加速溶剂萃取-超高效液相色谱-串联质谱法测定婴幼儿配方乳粉中17种磺胺类药物残留

Determination of 17 sulfonamides in infant formula by accelerated extraction and ultra-high performance liquid chromatography/mass spectrometry

建立了加速溶剂萃取(ASE)-超高效液相色谱-串联质谱法(UHPLC-MS/MS)测定婴幼儿配方乳粉中17种磺胺类药物残留的方法,并对方法的线性、灵敏度、回收率及基质效应等进行验证分析,同时将该方法应用于市场采集的婴幼儿配方乳粉样品中磺胺类药物残留进行分析和确证。试验结果表明,17种磺胺类药物在0.5~100μg·kg^(-1)范围内呈线性,决定系数均大于0.998,不同添加浓度下的回收率为75.3%~103.6%,相对标准偏差(RSD)均小于11.0%,基质效应为0.4~1.0,检出限为0.1~3.0μg·kg^(-1),定量限为0.3~10μg·kg^(-1)。该方法具有萃取便捷、灵敏度和准确度高等特点,可同时对婴幼儿配方乳粉中17种磺胺类药物残留进行测定。

A method for the determination of 17 sulfonamides residues in infant formula by accelerated solvent extraction(ASE) and ultra-high performance liquid chromatography/mass spectrometry(UHPLC-MS/MS) was developed. The linearity, sensitivity, recovery rate and matrix effect of the method were verified. Meanwhile, the screening analysis for 17 sulfonamides in infant formula collected from the market was carried out. The results showed that the linearity of sulfonamides were in the range of 0.5-100 μg·kg^(-1), and the correlation coefficient was greater than 0. 998, the recoveries were 75.3%-103.6%, the relative standard deviation was less than 11.0%, the matrix effect was 0.4-1.0, the detection limit for sulfonamides in infant formula was 0.1-3.0 μg·kg^(-1), and the limit of quantification(LOQ) was 0.3-10 μg·kg^(-1). The developed method has the merits for convenient extraction, high sensitivity and accuracy, and the method can simultaneously determine 17 sulfonamides residues in infant formula.