作者：辜慧, 杜钢, 李澍才, 张媛媛
作者单位：四川省食品检验研究院， 四川 成都 611731
关键词：超高效液相色谱-串联质谱(UPLC-MS/MS);中药制剂;非法添加;化药成分
摘要：
该文建立UPLC-MS/MS法同时检测减肥类、壮阳类、降糖类、解热镇痛类中药制剂中易被添加的27种化药成分。样品用甲醇提取，采用Agilent Eclipse Plus C18 RRHD色谱柱（3.0 mm×150 mm，1.8 μm）分离，以0.1%甲酸水溶液和乙腈为流动相，梯度洗脱，流量0.5 mL/min，柱温35 ℃，进样体积1 μL，采用电喷雾离子源（ESI），正离子模式，多反应监测（MRM）进行检测。所测27种非法添加化药成分在一定范围内呈良好的线性关系（r2>0.99），各组分均分离良好，低、中、高3个添加水平的平均回收率为80.4%~120.9%，相对标准偏差(relative standard deviation, RSD)为0.8%~7.8%，检出限
Determination of 27 chemicals added illegally in traditional chinese medicines by UPLC-MS/MS
GU Hui, DU Gang, LI Shucai, ZHANG Yuanyuan
Sichuan Institute for Food Control, Chengdu 611731, China
Abstract: To establish an UPLC-MS/MS method for simultaneous determination of 27 chemicals easily added illegally in traditional chinese medicines which were prepared for weight loss, aphrodisiac, antidiabetic, antipyretic and analgesic. Samples were extracted by methanol. The analysis was performed on Agilent Eclipse Plus C18 RRHD (3.0 mm×150 mm, 1.8 μm) column with gradient elution using a mobile phase of 0.1% aqueous formic acid and acetonitrile at 0.5 mL/min, the column temperature was 35 ℃ and the injected sample solution volume was 1 μL. Mass spectrometry acquisition was done in the positive ion mode and analytes were detected in the MRM mode. 27 chemicals added illegally could be separately well and have a good linear relationship in a certain range (r2>0.99). The average recovery rates of low, medium and high concentration were 80.4%-120.9% with the relative standard deviation (RSD) of 0.8%-7.8%. The qualitative and quantitative limits were within the range of
-
μg/g and
-
μg/g. This method has the advantages of high specificity, high sensitivity and simple operation, which therefore can be applied for the analysis of 27 chemicals added illegally in traditional chinese medicines.
Keywords: ultra-high pressure liquid chromatography-tandem mass spectrometry;traditional chinese medicines;added illegally;chemicals
2021, 47(7):49-54 收稿日期: 2021-03-16;收到修改稿日期: 2021-04-21
基金项目:
作者简介: 辜慧(1988-),女,四川成都市人,主管药师,硕士,主要从事食品药品质量研究;杜钢(1977-),男,四川乐山市人,副主任药师,博士,主要从事食品药品质量研究
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