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目的建立UPLC-MS/MS法检测中成药及保健品中非法添加的10种抗风湿类化学成分的含量。方法以ACQUITY UPLC BEHC18(50 mm×2.1 mm,1.7μm)为色谱柱,以含0.1%乙酸0.02 mol/L醋酸铵溶液-乙腈为流动相梯度洗脱,体积流量为0.3 m L/min;质谱采用电喷雾离子源(ESI),多反应监测(MRM)模式进行定性定量分析。结果 10种化学物质的质谱检测线性范围宽,线性关系良好,r≥0.996 1,平均方法回收率为92.5%~101.8%,RSD为0.9%~3.1%,检出限为0.001 5~0.018μg,定量限为0.004 5~0.55μg,27批样品中有10批样品检出了非法添加的化学物质。结论本方法操作简单,灵敏度高,结果准确,可作为抗风湿类中成药及保健品中非法添加化学物质的测定方法。
OBJECTIVE To establish a UPLC-MS / MS method for the determination of ten anti-rheumatic chemicals in Chinese patent medicines and health supplements. Methods The mobile phase consisted of ACQUITY UPLC BEHC18 (50 mm × 2.1 mm, 1.7 μm) and gradient elution with 0.1% acetic acid in 0.02 mol / L ammonium acetate as mobile phase. The mass flow rate was 0.3 m L / min. The electrospray ionization source (ESI) and multiple reaction monitoring (MRM) mode were used for qualitative and quantitative analysis. Results The linear range of the 10 chemical substances was linear and the linearity was good. The average recovery was 92.5% ~ 101.8%, RSD was 0.9% ~ 3.1%, the detection limit was 0.001 5 ~ 0.018μg, The limit of quantification was 0.004 5-0.55 μg. Ten batches of 27 batches of samples were tested for illicitly added chemicals. Conclusion The method is simple, sensitive and accurate. It can be used as a method for the determination of illegally added chemicals in Chinese medicines and health products.