UPLC-MS/MS法同时快速测定消渴丸中3种成分的含量  

Simultaneous Analysis of Three Constituents in XiaoKe Pills Rapidly by UPLC-MS/MS

作　　者：蔡振世 CAI Zhen-shi(Quanzhou Institute For Food And Drug Control,Quanzhou 362000,China)

机构地区：[1]泉州市食品药品检验所,福建泉州362000

出　　处：《海峡药学》2022年第12期52-55,共4页Strait Pharmaceutical Journal

摘　　要：目的建立一种UPLC-MS/MS法同时快速测定消渴丸中葛根素、格列本脲、五味子酯甲含量的方法。方法采用Waters ACQUITY UPLC BEH柱(C_(18) 2.1×50 mm 1.7μm),以0.1%甲酸水溶液(含10 mmol·L^(-1)乙酸铵)-乙腈为流动相梯度洗脱,流速:0.3 mL·min^(-1),柱温30℃,进样量1μL。质谱采用ESI(电喷雾离子源),以正离子多反应监测模式定量分析。结果葛根素、格列本脲、五味子酯甲的线性范围分别为0.2054~5.135μg·mL^(-1)、0.02156~0.5390μg·mL^(-1)、0.02066~0.5165μg·mL^(-1)(r^(2)为0.99315~0.99920),平均加标回收率分别为98.5%、94.2%、93.3%,RSD为2.97%、2.04%、3.45%(n=6)。结论该方法操作方便、快捷、灵敏度高、准确度好,可一次性实现多个不同成分的检测。OBJECTIVE To establish an UPLC-MS/MS method for simultaneous determination of puerarin,glibenclamide,and schisantherin A in XiaoKe pills.METHODS Used ACQUITY UPLC BEH column(C_(18) 2.1×50 mm 1.7μm)with mobile phase of water(contain 0.1%formic acid and 10 mmol·L^(-1) ammonium acetate)and acetonitrile by gradient elution;the flow rate was 0.3 mL·min^(-1),the column temperature was 30℃,and the sample volume was 1μL.ESI(electro spray ion source)was used for mass spectrometry,and positive ion multiple reaction monitoring mode was used for quantitative analysis.RESULTS The linear ranges of puerarin,glibenclamide,and schisantherin A were 0.2054-5.135μg·mL^(-1),0.02156-0.5390μg·mL^(-1),0.02066-0.5165μg·mL^(-1)(r^(2) was 0.99315-0.99920);the average recoveries were 98.5%,94.2%,93.3%;RSD were 2.97%,2.04%,3.45%(n=6),respectively.CONCLUSION The method is convenient,rapid,sensitive and accurate,which can be used to detect multiple components at one time.

关 键 词：UPLC-MS/MS 消渴丸 葛根素 格列本脲 五味子酯甲 

分 类 号：R297[医药卫生—民族医学]