用HPLC-MS/MS研究动物毛发中克伦特罗的残留及代谢规律  被引量:12

Studies on the Determination of Clenbuterol in Swine Hairs Using LC-MS/MS and Its Residue Elimination

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作  者:苏晓鸥[1] 沈建忠[1] 

机构地区:[1]中国农业大学动物医学院

出  处:《中国畜牧杂志》2008年第11期41-46,共6页Chinese Journal of Animal Science

基  金:“十一五”国家科技支撑计划资助专项(2006BAD12B03)

摘  要:研究建立了高效液相色谱-串联质谱(HPLC-MS/MS)测定毛发中盐酸克伦特罗残留的方法。猪毛发以0.1moL/L盐酸溶液提取,MCX固相萃取柱净化,流动相溶解定容。以SB-C18柱为分离柱,1%乙酸水溶液和甲醇(60∶40,V∶V)作为流动相,MS/MS进行定性和定量分析。在优化条件下的最低检出限为0.05μg/kg,定量限为0.2μg/kg。毛发样品中添加不同浓度盐酸克伦特罗,测得回收率在79.0%~86.2%之间,变异系数均低于15.2%。应用该方法研究了盐酸克伦特罗在猪毛发中的代谢并初步探讨其代谢机理。结果表明:在较高饲喂浓度(10mg/kg)时,用药5d后,黑色猪毛发有少量盐酸克伦特罗残留,而白色猪毛发中未检出。从第7天起猪毛发中盐酸克伦特罗蓄积量逐渐增加,最高蓄积浓度为4852.5μg/kg。A method for determination of clenbuterol hydrochloride residue in swine hairs by using high performance liquid chromatography coupled with tandem mass spectrometry was developed. The clenbuterol hydrochloride was extracted from swine hair samples by employing 0. 1 mol/L hydrochloride acid aqueous solution, the cleaning procedure was performed by MCX solid phase extraction cartridge. The clenbuterol hydrochloride was determined by HPLC-MS/MS on SB-C18 column with 1% acetic acid aqueous solution : methanol (60:40) as the mobile phase. Under optimum conditions, the recoveries of different quantities of clenbuterol hydrochloride in swine hairs were from79.0 % to 86.2 %, white the relative standard deviation was below 15.2%. The limit of determination and limit of quantitative for the method were 0.05 μg/kg and 0.20 μg/kg, respectively. The developing method was applied to study the metabolize behavior and mechanism of clenbuterol hydrochloride in swine hair. The result indicated that a little of clenbuterol hydrochloride was found in black hairs of swine which were feed clenbuterol hydrochloride after five days while no found in white swine hair. From the seventh day, the content of clenbuterol hydrochloride in swine hairs was increased gradually, and the highest content of clenbuterol hydrochloride was 4852.5 μg/kg.

关 键 词:高效液相色谱串联质谱 猪毛发 盐酸克伦特罗 代谢 

分 类 号:S816.701.7[农业科学—饲料科学]

 

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