引用本文:
曹慧慧, 彭敬东张, 蕾. 老鼠血清中苯扎贝特的HPLC-MS法测定[J]. 应用化学,
2012, 29(5): 591-596.
doi:
10.3724/SP.J.1095.2012.00269
Citation: CAO Huihui, PENG Jingdong, ZHANG Lei. Quantitative Determination of Bezafibrate in Rat Plasma Using HPLC-MS[J]. Chinese Journal of Applied Chemistry, 2012, 29(5): 591-596. doi: 10.3724/SP.J.1095.2012.00269
Citation: CAO Huihui, PENG Jingdong, ZHANG Lei. Quantitative Determination of Bezafibrate in Rat Plasma Using HPLC-MS[J]. Chinese Journal of Applied Chemistry, 2012, 29(5): 591-596. doi: 10.3724/SP.J.1095.2012.00269
老鼠血清中苯扎贝特的HPLC-MS法测定
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GeminiC18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5μL。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30μg/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。
English
Quantitative Determination of Bezafibrate in Rat Plasma Using HPLC-MS
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.
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Key words:
- bezafibrate
- / HPLC-MS
- / rat plasma
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