UPLC-MS-MS法同时测定颠茄片中2个有效成分的含量  

Simultaneous Determination of Two Active Components in Belladonna Tablets by UPLC-MS-MS

作　　者：董丽荣 李应才 孙赟 DONG Lirong;LI Yingcai;SUN Yun(Kunming Institute for Food and Drag Control,Kunming 650031,China;Yunnan University of Chinese Medicine,Kunming 650500,China)

机构地区：[1]昆明市食品药品检验所,云南昆明650031 [2]云南中医药大学,云南昆明650500

出　　处：《云南中医药大学学报》2023年第2期86-89,共4页Journal of Yunnan University of Chinese Medicine

基　　金：云南省科技厅中医联合专项重点项目[2019FF029(-010)]。

摘　　要：目的 建立同时测定颠茄片中硫酸天仙子胺、东莨菪内酯含量的超高效液相色谱串联质谱(UPLC-MSMS)分析方法。方法 采用Waters Acquity UPLC HSS T3色谱柱(2.1 mm×100 mm,1.8μm),用0.1%甲酸水溶液-甲醇为流动相,进行梯度洗脱(0~1 min, 10%B;1~4 min, 10%B→90%B;4~6 min, 90%B;6~6.2 min,90%B→10%B;6.2~8 min, 10%B),流速为0.2 mL·min^(-1),柱温为40℃,进样量4μL;质谱采用电喷雾离子源,正负离子模式,多反应监测模式进行扫描。结果 硫酸天仙子胺、东莨菪内酯分别在193.6~968.0 ng·mL^(-1)(r=0.9996)、1.00~50.00 ng·mL^(-1)(r=0.9999)范围内呈良好线性关系;平均回收率(n=6)分别为94.3%,98.0%,RSD分别为1.18%,2.26%。结论 该方法简便、灵敏、准确、高效,可用于颠茄片的质量控制。Objective To establish an ultra-fast liquid chromatography with tandem mass spectrometry(UPLC-MS-MS)method for simultaneous determination of two active components in Belladonna tablets(hyoscyamine sulfate,scopoletin).Methods Chromatographic separation was performed on a Waters Acquity UPLC HSS T3(2.1 mm ×100 mm,1.8μm).The mobile phase consisted of 0.1%formic acid in water-methanol B was subjected to gradient elution(0-1 min 10%B;1~4 min,10%B→90%B;4~6 min,90%B;6~6.2 min,90%,B→10%B;6.2~8 min,10%B)at a flow rate of 0.2 mL·min^(-1).The column temperature was maintained at 40 C,and injection volume was 4μL.Detection was performed with electrospray ionization source in positive and negative ionization mode.Quantifacantion was performed using multiple reactions moniroring(MRM)mode.Results The linear range of hyoscyamine sulfate and scopoletin were 193.6~968.0 ng mL-(r=0.9996)and 1.00~50.00 ng·mL^(-1)(r=0.9999).Whose average recoveries were 94.3%and 98.0%(n=6).The RSD were 1.18%and 2.26%.Conclusion The method is simple,sensitive,accurate and efficient.It can be used for the quality control of Belladonna tablets.

关 键 词：超高效液相色谱串联质谱法 颠茄片 硫酸天仙子胺 东莨菪内酯 

分 类 号：R284.2[医药卫生—中药学]