液相色谱-串联质谱法检测猪肉中20种违禁药物残留的研究  

Multi-class Residue Analysis of 20 Illicit Drugs in Pork by High Performance Liquid Chromatography-tandem Mass Spectrometry

作　　者：怀文辉[1] 李建 倪香艳 张晶晶 魏紫嫣 李文辉[1] 赵莹[1] 孙志文[1] HUAI Wen-hui;LI Jian;NI Xiang-yan;ZHANG Jing-jing;WEI Zi-yan;LI Wen-hui;ZHAO Ying;SUN Zhi-wen(Beijing Institute of Veterinary Drugs Control,Beijing 102600,China)

机构地区：[1]北京市兽药监察所,北京102600

出　　处：《中国兽药杂志》2018年第11期59-67,共9页Chinese Journal of Veterinary Drug

基　　金：北京市科学技术委员会北京市科技重大专项(D171100002017004)

摘　　要：建立了猪肉中违禁药物(糖皮质激素、性激素、β2-肾上腺素受体激动剂、玉米赤霉烯酮4类)同时测定的高效液相色谱-串联质谱方法。试样经盐酸水解,乙酸乙酯提取,低温冷冻去除脂类,亲水亲脂平衡固相萃取柱净化。采用C18反相色谱柱分离,以乙腈+水为流动相梯度洗脱,分别在电喷雾离子源正、负离子模式下以多反应监测模式(MRM)分段扫描同时检测,基质匹配内标法定量。结果表明,20种违禁药物在相应的浓度范围内线性良好,相关系数均大于0.99;该方法在猪肉中的检测限(LOD,S/N=3)和定量限(LOQ,S/N=10)分别为0.5、1.0μg/kg。在0.5~10μg/kg添加浓度水平下,平均回收率为63.9%~117%,批内变异系数1.9%~9.1%,批间变异系数4.9%~13.1%。该方法简单、快速、准确,适用于猪肉中多类违禁药物的残留检测。A simultaneous multi-class analysis method for illicit drugs （glucocorticoid hormones, sex hormones,β-agonists,zearanlenone） in pork by high performance liquid chromatography -tandem mass spectrometry wasestablished. The samples were hydrolyzed by dilute hydrochloric acid, extracted by ethyl acetate and cryogenicallyfrozen to remove most lipids followed by clean-up with hydrophilic lipophilic balance SPE. The quantification andconfirmation of the 20 analytes were performed by LC-MS/ MS with electro-spray ionization （ESI） interface inmultiple reaction monitoring （MRM） mode. Matrix matching internal standard method was hired for quantitativeanalysis. The results showed that 20 illicit drugs were linear in the corresponding concentration range, and thecorrelation coefficient was greater than 0.99. The limits of detection （LODs） and limits of quantification （LOQs） were 0.2～0.5 μg/ kg and 0.5～1.0 μg/ kg, respectively. The spiked recoveries at three levels were from 63.9% to117%. The repeatability and the within-laboratory reproducibility were from 1.9% to 9.1% and from 4.9% to13.1%, respectively. The method is simple, rapid,accurate and suitable for simutaneous residue detection of multi-class illicit drugs in pork.

关 键 词：高效液相色谱-串联质谱法 违禁药物 残留检测 

分 类 号：S859.84[农业科学—临床兽医学]