鸡肉和鸡蛋中5种利尿剂残留的超高液相色谱-串联质谱检测方法研究

Study of Detection Method for 5 Kinds of Diuretic Residues in Chicken and Eggs by UPLC-MS/MS

为了快速高效测定鸡肉和鸡蛋中5种利尿剂(卞氟噻嗪、氯噻嗪、氯噻酮、呋塞米、氢氯噻嗪)的残留量,样品经过乙腈试剂和萃取盐提取,用Bond Elut QuEChER净化柱净化,建立了一种超高液相色谱-串联质谱法(UPLC-MS/MS)方法。结果显示:5种利尿剂在1~200 ng/mL范围内具有良好的线性相关性,相关系数均大于0.99;建立的方法检测限在0.5~1.0μg/kg,定量限在1.5~2.0μg/kg;鸡蛋和鸡肉中5种利尿剂药物在2~200.0μg/kg添加范围内平均回收率在60.8%~108.7%,批内、批间相对标准偏差的范围为0.9%~11.4%。研究表明建立的UPLC-MS/MS方法操作方便、结果准确、高效、重现性好,符合兽药残留标准检测的相关要求,可用于禽产品利尿剂残留的快速检测。

A ultra high-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS) method was established for the rapid and efficient determination the residues of 5 kinds of diuretics(benzofluorothiazide, chlorothiazide,chlorothiazide, furosemide and hydrochlorothiazide) in chicken and egg. The samples were extracted by acetonitrile and extracted salt, purified by bond elut quencher column. The results showed that in the concentration range of 1 to 200 ng/mL,the chromatographic peak area of 5 kinds of diuretics showed good linear correlation, and the correlation coefficients were all higher than 0.99. The detection limit was 0.5 to 1.0 μg/kg with the quantitation limit of 1.5 to 2.0 μg/kg. The average recoveries of 5 kinds of diuretics ranged from 60.8% to 108.7% at the supplemental level of 2 to 200 μg/kg,and the relative standard deviations within and between batches ranged from 0.9% to 11.4%. The established UPLC-MS/MS method was simple, accurate, efficient and reproducible, which was in line with the relevant requirements of veterinary drug residue detection and could be used for the rapid determination of diuretics residues in poutry products.