HPLC-MS/MS法检测降压类中药制剂中非法添加的3种化学药品  

Determination of three illegally added chemical composition in antihypertensive traditional Chinese medicines by HPLC-MS/MS

作　　者：赵静 张禄 刘文博 裴晓芬 申国华 ZHAO Jing;ZHANG Lu;LIU Wenbo;PEI Xiaofen;SHEN Guohua(Institute of Drug Testing Technology,Shanxi Provincial Inspection and Testing Center,Taiyuan 030031,China)

机构地区：[1]山西省检验检测中心,药品检验技术研究所,太原030031

出　　处：《山西医科大学学报》2022年第11期1458-1463,共6页Journal of Shanxi Medical University

摘　　要：目的建立可以同时定性和定量检测降压类中药制剂中3种非法添加化学药品(曲克芦丁、美托拉宗、阿齐沙坦)的液相色谱-质谱联用(LC/MS)方法。方法首先采用高效液相色谱法(配DAD检测器)、SHISEIDO C_(18)(250 mm×4.6 mm,5μm)色谱柱对样品中的目标物进行初筛和含量测定,再采用液质联用方法对目标物进行结构确认。实验时采用Dikma Spursil C_(18)(150 mm×2.1 mm,3μm)色谱柱,乙腈和0.1%甲酸水溶液为流动相进行梯度洗脱。结果3种非法添加物(曲克芦丁、美托拉宗、阿齐沙坦)浓度在0.005~0.2 mg/ml范围内,峰面积与浓度呈良好线性关系,平均回收率分别为98.3%,98.8%,99.1%,均RSD≤1.0%(n=9)。结论该方法便捷、准确性高、专属性强,可作为分析检测降压类中药制剂或有辅助降压功能保健食品中3种非法添加物有效可行的方法。Objective To establish a method for simultaneously quantitative and qualitative determination of the three kinds of chemicals(troxrutin,metolazone,azisartan)illegally added in antihypertensive traditional Chinese medicine by liquid mass spectrometry(LC/MS).Methods The targets in samples were screened and determined by high performance liquid chromatography(HPLC)equipped with DAD detector using SHISEIDO C_(18)(250 mm×4.6 mm,5μm)column,and then the structures of the targets were confirmed by LC/MS,and the confirmation test was carried out on a Dikma Spursil C_(18) column(150 mm×2.1 mm,3μm),with acetonitrile and 0.1%formic acid solution as mobile phases for gradient elution.Results There was a good linear relationship between the areas and the concentrations of the three illegal additives(troxrutin,metolazone,azisartan)within the range of 0.005-0.2 mg/ml,and their average recoveries were 98.3%,98.8%,99.1%,respectively(RSD≤1.0%,n=9).Conclusion The method is convenient,accurate and specific,and can be used as an effective and feasible method for determining the three illegal additives in antihypertensive traditional Chinese preparations and health food with auxiliary antihypertensive function.

关 键 词：降压类中药制剂 非法添加化学药品 液质联用(HPLC-MS/MS) 

分 类 号：R286[医药卫生—中药学]