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[摘要]
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,1.7 μm)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 mL/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 5~0.018 μg,定量限为0.004 5~0.55 μg,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。
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[Abstract]
Objective To establish a UPLC-MS/MS method for determination of 10 anti-rheumatic constituents illegally added in Chinese traditional medicine and health products preparation. Methods The column was ACQUITY UPLC BEHC18 (50 mm×2.1 mm, 1.7 μm), The mobile phase was acetonitrile -Ammonium acetate solution (containing 0.1% Acetic acid) with gradient elution at a flow rate of 0.3 mL/min. The ion source was electrospray ionization (ESI), Multiple-reaction monitoring (MRM) was performed to identify and quantify 10 anti-rheumatic constituents. Results 10 linear calibration curves were obtained with r ≥ 0.996 1. The recoveries were determinated at three concentration and ranged from 92.5% to 101.8%.The precision of the method was shown by RSD (n=5) ranged from 0.9% to 3.1%. The ranges of limit of detection were from 0.001 5 to 0.018 μg, and quantitation were from 0.004 5 to 0.55 μg. The illegally added chemicals were detected with 10 batches of 27 batches of samples. Conclusion The method were simple, sensitivity, accurate, and can be used to detect Anti-rheumatic constituents illegally added in Chinese traditional medicine and health products.
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