SinChERS结合超高效液相色谱-串联质谱法同时测定禽类产品中磺胺类药物及其增效剂  

Simultaneous determination of sulfonamides and sulfonamide potentiators residues in poultry products by SinChERS combined with ultra performance liquid chromatography-tandem mass spectrometry

作　　者：乔颖 刘雪红 韩凤丽 袁奎敬 侯颖 孙进健 李俊[2] 葛祥武 QIAO Ying;LIU Xue-Hong;HAN Feng-Li;YUAN Kui-Jing;HOU Ying;SUN Jin-Jian;LI Jun;GE Xiang-Wu(Dalian Center for Food and Drug Control and Certification,Dalian 116037,China;Institute of Feed Research of Chinese Academy Agricultural Sciences,Beijing 100081,China)

机构地区：[1]大连市检验检测认证技术服务中心,大连116037 [2]中国农业科学院饲料研究所,北京100081

出　　处：《食品安全质量检测学报》2021年第23期9063-9070,共8页Journal of Food Safety and Quality

摘　　要：目的建立SinChERS结合超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry,UPLC-MS/MS)同时测定禽类产品中磺胺类药物及其增效剂的分析方法。方法样品经甲酸乙腈提取后,经基质分散净化装置(SinChERS)净化,采用Agilent SB RRHD C_(18)色谱柱(100 mm×2.1 mm,1.8μm)进行分离,以0.1%甲酸水溶液和0.1%甲酸乙腈溶液为流动相进行梯度洗脱,质谱采集采用电喷雾正离子模式,通过多反应监测(multiple reaction monitoring,MRM)方式检测。结果磺胺类药物及其增效剂在1~50μg/L浓度范围内线性关系良好,相关系数(r^(2))为0.9994~0.9999。在1.0、2.0、10.0μg/kg 3个添加水平下,其平均回收率均在70.2%~99.5%之间,相对标准偏差(relative standard deviations,RSDs)均小于等于8.6%,方法定量限为1.0μg/kg。结论该方法快速简便、准确可信、灵敏度高,适合禽类产品中磺胺类药物及其增效剂的残留检测。Objective To establish a method for the simultaneous determination of sulfonamides and sulfonamide potentiators residues in poultry products by SinChERS combined with ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).Methods The samples were extracted by formic acid-acetonitrile,purified by a novel pressing of the SinChERS packing column,separated by Agilent SB RRHD C_(18) column(100 mm×2.1 mm,1.8μm)with 0.1% formic acid-water and 0.1% formic acid-acetonitrile as mobile phases for gradient elute,then analyzed by UPLC-MS/MS.The determination was carried out with electrospray ion source under the positive ion mode and multiple reaction monitoring(MRM)mode.Results The calibration curves of the sulfonamides and sulfonamide potentiators showed an excellent linearity in the range of 1-50μg/L,the correlation coefficient(r^(2))were between 0.9994 and 0.9999.The average recoveries were between 70.2%-99.5% at 3 spiked levels of 1.0,2.0 and 10.0μg/kg.The relative standard deviations(RSDs)were less than or equal to 8.6%.The limits of quantitation for the sulfonamides and sulfonamide potentiators were 1.0μg/kg.Conclusion The proposed method is efficient,reliable and sensitive,which can be used for the detection of sulfonamides and sulfonamide potentiators residues in poultry products.

关 键 词：SinChERS 超高效液相色谱-串联质谱法 禽类产品 磺胺类药物 磺胺增效剂 

分 类 号：O657.63[理学—分析化学] TS251.7[理学—化学]