UPLC-MS/MS测定犬血浆中的氢溴酸加兰他敏

目的采用超高效液相色谱-串联质谱法测定犬血浆中氢溴酸加兰他敏(GH)的含量。方法采用BEH C18色谱柱(50 mm×2.1 mm,1.7μm),流动相为乙腈-0.01 mol·L-1醋酸铵(含0.1%甲酸)(40∶60),流速0.1 mL·min-1,柱温40℃,进样量3μL。GH及内标盐酸克仑特罗的监测离子分别为:m/z 288.23→198.06,m/z 277.08→202.93。结果 GH的线性范围为2.38～609.60μg·L-1(r=0.998,n=5),在人血浆基质中,高、中、低浓度(4.76、38.10、304.80μg·L-1)的日内、日间RSD均小于15%,方法的平均回收率为102.3%;血浆基质对测定无干扰。结论所建方法处理简单、快速、灵敏、特异性高,定量准确,适用于血浆中GH的测定。

Determination of Galanthamine hydrobromide in the dog plasma by UPLC-MS/MS

OBJECTIVE To establish a selective and sensitive UPLC-MS/MS method for determination of Galanthamine hydrobromide in the dog plasma.METHODS BEH C18(50 mm×2.1 mm,1.7 μm)was used as the solid phase,the mobile phase consisted of acetonitrile-0.01 mol·L-1 ammonium acetate(contained 0.1% formic acid)(40:60).The flow rate was 0.1 mL·min-1,column temperature was 40 ℃,and inject volume was 3 μL.The monitoring ion of Galanthamine hydrobromide and internal standard clenbuterol hydrochloride was m/z 288.23→198.06,m/z 277.08→202.93,respectively.RESULTS A good linearity was shown in the range of 2.38-609.60 μg·L-1(r=0.998,n=5).The average recovery was 102.3% with intra-day RSD and inter-day RSD less than 15%.Plasma matrix had no effect on quantification of Galanthamine hydrobromide.CONCLUSION A simple,rapid,sensitive,selective and accurate UPLC-MS method was developed for the determination of Galanthamine hydrobromide in plasma.