time Analysis,Chongqing 400715)
  • Received:2011-06-21 Revised:2011-08-13 Published:2012-05-10 Online:2012-05-10

摘要: 建立一种简便、快速、灵敏的高效液相色谱-质谱联用测定老鼠血清中苯扎贝特的方法。 采用Gemini C18色谱柱;流动相:V(乙腈)∶V(甲醇)∶V(水)=60∶15∶25(0.03%甲酸水溶液);柱温35 ℃,流速0.3 mL/min;紫外吸收波长为235 nm;进样量5 μL。 质谱采用电喷雾电离负离子模式,用于定量分析的离子分别为[M-H]- m/z 359.65→273.70(苯扎贝特)和[M-H]- m/z 212.95→127.08(氯贝酸)。 对苯扎贝特检测的线性范围为0.073~7.884 mg/L,r=0.9995。 得到苯扎贝特的平均回收率为94.3%~103.1%;方法的日内和日间的相对标准偏差(RSD)均小于6%;最低检测限(LOD)与定量限(LOQ)分别为9.0和30 μg/L;为临床上人体血清中苯扎贝特的浓度检测提供了一种重现性好、灵敏度高的分析方法。

关键词: 苯扎贝特, HPLC&, ndash, MS, 老鼠血浆

Abstract: A simple, rapid and sensitive HPLC-MS method was developed and validated for determining bezafibrate in rat plasma. Chromatographic separation was achieved on a reversed-phase Gemini C18 at 35 ℃ using acetonitrile, methanol and 0.03% aqueous solution of formic acid(volume ratio 60∶15∶25) as mobile phase at flow rate of 0.3 mL/min. The UV absorption wavelength was set at 235 nm and the injection volume was 5 μL. Under these conditions, the detection was performed with negative electrospray ionization, monitoring the transitions m/z 359.65→273.70 for bezafibrate and m/z 212.95→127.08 for the clofibric acid(internal standard). A good linearity was achieved within the concentration range of 0.073~7.884 mg/L(r=0.9995) for bezafibrate and the mean recovery of samples ranged from 94.3% to 103.1% at three tested concentrations. The intra-day and inter-day precisions(as relative standard deviation) were below 6%. The limit of quantification(LOQ) was 30 μg/L and the limit of detection(LOD) was 9 μg/L. This HPLC-MS method was reproducible and sensitive enough for routine analysis of bezafibrate in human plasma.

Key words: benzafibrate, HPLC&, ndash, MS, rat plasma

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