动物源性产品中10种利尿剂残留的超高液相色谱-串联质谱检测方法的研究

Establishment of a method for determining ten diuretic residues in animal derived products by ultra-high liquid chromatography-tandem mass spectrometry

建立了一种超高效液相色谱-串联质谱法(ultrahigh-performance liquid chromatography-tandem mass spectrometry,UPLC-MS/MS)对鸡蛋、鸡肉、猪肉、牛肉中10种利尿剂类药物(精磺胺、乙酰唑胺、苄氟噻嗪、坎利酮、氯噻嗪、氯噻酮、呋塞米、氢氯噻嗪、螺内酯、氨苯蝶啶)残留量的同步测定的方法。样品经乙腈和萃取盐提取,Captiva EMR-Lipid柱净化,超高效液相色谱-串联质谱仪测定,基质标准曲校正,外标法定量。10种利尿剂类药物在1~200 ng/mL的浓度范围内呈线性相关,相关系数均大于0.99;本方法的检测限为0.5~1.0μg/kg、定量限为1.5~2.0μg/kg;4种基质中10种利尿剂类药物在2~200.0μg/kg添加水平内的平均回收率在60.0%~112.8%之间,批内、批间相对标准偏差均在0.8%~13.5%之间。本研究建立的UPLC-MS/MS方法简便、准确、重现性良好,可作为动物源性产品中利尿剂残留快速检测的方法。

A method of Ultrahigh-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)was developed in this study for the simultaneous determination of ten diuretic residues(sulfonamide,acetazolamide,benzfluorothiazide,canidone,chlorothiazide,chlorothiazone,furosemide,hydrochlorothiazide,spirolactone,terteridine)in eggs,chicken,pork and beef.The samples were extracted by acetonitrile and extracted salt,and purified by the Captiva EMR-lipid column.The filtrate was determined by UPLC-MS/MS,corrected using the Matrix standard and quantified external standard method.In the concentration range of 1-200μg/kg,the chromatographic peak area of the ten diuretics showed good linear correlation with concentration,and the correlation coefficients were all higher than 0.99.The detection limit was 0.5 to 1.0μg/kg and the quantitation limit was 1.0 to 2.0μg/kg,respectively.The average recoveries of the 10 diuretic drugs in the four matrices ranged from 60.8%to 112.8%at the supplemental levels of 2 to 200μg/kg,and the relative standard deviations(RSDs)within and between batches ranged from 0.8%to 13.5%.In short,the present method was simple,accurate and reproducible,and could be used for rapid determination of diuretics residues in animal-derived products.