QuEChERS试剂盒—超高效液相色谱串联质谱法同时检测畜禽肉中18种喹诺酮类兽药残留研究  

Simultaneous Determination of 18 Quinolone Residues in Livestock and Poultry Meat by QuEChERS Kit-UPLC/MS/MS

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

机构地区：[1]沈阳出入境检验检疫局,辽宁沈阳110016

出　　处：《畜牧与饲料科学》2016年第12期12-16,共5页Animal Husbandry and Feed Science

基　　金：沈阳市科技局项目(F15-168-4-00)

摘　　要：建立了一种同时测定畜禽肉中18种喹诺酮类兽药残留的QuEChERS试剂盒一超高效液相色谱串联质谱检测方法。样品经1％乙酸乙腈水溶液（20：80，V／V）振荡离心后，取上清液于净化管中净化，再取上清液浓缩至干，甲醇水溶液（甲醇：水=1：4）溶解残渣，过膜，待测。采用C18色谱柱（100mm×2．1mm，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、定量测定畜禽肉中18种喹诺酮类兽药残留。结果表明．18种喹诺酮类兽药在0．5～80ng／mL范围内线性关系良好，相关系数（r）均大于0．99；以5．0、10．0、50．0μg／kg3个浓度水平进行添加回收实验，18种喹诺酮类兽药的平均回收率在60．5％-97．0％，相对标准偏差为2．1％-19．5％，该方法的检出限为5．0μg／kg。该方法重现性好、灵敏度高、分析时间短、确证能力强，适用于畜禽肉中18种喹诺酮类兽药残留的同时检测。A QuEChERS Kit-UPLC/MS/MS method for simultaneously determination of 18 quinolone residues in livestock and poultry meat was developed in this study. The samples were oscillated and centrifuged in a 1% aqueous solution of acetic acid and acetonitrile （20：80, V/V）. The obtained supernatant was purified after transferring to purification pipe and was then concentrated to dry. The residues were dissolved in aqueous solution of methanol （methanol ：water=1：4） and were then filtered. The Cls chromatographic column （100 mm×2.1 mm, 1.7 μm） was used to isolate, and the 0.2% aqueous solution of formic acid and acetonitrile solution containing 0.2% formic acid were used as mobile phase to gradient elute. The 18 quinolone residues in livestock and poultry meat were qualitatively and quantitatively determined by UPLC/MS/MS. A good linear relationship of the 18 quinolone in the range of 0.5-80 ng/mL was observed, and the correlation coefficient （r） was all above 0.99. Recovery test was performed with three concentration levels of 5.0, 10.0, 50.0 μg/kg. The average recovery of the 18 quinolone ranged from 60.5% to 97.0%, the relative standard deviation ranged from 2.1% to 19.5%, and the detection limit of the method was 5.0 μg/kg. The developed method with good reproducibility, high sensitivity, short analysis time and strong ability of confirmation was suitable for the simultaneous determination of 18 quinolone residues in livestock and poultry meat.

关 键 词：畜禽肉 喹诺酮 QuEChERS试剂盒 液相色谱串联质谱 

分 类 号：S859.84[农业科学—临床兽医学]