UPLC-MS/MS同时测定乳核内消液中的贝母素甲、贝母素乙、西贝母碱和湖贝甲素

Simultaneous determination of peimine,peiminine,sipeimine and hupehenine in Ruhe Neixiao liquids by UPLC-MS/MS

目的采用超高效液相色谱-串联质谱法同时测定乳核内消液中贝母素甲、贝母素乙、西贝母碱、湖贝甲素的含量。方法经超声离心后,采用YMC-Triart C_(18)色谱柱(150 mm×2.1mm,3μm),流动相为乙腈-0.1%甲酸溶液,梯度洗脱,流速0.3 mL·min^(-1),柱温35℃;质谱采用ESI^(+)离子源,多反应监测模式检测。结果贝母素甲、贝母素乙、西贝母碱、湖贝甲素等的线性范围分别为0.119~23.72μg·mL^(-1)(r=0.9958)、0.120~23.94μg·mL^(-1)(r=0.9951)、0.105~20.93μg·mL^(-1)(r=0.9942)、0.109~21.72μg·mL^(-1)(r=0.9900),平均回收率(n=6)分别为99.4%(RSD=2.00%)、98.3%(RSD=2.20%)、100.9%(RSD=1.90%)、98.7%(RSD=2.50%)。结论所用方法同时测定了乳核内消液中4种生物碱成分的含量,方法灵敏、准确、重复性好,为乳核内消液的质量控制和综合评价提供了方法。

OBJECTIVE To simultaneously determine the contents of peimine,peiminine,sipeimine and hupehenine in Ruhe Neixiao liquids by UPLC-MS/MS.METHODS The samples were separated on a YMC-Triart C_(18) column(150 mm×2.1 mm,3μm)by gradient elution at the flow rate of 0.3 mL·min^(-1) using acetonitrile and 0.1%aqueous formic acid as the mobile phase.The column temperature was set at 35℃.Multiple reaction monitoring scanning(SRM)was employed for the quantification with ESI source polarity in positive mode.RESULTS The linear ranges of peimine,peiminine,sipeimine and hupehenine were good,which were in the ranges of 0.119-23.72μg·mL^(-1)(r=0.9958),0.120-23.94μg·mL^(-1)(r=0.9951),0.105-20.93μg·mL^(-1)(r=0.9942)and 0.109-21.72μg·mL^(-1)(r=0.9900).The average recoveries(n=6)were respectively 99.4%(RSD=2.00%),98.3%(RSD=2.20%),100.9%(RSD=1.90%)and 98.7%(RSD=2.50%).CONCLUSION Peimine,peiminine,sipeimine and hupehenine in Ruhe Neixiao liquids are determined by this method simultaneously.This method is sensitive,accurate and reproducible.