UPLC-MS-MS法同时测定鸡肉食品中37种兽药残留  

Determination of 37 veterinary residues in chickenby QuEChERS-UPLC-MS-MS

作　　者：黄华 谢文东 谷雨 孟照琦 孙元洁 杜洪淼[1] 孙娅娜[1] 康帅 HUANG Hua;XIE Wendong;GU Yu;MENG Zhaoqi;SUN Yuanjie;DU Hongmiao;SUN Yana;KANG Shuai(Beijing Products Quality Supervision and Inspection Institute,Beijing 101300,China)

机构地区：[1]北京市产品质量监督检验院,北京101300

出　　处：《食品与发酵工业》2022年第13期290-295,I0004,共7页Food and Fermentation Industries

摘　　要：建立了一种全新的以QuEChERS法为样品前处理技术以及结合超高效液相色谱法-串联质谱法(ultra high performance liquid chromatography-tandem mass spectrometry,UPLC-MS-MS)法快速测定鸡肉37种兽药残留的方法。样品经甲醇-乙腈混合溶液提取并通过DISQUE^(TM)净化管净化,上清液经正己烷除去脂肪、样品浓缩后用BEH C_(18)色谱柱分离,以甲醇和5 mmol/L醋酸铵(含0.1%甲酸水溶液)为流动相进行梯度洗脱,电喷雾正/负离子模式同时电离,多反应监测模式检测,外标法定量。结果表明,目标物在1~50μg/kg均有良好线性关系,相关系数(r^(2))均>0.99;样品中37种兽药的检出限均为0.5μg/kg,定量限均为1.0μg/kg;添加水平为1~20μg/kg的平均回收率为71%~104%,相对标准偏差为3.1%~14.7%。该方法具备快速、简便、准确性高、通用性强等特点,适合鸡肉食品中37种药物残留的定性定量检测。A method for the simultaneous determination of 37 veterinary residues in chicken by QuEChERS and UPLC-MS-MS was developed in this study.The sample was supersonically extracted with methanol-acetonitrile(2∶1)by DISQUE^(TM) extraction tube,the supernatant liquid was defatted with n-hexane,then dried under nitrogen stream and redissolved with acetonitrile-ammonium acetate(1∶9).The separation of the target objects was performed on the Waters Acquity UPLC BEH C_(18) column using methanol-0.05mmol/L ammonium acetate solution(0.1%formic acid)as a gradient elution.The identification and external standard method quantification were achieved by using electrospray ionization in positive ion mode(ESI^(+))with multiple reaction monitoring(MRM).The matrix-matched internal standard calibration curves were used for quantification determination.The linear range was from 1-50μg/kg.The average recoveries and relative standard deviations were 71%-104%and 3.1%-14.7%respectively in the spiked range of 1-20μg/kg.The limits of detection were 0.5μg/kg,and the limits of quantification were 1μg/kg for 37 veterinary residues.The method is rapid,simple,sensitive and accurate.It is suitable for the quantitative determination and confirmation of sulfonamide,quinolone,benzimidazole,tetracycline,macrolide and penicillin.

关 键 词：QUECHERS UPLC-MS-MS 磺胺 喹诺酮 苯并咪唑 四环素 大环内酯 青霉素 

分 类 号：O657.63[理学—分析化学] TS251.55[理学—化学]