HPLC-MS/MS法测定动物源食品中7种磺胺类药物残留

Determination of Seven Sulfonamides Residues in Food of Animal Origin by HPLC-MS/MS

建立了超高效液相色谱-串联质谱法(High Performance Liquid Chromatography-tandem Mass Spectrometry,PLC-MS/MS)测定动物源食品中7种磺胺类药物残留的检测方法。样品经过80%乙腈水(含0.2%甲酸)提取、Prime HLB固相萃取柱净化,滤膜过滤后,采用InfinityLab Poroshell 120 EC-C_(18)(2.1 mm×100 mm,1.9μm)色谱柱分离,以甲醇和5 mmol/L乙酸铵0.1%甲酸水为流动相梯度洗脱,采用多反应检测方式和正离子扫描方式检测,以外标法定量。结果表明,7种磺胺类药物在10~200 ng/mL范围内有良好的线性关系,相关系数均大于0.9991,检出限为2.5μg/kg,定量限为9.0μg/kg;在20,80,160μg/kg 3个加标水平上4种样品基质的平均回收率为66.3%~104.3%,相对标准偏差(RSD,n=6)为0.2%~5.5%。该方法操作简便、灵敏度高、重现性好,适用于动物源食品中磺胺残留的测定。

A High Performance Liquid chromatography-tandem Mass Spectrometry(HPLC-MS/MS)method was developed for the determination of seven sulfonamides residues in food of animal origin.The samples were extracted with 80%acetonitrile water(containing 0.2%formic acid),purified with Prime HLB SPE column,filtered with membrane,and separated on an Infinity Lab Poroshell 120 EC-C_(18)(2.1 mm×100 mm,1.9μm)column.Methanol and 5 mmol/L ammonium acetate 0.1%formic acid water were used as mobile phase for gradient elution.Multiple reaction detection method and positive ion scanning method were used for detection.The quantitative analysis was performed by external standard method.The results showed that the seven sulfonamides had good linear relationships in the range of 10~200 ng/mL,and the correlation coefficients were all greater than 0.9991.The limit of detection was 2.5μg/kg,and the limit of quantification was 9.0μg/kg.The average recoveries at the spiked levels of 20,80 and 160μg/kg ranged from 66.3%to 104.3%,with relative standard deviations(RSD,n=6)ranging from 0.2%to 5.5%.The method was simple,sensitive and reproducible.It was suitable for the determination of sulfonamide residues in food of animal origin.