高效液相色谱-串联质谱法测定凉茶中19种非法添加药物
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摘要
液态凉茶采用甲醇-乙腈(1:1,V/V)超声提取,经过简单的稀释和过滤,经C_(18)色谱柱分离,以甲醇-0. 5%甲酸水溶液为流动相进行梯度洗脱,电喷雾正离子模式电离,多反应监测模式检测,标准曲线法定量。19种药物在10～200μg/L线性关系良好,相关系数均大于0. 9963,加标浓度为20,50,100μg/L,平均回收率在69. 6%～117. 8%,相对标准偏差(RSD)在0. 92%～13%,检出限(LOD)在0. 2～5. 0μg/L。方法适用于凉茶等植物型饮料中非法添加化学药物的快速测定。
A high performance liquid chromatography tandem mass spectrometry( HPLC-MS/MS)method was developed for simultaneous determination of 19 kinds of illegally added chemical substances in herbal tea. The liquid herbal tea was extracted by methanol acetonitrile( 1: 1,V/V).After simple dilution and filtration,it was separated on C_(18) column with the mibile phase of aqueous solution of methanol-0. 5% formic acid was used as the mobile phase for gradient elution. The determination was carried out on mass spectrometer with electrosprayion source in the positive mode and monitored by the multiple reaction monitoring( MRM) mode. The samples were quantified by the matrixmatched calibration curves. The 19 drugs showed good linearity in the range of 10 ～ 200 μg/L with the correlation coefficients( r) higher than 0. 9963 at the spiked levels of 20,50,100 μg/L. The average recoveries were in the range of 69. 6% ～ 117. 8% with the relative standard deviations in the range of0. 92% ～ 13%. The limits of detection of the method were between 0. 2 and 5. 0 g/L. The method is suitable for the rapid determination of illegal chemical drugs in herbal beverages such as herbal tea.
A high performance liquid chromatography tandem mass spectrometry( HPLC-MS/MS)method was developed for simultaneous determination of 19 kinds of illegally added chemical substances in herbal tea. The liquid herbal tea was extracted by methanol acetonitrile( 1: 1,V/V).After simple dilution and filtration,it was separated on C_(18) column with the mibile phase of aqueous solution of methanol-0. 5% formic acid was used as the mobile phase for gradient elution. The determination was carried out on mass spectrometer with electrosprayion source in the positive mode and monitored by the multiple reaction monitoring( MRM) mode. The samples were quantified by the matrixmatched calibration curves. The 19 drugs showed good linearity in the range of 10 ～ 200 μg/L with the correlation coefficients( r) higher than 0. 9963 at the spiked levels of 20,50,100 μg/L. The average recoveries were in the range of 69. 6% ～ 117. 8% with the relative standard deviations in the range of0. 92% ～ 13%. The limits of detection of the method were between 0. 2 and 5. 0 g/L. The method is suitable for the rapid determination of illegal chemical drugs in herbal beverages such as herbal tea.
引文
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