UPLC-MS/MS法测定中成药和保健食品中萘丁美酮等抗痛风类化学成分

Determination of anti-gout components nabumetone in traditional Chinese patent medicine and health-care food by UPLC-MS/MS

目的建立UPLC-MS/MS法同时测定中成药和保健食品中萘丁美酮等14种非法添加的化学成分。方法样品采用乙腈超声提取,以Agilent Poroshell 120 EC-C18(2.1 mm×100 mm,2.7μm)色谱柱分离,以含0.005 mol·L^(-1)甲酸铵的0.1%甲酸溶液-乙腈为流动相梯度洗脱,采用电喷雾离子源,正负离子扫描模式,多反应监测(MRM)模式检测14种抗痛风类化学成分。结果14种抗痛风类化学成分的线性关系良好,r均≥0.9990;定量限为0.004~0.053 mg·kg^(-1),检测限为0.001~0.016 mg·kg^(-1),精密度的RSD(n=6)为0.60%~3.9%,平均回收率为83.3%~109.3%。23批样品中共2批检出非法添加化学成分,其中1批检出酮咯酸氨丁三醇,另1批检出别嘌醇。结论该方法操作简便,选择性好、灵敏度高、准确度高,能够用于中成药和保健食品中非法添加抗痛风类化学成分的检测。

Objective To establish UPLC-MS/MS method to simultaneously determine 14 illegally added chemical components such as nabumetone in traditional Chinese patent medicine and health-care food.Methods The samples were extracted by acetonitrile ultrasound.The separation was conducted on Agilent Poroshell 120 EC-C18(2.1 mm×100 mm,2.7μm)chromatographic column with 0.1%formic acid solution containing 0.005 mol·L^(-1)ammonium formate-acetonitrile as the mobile phase in gradient elution.Totally 14 anti-gout chemical components were detected by electrospray ionization source in both positive and negative ion mode and multiple reaction monitoring(MRM)mode.Results The 14 anti-gout chemical components had good linearity with the correlation coefficients no less than 0.9990.The limit of quantitation ranged from 0.004 to 0.053 mg·kg^(-1),and detection ranged from 0.001 to 0.016 mg·kg^(-1).The RSD of precision of method(n=6)ranged from 0.60%to 3.9%,and the average recoveries from 83.3%to 109.3%.Two out of 23 batches of samples,detected illegal addition of chemical components:ketorolac tromethamine in one sample and allopurinol in the other.Conclusion The method is simple,selective,sensitive and accurate,and can be used to determine illegally added anti-gout chemical components in traditional Chinese patent medicine and health-care food.