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DISQUETM净化管净化,上清液经正己烷除去脂肪、样品浓缩后用BEH C18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1~50 μg/kg均有良好线性关系,相关系数(r2)均>0.99;样品中37种兽药的检出限均为0.5 μg/kg,定量限均为1.0 μg/kg;添加水平为1~20 μg/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 DISQUETM 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 C18 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 1-50 μg/kg. The average recoveries and relative standard deviations were 71%-104% and 3.1%-14.7% respectively in the spiked range of 1-20 μg/kg. The limits of detection were 0.5 μg/kg, and the limits of quantification were 1 μg/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.
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