保健品中42种非法添加物的HPLC-MS/MS法快速筛选和测定

Rapid Screening and Determination of 42 Kinds of Illegally Added Substances in Health Care Products by HPLC-MS/MS

通过选择适宜色谱柱,优化色谱条件和质谱条件,建立了一种快速检测保健品中42种非法添加化学物质高效液相色谱-串联质谱法。样品中的目标物经甲醇萃取后,使用五氟苯基丙基色谱柱(100 mm×2.1 mm,5μm)分离,以乙腈、20 mmol/L乙酸铵和体积分数0.1%甲酸缓冲水溶液为流动相进行梯度洗脱,在电喷雾离子源正离子(ESI+)模式下,采用多反应监测模式测定及外标法定量。结果表明:该HPLC-MS/MS法可以准确快速测定保健品中42种非法添加化学物质,42种化学物质在10~1000 ng/mL浓度范围内线性关系良好,相关系数(r^(2))均大于0.99;检出限(LOD,S/N=3)和定量限(LOQ,S/N=10)分别为0.5~10 ng/g和1~50 ng/g;42种化学物质在空白基质中3个添加水平下的平均回收率为80.59%~136.76%,相对标准偏差为0.41%~13.44%。该方法操作简单,检测覆盖范围广、耗时少、准确度高,适用于保健品中非法添加化学物质的快速筛查和定量分析。

A high-performance liquid chromatography tandem mass spectrometry(HPLC-MS/MS)method for rapid detection of 42 kinds of illegally added substances in health care products was established by selecting suitable chromatographic column and optimizing chromatographic and mass spectrometry conditions.The targets were separated on a pentafluorophylpropyl column(100 mm×2.1 mm,5μm)with gradient elution using a mobile phase containing acetonitrile,20 mmol/L ammonium acetate and volume fraction 0.1%of formic acid buffer solution.Electrospray ionization mass spectrometry was performed in multiple reaction monitoring modes for determination of the targets.The results showed that the HPLC-MS/MS method can accurately and rapidly determine 42 kinds of illegally added substances in health care products.The linear relationship of 42 kinds of substances is good in the concentration range of 10-1000 ng/mL,and the correlation coefficients are greater than 0.99.The limit of detection(S/N=3)and limit of quantification(S/N=10)are 0.5-10 ng/g and 1-50 ng/g,respectively.The average recoveries are 80.59%-136.76%and the relative standard deviations are in the range of 0.41%-13.44%,which meets the requirements of analytical determination.The method is expected be used in rapid screening and quantitative analysis of illegally added substances in health care products with simple operation,wide detection coverage,less time consuming and high accuracy.