HPLC/MS测定人血浆中盐酸班布特罗及其代谢物特布他林的浓度

Determination of Bambuterol and Its Metabolites Terbutaline in Human Plasma by HPLC/MS

目的 :用高效液相 /质谱联用法测定人血浆中盐酸班布特罗及其代谢物特布他林的浓度。方法 :液相 :采用SupelcodiscoveryC18色谱柱 (5 μm ,2 5 0mm× 4 6mm) ;柱温 40℃ ;流动相为甲醇 -醋酸铵溶液 (0 0 0 7mol·L-1) (2 0∶80 ) (并用冰醋酸调 pH =4 8) ,流速 0 6mL·min-1,进样量 6 0 μL ;质谱 :大气压化学电离源 (APCI) ,选择性监测 (SIR)质荷比 (m/z)分别为 2 2 6 (特布他林 ) ,2 6 0 (内标 ) ,36 8(班布特罗 )带正电荷的分子离子峰定量。样品用固相萃取小柱提取处理。结果 :班布特罗线性范围 0 12 5～ 16 μg·L-1,最低检测浓度为 0 0 5 μg·L-1。特布他林线性范围 0 312 5～ 40 μg·L-1,最低检测浓度为 0 0 5 μg·L-1。班布特罗和特布他林的萃取回收率均在 90 %以上 ,日内、日间的RSD皆小于 15 %。结论

Objective:To establish a HPLC/MS method for the determination bambuterol and its metabolites terbutaline in human plasma.Methods:LC: Use Supelco discovery C 18 column(5 μm,250 mm×4 6 mm);The mobile phase consisting of methanol-0 007 mol·L -1 ammonium acetate buffer(20∶80)(pH adjusted to 4 8 by acetic acid),a flow rate of 0 6 mL·min -1 ,injection volume 60 μL. MS: Use atmospheric pressure chemical ionization(APCI),and selected ion mass spectral (m/z) 226(terbutaline),260(internal standard),368(bambuterol)to quantify.The plasma samples were extracted with solid phase extraction.Results:The linear range of bambuterol was 0 125～16 μg·L -1 and limit of test was 0 05 μg·L -1 .The linear range of terbutaline was 0 312 5～40 μg·L -1 and the limit of detection was 0 05 μg·L -1 .Bambuterol and terbutaline extraction recovery rates were more than 90%;intra-day RSD and inter-day RSD were less than 15%.Conclusion: This method was found to be sensitive,fast,and accurate.Therefore,it can be used for pharmacokinetic studies of bambuterol and terbutaline in human plasma.