GC/MS分析牛尿中瘦肉精残留

目的: 建立牛尿中"瘦肉精"的GC/MS分析方法,为保障食品安全提供有效的分析手段。 方法: 调节样品的pH为5.2,用乙酸乙酯-异丙醇提取,蒸干后用乙酸铵溶解,经固相萃取小柱净化,氮气吹干后经双三甲基硅基三氟乙酰胺(BSTFA)衍生,GC/MS分析。 结果: 以牛尿为基质,"瘦肉精"在20.0~160.0 μg·L^-1添加浓度范围内线性关系良好,r=0.9980,其回收率在65.6%~99.0%之间,检出限为0.3 μg·L^-1。 结论: 本方法专属性好,准确,杂质少,适用于牛尿中"瘦肉精"的检测。

Objective: The establishment of GC/MS determination of clenbuterol in bovine urine was to provide an effective means of analysis for the protection of food safety. Method: Adjusted the sample pH value to 5.2,and extracted with ethyl acetate-isopropanol.Dissolved with ammonium acetate after the evaporation,and purified by solid phase extraction column.Dried by nitrogen and double trimethyl trifluoro-acetamide derivatives and determined by GC/MS. Results: The bovine urine for the matrix,20.0-160.0 μg·L^-1 added clenbuterol concentration range a good linear relationship,correlation coefficient r=0.9980,the recovery rate of 65.6%-99.0% and the detection limit was 0.3 μg·L^-1. Conclusion: The method is specific,and accurate,less impurities,apply to the detection of clenbuterol in bovine urine.

[1] LI Xian-jun(李羡筠).Study on toxicity and mutagenicity of clenbuterol (瘦肉精的毒性和致突变性研究进展).J Guangxi Med Univ (广西医科大学学报),2009,26(4):653
[2] CHEN Li-xian(陈莉娴).Status and countermeasures of clenbuterol residue in pig (生猪瘦肉精残留的现状与对策).Chin J Anim Quar (中国动物检疫),2010,27(5):21
[3] ZHANG Hua(张华).Harm of shouroujing and its examination (瘦肉精的危害及检测方法).Guizhou Agr Sci (贵州农业科学),2004,32(1):83
[4] WEI Wan-li(魏万里).Examining columtro ingredients in urine with multi-stage series mass-spectrography (多级串联质谱法检测尿液中的克伦特罗成分). J Chin People’s Pub Security Univ (中国人民公安大学学报),2003,9(3):8
[5] ZHU Yong-lin(朱永林),SHAO De-jia(邵德佳),JIANG Tian-mei(蒋天梅),et al.Determination of clenbuterol in swine urine and liver by isotopic internal standard GC /MS method(同位素内标GC/MS法测定猪尿和猪肝中克伦特罗).Chin J Veter Drug (中国兽药杂志),2007,41(8):7
[6] MIAO Hong(苗虹),WU Yong-ning(吴永宁),ZHAO Jing-ling(赵京玲),et al.Determination of clenbuterol residues in animal foods and biological materials by gas chromatographic-mass spectrometric method(气相色谱-质谱法测定动物性食品及生物材料中的克伦特罗残留). Chin J Food Hyg (中国食品卫生杂志),2003,15(1):18
[7] ZHANG Yi-nong (张亦农),ZHANG Chang-jiu(张长久),WU Mou-tian(吴侔天),et al.Analysis of clenbuterol in residue of pig and pig liver by GC/MS(猪肉及其可食性组织中残留克伦特罗的GC/MS检测方法). Chin J Sports Med (中国运动医学杂志),2003,22(6):620
[8] ZHU Bao-Ping(朱宝平),LUO He-Dong(骆和东),CHEN Kai-Ling(陈恺玲),et al.Detection of clenbuterol remains in the animal tissue by GC-MS/MS Method(GC-MS/MS法测定动物性食品中的克伦特罗残留量).Chin J Prev Med(海峡预防医学杂志),2006,12(3):8
[9] TAO Yan-fei(陶燕飞),LIU Deng-cai(刘登才),MA Su-ning(马素英),et al.The determination of the clenbuterol residues in bovine tissues by SPE GC-MS with derivatisation(衍生固相萃取GC-MS检测牛可食组织中克伦特罗的残留量).J Instrum Anal (分析测试学报),2003,23(增刊):211
[10] ZHAO Jing-jing(赵晶晶),LI Yun-lan(李云兰),LIANG Jin-qiong(梁晋琼),et al.Contribution and correlation of residual clenbuterol hydrochloride in hair,liver,kidney and muscle of rat(盐酸克伦特罗在小鼠毛发与肝肾和肌肉中残留量关系的研究).Chin J Pharm Anal(药物分析杂志),2009,29(8):1277
[11] ZHANG Xue-man(张雪曼),SU Qing-yun(苏青云),CHENG Xue-mei(程雪梅).Determination of clenbuterol residues in animal tissue and urine by SPE and GC-MS(固相萃取-气相色谱-质谱法测定动物组织及尿液中盐酸克伦特罗药物残留量). J Instrum Anal (分析测试学报),2005,24(增刊):180