QuEChERS-高效液相色谱-串联质谱法联用测定鸡肉中磺胺类药物残留

Determination of sulfonamides residues in chicken by QuEChERS combined with high performance liquid chromatography-tandem mass spectrometry

目的建立QuEChERS-高效液相色谱-串联质谱法测定鸡肉中磺胺类药物残留量的分析方法。方法以乙腈为提取溶剂,氯化钠盐析分层,离心后上清液经C18填料萃取净化,用乙腈和0.1%(V:V)甲酸水溶液作为流动相进行梯度洗脱,Endeavorsil C18柱色谱柱进行色谱分离,在高效液相色谱-串联质谱仪上采用电喷雾正离子扫描模式(electrospray ionization,ESI+)检测,外标法定量。结果该方法在5~200μg/L范围内有良好的线性关系,8种磺胺类药物残留的相关系数均大于0.99,方法检出限在3~6μg/kg范围,定量限在10~20μg/kg范围。分别在3个浓度水平20、100、300μg/kg加标,平均回收率在75.6%~115.2%范围,相对标准偏差在1.9%~12.4%范围。结论本方法操作简便,准确度和精密度好,可快速检测鸡肉中磺胺类药物的残留量。

Objective To establish an analytical method for the determination of sulfonamides in chicken by QuEChERS combined with high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS).Methods The sulfonamides were extracted with acetonitrile,and salting out stratification by sodium chloride.C18 purification material was applied to purify the supernatant after centrifugation,and separated by Endeavorsil C18 chromatogaphic column with gradient elution of acetonitrile and 0.1%(V:V)famic acid solution.The target was determined by electrospray positive ion scanning mode(electrospray ionization,ESI+)with HPLC-MS/MS,and quantified by the external standard method.Results The good linear relationship was in the range of 5~200μg/L for analyte,and the correlation coefficient square of the 8 kinds of sulfonamides residues was greater than 0.99.The limit of detection(LOD)for sulfonamides was 3~6μg/kg,and limit of quantitation(LOQ)was 10~20μg/kg.Three kinds of concentrations were labeled 20,100 and 300μg/kg,respectively,the average recoveries were 75.6%~115.2%,and the relative standard deviation(RSD)was 1.9%~12.4%.Conclusion This method is easy to operate,accurate and precise.The residue of sulfonamides in chicken can be detected quickly.