HPLC-MS/MS同时测定尿酸调节类中药及含中草药食品中22种非法添加药物

Simultaneous Determination of 22 Illegally Drugs Added in Uric Acid Regulating Traditional Chinese Medicine and Chinese Herbal Food by HPLC-MS/MS

关键词:  尿酸  高效液相-串联质谱法  中药  中草药食品  非法添加

Key words:  uric acid  hplc-ms/ms  traditional Chinese medicine  chinese herbal food  illegal addition

摘要:

目的 采用高效液相色谱-串联质谱法同时测定尿酸调节类中药及含中草药食品中22种非法添加药物。方法 样品经含0.1%氨水的甲醇超声提取后,采用Agilent Poroshell 120 Bonus-RP(2.1 mm×100 mm,2.7 μm)色谱柱进行分离,以甲醇-乙腈(1:1)和0.005 mol·L^-1甲酸铵溶液为流动相梯度洗脱。采用电喷雾离子源正、负离子模式,以多反应监测扫描方式检测。结果 22种药物在10.0~200 μg·L^-1内线性关系良好,相关系数r²均>0.99,检测限和定量限分别为0.125~0.750 mg·kg^-1和0.416~2.81 mg·kg^-1,平均回收率为80.2%~120.1%,RSD为1.1%~5.9%。收集的37批样品中均未检出非法添加的药物。结论 该方法操作简单、快速、灵敏度高,可实现同时检测尿酸调节类中药及含中草药食品中22种非法添加药物。

Abstract:

OBJECTIVE To simultaneous determine 22 illegally drugs added in uric acid regulating traditional chinese medicine and chinese herbal food by HPLC-MS/MS. METHODS The samples were extracted by methanol mixed with 0.1% ammonium hydroxide and separated on an Agilent Poroshell 120 Bonus-RP column(2.1 mm×100 mm, 2.7 μm), with methanol-acetonitrile(1:1) and 0.005 mol·L^-1 ammonium formate as mobile phases by gradient elution. The analytes were detected by electrospray ionization source in the positive or negative mode and the multiple reaction monitoring mode. RESULTS the calibration curves for 22 drugs were linear in the range of 10.0-200 μg·L^-1 with their correlation coefficients r²>0.99, the limits of detection and quantitation were in the ranges of 0.125-0.750 mg·kg^-1 and 0.416-2.81 mg·kg^-1 respectively. The average recoveries were in the ranges of 80.2%-120.1%, with RSDs of 1.1%-5.9%. Illegal added drugs were not found in 37 tested practical samples. CONCLUSION The established method is simple, rapid and sensitive, and can be used for the simultaneous of determination of 22 illegally drugs added in uric acid regulating traditional Chinese medicine and Chinese herbal food.