QuEChERS-超高效液相色谱-串联质谱法同时测定保健食品中21种非法添加化学药物

Determination of 21 illegally added chemical drugs in health foods using ultra performance liquid chromatography-tandem mass spectrometry coupled with QuEChERS

建立了QuEChERS-超高效液相色谱-串联质谱测定改善睡眠类和提高免疫力类保健食品中21种非法添加化学药物的分析方法。口服液、保健酒分别用乙腈和乙腈-水-甲酸(60∶39∶1,v/v/v)振荡提取,QuEChERS法净化;采用Acquity UPLCTMBEH C18色谱柱(50 mm×2.1 mm,1.7μm)分离,以乙腈和2 mmol/L乙酸铵溶液(含0.1%(v/v)甲酸)为流动相进行梯度洗脱;在电喷雾离子源正离子模式(ESI+)下电离,多反应监测(MRM)模式检测。结果表明,21种化学药物在1~100μg/L范围内线性关系良好,相关系数(R2)均≥0.992,检出限(LOD)为0.07~3.41μg/kg,定量限(LOQ)为0.22~11.36μg/kg。3种加标水平(10、20和100μg/kg)下,21种化学药物在口服液和保健酒中的平均加标回收率分别为61.4%~116.5%和67.4%~98.4%;相对标准偏差(RSD)分别为0.2%~13.4%和0.2%~11.8%。该法简便,灵敏性高,实用性强,可用于改善睡眠和提高免疫力类保健食品中21种非法添加化学药物的检测。

A method for the simultaneous determination of21illegally added chemical drugs inimproving sleep and immunity health foods using ultra performance liquid chromatography tandem mass spectrometry(UPLC-MS/M S)was developed.Oral liquid and health wine samples were shaken with acetonitrile and acetonitrile-water-formic acid(60:39:1,v/v/v),respectively,then purified by QuEChERS method.The extracts were separated on an Acquity UPLCTM BEH C18column(50mmx2.1mm,1.7pm)with gradient elution of acetonitrile and2mmol/L ammonium acetate solution containing0.1%(v/v)formic acid as mobile phases.The electrospray ionization in positive ion mode was used for analysis in multiple reaction monitoring(MRM)mode.The results showed that the target drugs had a good linear relationship in the range of1-100pg/L with the correlation coefficients(R2)≥0.992.The limits of detection(LODs)and limits of quantification(LOQs)were0.07-3.41pg/kg and0.22-11.36pg/k g,respectively.The average recoveries of the21chemical drugs in oral liquid and health winewere in the range of61.4%-116.5%and67.4%-98.4%with the relative standard deviations(RSDs)of0.2%-13.4%and0.2%-11.8%,respectively.The developed method is sensitive andreliable.It has been successfully used for the detection of illegally added chemical drugs in real samples.