屠宰动物肌肉组织中的保泰松残留量的LC-UV测定方法研究  

DETERMINATION OF PHENYLBUTAZONE IN ANIMAL TISSUES-LIQUID CHROMATOGRAPHIC METHOD

作　　者：庞国芳[1] 王飞[1] 曹彦忠[1] 贾光群[1] 李学民[1] 张进杰[1] 范春林[1] 刘永明[1] 石玉秋[1] 

机构地区：[1]秦皇岛出入境检验检疫局,河北秦皇岛066002

出　　处：《检验检疫科学》2007年第5期3-7,共5页Inspection and Quarantine Science

基　　金：国家标准化管理委员会20051867-T-326国家标准制订任务项下的GB/T20754-2006<畜禽肉中保泰松残留量的测定方法液相色谱-紫外检测法>标准研究项目

摘　　要：[目的]利用液相色谱法测定屠宰动物中保泰松残留量。[方法]采用含有稳定剂二硫苏糖醇的乙酸乙酯与甲醇混合溶液提取牛、猪、羊、鸡肌肉中保泰松残留,用甲醇+氨水+二氯甲烷+二硫苏糖醇的乙酸乙酯溶液溶解,固相萃取柱净化,用冰乙酸+甲醇+二氯甲烷+乙醚混合溶液洗脱并蒸至近干,流动相定容、外标法定量。[结果]回收率89.0%～111.49%,相对标准偏差在8%以内,检出限5.0 mg/kg。An analytical method has been established for the determination ofphenylbutazone in animal tissues by Liquid chromatographic method. Phenylbutazone is extracted from muscle tissue with methanol/ethyl acetate containing DL-dithiothreitol. After concentrating, the extract is reconstituted by methanol/ammonia/methylene chloride/ethyl acetate containing DL-dithiothreitol and cleaned up on a conditioned Florisil solid phase extraction cartridge. Phenylbutazone is eluted from the cartridge with a mixture of glacial acetic acid, methanol, methylene chloride and aether. The eluate is dried, and the residues reconstituted in mobile phase and analysed on a reversed phase high performance liquid chromatography system with UV detection and uantified by external standard method. At fortification levels of 5.0 μ g/kg- 150μg/kg,, recoveries are 89.0%- 111.49%, RSD%≤ 9.888%, and limit of detection for the method 5.0 mg/kg. The method is simple, easy to operate with relatively high recoveries and applicable to determination of phenylbutazone residue in animal tissues.

关 键 词：屠宰动物 肌肉 保泰松 LC-UV 

分 类 号：O657.7[理学—分析化学] TS251.7[理学—化学]