气相色谱-质谱法确证分析饲料中6种利尿剂的研究  

Study on confirmation analysis of the diuretics in animal feed by gas chromatography-mass spectrometry

作　　者：王培龙[1] 范理[1] 宋荣[1] 田静[1] 王彤[1] 苏晓鸥[1] 

机构地区：[1]中国农业科学院农业质量标准与检测技术研究所,北京100081

出　　处：《分析试验室》2009年第12期31-34,共4页Chinese Journal of Analysis Laboratory

基　　金：十一五科技支撑计划重点课题(2006BAD12B03)资助

摘　　要：研究建立了气相色谱-质谱确证分析配合饲料中依他尼酸、氢氟噻嗪、氯噻嗪、呋噻米、氯噻酮和氢氯噻嗪等6种利尿剂的方法。本研究用磷酸盐缓冲液和甲醇混合提取液提取饲料中6种利尿剂,通过液液提取净化,在碳酸钾催化下用碘甲烷衍生,气相色谱-质谱定性和定量分析。确定了磷酸盐缓冲液和甲醇的提取体系,优化了6种利尿剂的色谱分离条件和质谱检测条件。在优化条件下,6种利尿剂线性范围为0.05～1.0μg/mL,线性相关系数高于0.99,方法的定量限为0.5μg/g。在饲料样品中,不同添加浓度水平回收率高于57.6%,相对标准偏差低于12%。该方法适用于饲料样品中6种利尿剂的定性和定量分析。A stable method for the confirmation analysis of six kinds of diuretics including ethacrynic acid, hydroflu- methiazide, furosemide, chlorthalidone, chlorothiazide and hydrochlorothiazide in animal feed by gas chromatographymass spectrometry was developed. The diuretics in animal feed were extracted with phosphate buffer and methanol, the cleaning procedure was carried out by liquid-liquid extraction, the diuretic derivatives were gained in acetone by using methane iodide, and the determination was performed by GC-MS. The extraction solution and the parameters of GC-MS for diuretics were optimized. Under optimum condition, there is a good linear correlation （the correlation coefficient is above 0.99） in the range of 0.05 - 1.0μg/mL. The limits of quantitation were 0.5 μg/g. The recoveries of all diuretics in animal feed were above 57.6%, the relative standard deviation was below 12%. The method is suitable for the determination of the diuretics in animal feed, and it possesses some advantages including simple operation procedure, high sensitivity and precision.

关 键 词：利尿剂 配合饲料 气相色谱-质谱 

分 类 号：O557.63[理学—热学与物质分子运动论]