补肾壮阳类中成药中15种非法添加化学药物的检测方法研究  

Study on the detection methods of 15 kinds of chemical drugs illegally added to kidney-tonifying and aphrodisiacal Chinese patent medicine

作　　者：朱泽兵 郭娅 张德伟 张华 ZHU Zebing;GUO Ya;ZHANG Dewei;ZHANG Hua(Chongqing Wanzhou Food and Drug Inspection Institute,Chongqing,404100,China;Chongqing Key Laboratory of development and utilization of Dao-di herbs in the Three Gorges Reservoir Area)

机构地区：[1]重庆市万州食品药品检验所,重庆万州404000 [2]三峡库区道地药材开发利用重庆市重点实验室

出　　处：《质量安全与检验检测》2024年第1期42-49,68,共9页QUALITY SAFETY INSPECTION AND TESTING

基　　金：重庆市药品监督管理局与重庆市科学技术局药品科研项目(渝药监〔2022〕2号)。

摘　　要：为了建立一种高效液相色谱-串联质谱检测补肾壮阳中成药中15种非法添加化学药物的方法。将试样经乙腈超声萃取,以0.1%甲酸水溶液-乙腈为流动相,通过液质色谱柱进行分离,并进行梯度洗脱,对15种化学物质进行测定。经检测15种化学物质在4.574~223.552 ng/mL范围内呈现出良好线性关系,相关系数(R^(2))均在0.996以上;平均回收率为84.6%~115.3%;精密度为0.14%~0.52%,RSD为0.66%~1.48%;检出限为0.024~0.334 ng/mL;定量限为0.072~1.002 ng/mL。该方法精确度高,灵敏度强,专属性好,检测下限低,可用于补肾壮阳一类中成药中15种非法添加化学药物的定性检测和含量检测。In order to establish a high performance liquid chromatography-tandem mass spectrometry(principle:four-stage bar-electrostatic field orbital ion trap)test method for the illegal addition of 15 kinds of chemical agents in tonifying kidney and aphrodisiacs.The samples were extracted by acetonitrile and separated with 0.1%formic acid-acetonitrile as mobile phase by liquid chromatographic column.Then 15 kinds of chemicals were determined by gradient elution.The standard curve linearity of 15 chemical substances was good in the range of 4.574-223.552 ng/mL,and the correlation coefficient(R^(2))was above 0.996.The average recovery rate was 84.6-115.3%.The precision was 0.14-0.52%,RSD was 0.66-1.48%.The detection limit was 0.024-0.334 ng/mL.The limit of quantification was 0.072-1.002 ng/mL.The method has high accuracy,strong sensitivity,good specificity and low detection limit.It can be used for qualitative detection and content detection of 15 illegal chemicals in tonifying kidney and strengthening Yang class of Chinese patent medicine.

关 键 词：补肾壮阳 中成药 非法添加 化学药物 高效液相色谱-串联质谱法 

分 类 号：R927.2[医药卫生—药学]