组织研磨-QuEChERS-高效液相色谱-串联质谱法测定动物源食品中磺胺类药物残留以及基质效应的研究

建立起组织研磨-QuEChERS-高效液相色谱-串联质谱法测定动物源食品中磺胺类药物残留的分析检测方法。样品用EDTA缓冲液溶解后,通过组织研磨仪高速处理样品,以乙腈提取目标化合物,经Bond QuEChERS提取、QuEChERS EMR-Lipid 净化,使用三重四极杆液质联用仪进行分析。C₁₈色谱柱分离,0.1%甲酸-乙腈梯度洗脱,外标法定量。结果表明,10种磺胺在一定浓度范围内线性关系良好,决定系数(R²)均大于0.99,目标化合物检出限(S/N=3)为0.2 μg/kg,定量限(S/N=10)为0.5 μg/kg。方法平均回收率为89.4%~111.0%,相对标准偏差(n=6)为0.8%~4.9%,该方法操作简单,回收率高,适用于动物源食品中磺胺类药物残留的测定。低质量浓度的磺胺类药物在猪肉、牛奶、鸡蛋中均存在明显基质效应,采用基质匹配标准曲线校正法可以对基质效应产生的影响进行补偿与消除。

Determination of Sulfonamides in Animal-originated Foods by Grinder-QuEChERS-High Performance Liquid Chromatography-Tandem Mass Spectrometry and Research on Matrix Effects

A method based on grinder-QuEChERS coupled with high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)was developed for the determination of ten sulfonamides residues in animal-originated food.After mixing with EDTA,the sample was grinded,extracted with acetonitrile and Bond QuEChERS,purified by QuEChERS EMR-Lipid,analysed by HPLC-MS/MS.The separation of sulfonamides was carried out on a C18 column with a gradient elution of 0.1%acetate and acetonitrile.The results showed that,the 10 kinds of sulfonamides had a good linear relationship in a certain concentration range with correlation coefficients(R2)greater than 0.99.The limits of detection(S/N=3)were 0.2μg/kg,the limits of quantitation(S/N=10)were 0.5μg/kg.The average recoveries of sulfonamides were 89.4%~111.0%and the relative standard deviations(RSDs)were 0.8%~4.9%.The method with a simple operation and a high recovery was suitable for the determination of 10 sulfonamides in animal-originated food.Furthermore,matrix-matched calibration curve could be used to compensate or eliminate the matrix effects in analysis of low concentration sulfonamides in swine,milk and egg samples.