鸡肉鸡肝中20种磺胺类兽药残留的测定——QuEChERS-超高效液相色谱串联质谱法  

Determination of 20 Sulfonamides Residues in Chicken and Chicken Liver-QuEChERS-UPLC-MS/MS

作　　者：赵颖[1] 李晓东[1] 姜玲玲[1] 刘瑜[1] 金雁[1] 徐宜宏[1] 吴渺渺 

机构地区：[1]沈阳出入境检验检疫局,辽宁沈阳110016

出　　处：《当代畜牧》2016年第11期44-46,共3页Contemporary Animal Husbandry

基　　金：沈阳市科技局项目(F15-168-4-00)

摘　　要：笔者建立了一种同时测定鸡肉及鸡肝中20种磺胺类兽药残留的Qu ECh ERS-超高效液相色谱串联质谱检测方法。样品经1%的乙酸乙腈水溶液(20/80,V/V)提取,振荡离心后,取上清液于Qu ECh ERS净化管中净化,取净化液,浓缩至干,甲醇水溶液(甲醇∶水=1∶4)溶解残渣,过膜,待测。采用C18色谱柱(2.1 mm×100 mm,1.7μm)分离,以0.2%甲酸水溶液和0.2%甲酸乙腈溶液作为流动相进行梯度洗脱,UPLC-MS/MS法同时定性、定量测定鸡肉和鸡肝中20种磺胺类兽药残留。20种磺胺类兽药在0.5 ng/m L^80 ng/m L范围内线性关系良好,相关系数(r)均大于0.99μg/kg。以5μg/kg、10μg/kg和50μg/kg 3个浓度水平进行添加回收实验,20种磺胺类兽药的平均回收率在64.4%~108.0%之间,相对标准偏差为2.6%~19.0%,方法的定量限为5μg/kg。方法重现性、灵敏度高,分析时间短,确证能力强,适用于鸡肉及鸡肝中20种磺胺类兽药残留的同时检测。A method for simultaneous determination of 20 sulfonamides residues in chicken and chicken liver by QuEChERS-UPLC- MS/MS. Samples were extracted with 1% acetic acid in acetonitrile, and the extraction was centrifuged and purified in QuEChERS kit, separated on a Cis column （2.1 mm×100 mm, 1.7 μm）. The determination of 20 sulfonamides residues in chicken and chicken livers by UPLC-MS/MS was carried out by gradient elution with 0.2% formic acid in water and 0.2% formic acid in acetonitrile as mobile phase. The correlation coefficients （r） of the 20 sulfonamides residues in the range of 0.5 ng/mL^80 ng/mL were all better than 0.99. The addi- tion and recovery experiments were carried out at the concentration of 5 μg/kg, 10 μg/kg, 50 μg/kg, The average recoveries of 20 sulfon- amides were 64.4%~108.0%, the relative standard deviations were 2.6%-19.0%. The limit of quantitation was 5 μg/kg. The repro- ducibility, high sensitivity, short analysis time and strong confirmation ability were suitable for the simultaneous determination of 20 sul- fonamides residues in chicken and chicken livers.

关 键 词：鸡肉 鸡肝 磺胺药残留 液相色谱串联质谱 

分 类 号：S859.84[农业科学—临床兽医学]