摘要
目的建立中药酒剂中24种毒性成分的超高效液相色谱串联质谱快速检验方法。方法样品采用0.5%氨水甲醇直接1∶1稀释,采用Shim-pack GISS C_(18)色谱柱(100 mm×2.1 mm,1.9μm)进行分离,以乙腈-5 mmol·L^(-1)乙酸铵水溶液为流动相梯度洗脱,在电喷雾正离子模式下以多反应监测(MRM)方式测定。结果24个待测指标在相应的质量浓度范围内线性关系良好,相关系数r均大于0.99。检测限为0.3~0.5 ng·mL^(-1),定量限为0.9~1.3 ng·mL^(-1),3个加标水平下的平均回收率为79.6%~107.0%,相对标准偏差(RSD)为5.3%~17.0%。结论该方法前处理简便,高效,灵敏度高,选择性好,适用于中药酒剂中毒性成分的检测及安全性评价。
OBJECTIVE To develop a method for the determination of 24 toxic compounds in traditional Chinese medicine wine using ultra-performance liquid chromatography coupled to triple quadrupole mass spectrometry(UPLC-MS/MS).METHODS The samples were double diluted with 0.5%ammonia methanol(v/v),performed on a Shim-pack GISS C_(18) column(100 mm×2.1 mm,1.9μm)with isocratic elution of acetonitrile and 5 mmol·L^(-1) ammonium acetate.Electrospray ionization(ESI)source was applied by positive ionization in multiple reaction monitoring(MRM)modes.RESULTS All the 24 kinds of targets had good linear relationship,with correlation coefficients above 0.99.The limits of detections(LODs)were 0.3-0.5 ng·mL^(-1),and the limits of quantifications(LOQs)were 0.9-1.3 ng·mL^(-1).The average recoveries at three levels for all target were in the range of 79.6%-107.0%,with RSD of 5.3%-17.0%.CONCLUSION The method has the advantages of fast and simple sample pretreatment,high detection sensitivity and good selectivity,and is suitable for the rapid analysis of toxic compounds in traditional Chinese medicine wine and security elevation.
作者
李纯
朱照兰
栗建明
侯惠婵
LI Chun;ZHU Zhaolan;LI Jianming;HOU Huichan(NMPA Key Laboratory for Quality Evaluation of Traditional Medicine,Guangzhou Institute for Drug Control,Guangzhou,Guangdong 510160,China)
出处
《今日药学》
CAS
2023年第6期425-430,共6页
Pharmacy Today
基金
广州市科技计划项目(20212210005)
广州市市场监督管理局科技项目(2021KJ41)。
