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。
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.
出处
《应用化学》
CAS
CSCD
北大核心
2012年第5期591-596,共6页
Chinese Journal of Applied Chemistry
