超高效液相色谱-串联质谱法测定凉茶中3种非法添加的解热镇痛药物

Determination of 3 kinds of illegally added antipyretic and analgesic drugs in herbal tea by ultra performance liquid chromatography-tandem mass spectrometry

目的建立超高效液相色谱-串联质谱法测定凉茶中3种非法添加解热镇痛药(阿司匹林、布洛芬、吲哚美辛)的分析方法。方法样品经0.1%(V:V)甲酸-甲醇超声提取后,以乙酸铵-乙腈为流动相进行梯度洗脱。采用多反应监测模式监测(multiple reaction monitoring,MRM),负离子模式扫描,外标法进行定量检测。结果3种待测化合物在相应的线性范围内线性关系良好,相关系数大于0.997;检出限范围为0.01~0.04 mg/kg,定量限范围为0.03~0.14 mg/kg。在3个添加水平下,3种化合物的平均回收率为94.5%~102.0%,相对标准偏差为2.37%~8.86%(n=6)。结论该方法简单、重复性好、灵敏度高,适用于凉茶中阿司匹林、布洛芬、吲哚美辛非法添加的检测。

Objective To establish a method for the determination of 3 kinds of illegally added antipyretic and analgesic drugs(aspirin,ibuprofen and indomethacin)in herbal tea by ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).Methods The samples were extracted by 0.1%(V:V)formic acid methanol,and then eluted by gradient with ammonium acetate acetonitrile as mobile phase.The samples were monitored by multiple reaction monitoring mode(MRM),scanned by negative ion mode,and quantitative detected by external standard method.Results The 3 compounds showed good linear relationships in the corresponding linear ranges with all the correlation coefficients greater than 0.997.The limits of detection were 0.01-0.04 mg/kg,and the limits of quantitation were 0.03-0.14 mg/kg.Under the 3 addition levels,the average recoveries of 3 compounds were 94.5%-102.0%,and the relative standard deviations were 2.37%-8.86%(n=6).Conclusion This method is simple,reproducible and sensitive,which can be used for detection of aspirin,ibuprofen and indomethacin illegally added in herbal tea.