固相萃取/气相色谱-质谱同时测定猪肉中4种β-激动剂类药物残留量  

Simultaneous Determination of Four β-agonist Residues in Pork Meat by Solid-phase Extraction and Gas Chromatography-Mass Spectrometry

作　　者：孔莹[1] 邱月明[2] 李鹏[2] 沈建忠[1] 

机构地区：[1]中国农业大学动物医学院,北京100094 [2]中国检验检疫科学研究院,北京100025

出　　处：《分析测试学报》2006年第2期63-66,70,共5页Journal of Instrumental Analysis

摘　　要：建立了用气相色谱-质谱同时检测猪肉中克伦特罗、沙丁胺醇、特布它林和非诺特罗残留量的方法。样品经β-葡萄糖苷酸酶水解后，用乙酸铵溶液提取，MCX固相萃取柱进一步净化，再用N，O双（三甲基硅基）三氟乙酰胺-三甲基氯硅烷（BSTFA＋TMCS，99＋1）衍生化。采用选择离子监控模式（SIM）检测，所选的离子（斜体为定量离子）分别为克伦特罗：86、187、212、262，沙丁胺醇：86、350、369、440，特布它林：86、336、356、357，非诺特罗：236、322、356、412。克伦特罗和沙丁胺醇的检出限为0．5μg/kg，线性范围为0．5～200μg/kg；特布他林和非诺特罗的检出限为5μg／kg，线性范围均为5—200μg／kg；4种组分的线性相关系数均大于0．99。该方法的回收率为68％～128％，相对标准偏差为3％-17％。A method was developed for the simultaneous determining of Clenbuterol, Salbutamol, Terbutaline and Fenoterol residues in pork tissues using gas chromatography - mass spectrometry （ GC - MS）. The homogenized samples were enzyme digested by β-glucuronidase enzyme, and extracted with ammonium acetate. Further cleanup was performed on a MCX cartridge and the purified drugs were derivatized with Sylon BFT [ N, O-his （trimethylsilyl） trifluoroacetamide （BSTFA） - trimethylchlorosilane （TMCS）, 99 ＋ 1 ]. The selected ion monitoring（SIM） method was used for detection, and the monitored ions were m/z 86, 187, 212, and 262 for Clenbuterol, m/z 86,350,369, and 440 for Salbutamol, m/z 86,336,356, and 357 for Terbutaline, and m/z 236,322,356, and 412 for Fenoterol, respectively. Quantitation ions were selected at m/z 86 for Clenbuterol, m/z 369 for Salbutamol, m/z 356 for Terbutaline, and m/z 322 for Fenoterol. The limits of detection were 0.5 μg/kg for Clenbuterol and Salbutamol, 5 μg/kg for Terbutaline and Fenoterol. The correlation coefficients were better than 0.99 for the calibration curves for the drugs. The linear range is 0.5 -200 μg/kg for Clenbuterol and Salbutamol, 5 -200 μg/kg for Terbutaline and Fenoterol. The recoveries were 68% - 128% , with relative standard deviations of 3% - 17%.

关 键 词：气相色谱-质谱 克伦特罗 沙丁胺醇 特布它林 非诺特罗 固相萃取 猪肉 

分 类 号：O657.63[理学—分析化学]