鸡饲料中氢溴酸常山酮含量的反相HPLC检测方法的建立  

Development of RP-HPLC method for determination of halofuginone hydrobromide in chicken feeds

作　　者：吴虎虎 彭麟[1] 季辉[1] 刘晓晓[1] 滕佩 江善祥[1] WU Huhu, PENG Lin, JI Hui, LIU Xiaoxiao ,TENG Pei ,JIANG Shanxiang(College of Veterinary Medicine, Nanjing Agricultural University, Nanjing 210095, Chin)

机构地区：[1]南京农业大学动物医学院,江苏南京210095

出　　处：《南京农业大学学报》2018年第2期377-381,共5页Journal of Nanjing Agricultural University

摘　　要：[目的]本文旨在建立检测饲料中氢溴酸常山酮含量的固相萃取-反相高效液相色谱法。[方法]在鸡饲料中添加一定浓度氢溴酸常山酮,经100 g·L^(-1)碳酸钠溶液碱化后用乙酸乙酯提取饲料中氢溴酸常山酮,0.125 mol·L^(-1)乙酸铵缓冲液萃取,HLB柱净化后供HPLC测定。流动相为体积比5∶3∶12的乙腈、0.25 mol·L^(-1)乙酸铵缓冲液、水溶液(冰乙酸调pH4.3),检测波长243 nm。[结果]该方法对鸡饲料中氢溴酸常山酮的检测限为0.05μg·g^(-1),定量限为0.2μg·g^(-1)。在0.2~15μg·g^(-1)范围内,线性关系良好,其相关系数大于0.999,在0.2、1.0、5.0和15.0μg·g^(-1)添加水平下,鸡饲料中氢溴酸常山酮的回收率为87%~113%,日内变异系数为1.1%~17%,日间变异系数为7.1%~12%。[结论]该方法具有良好的线性关系和较高的精密度、回收率,可以简便、灵敏、快速地检测鸡饲料中氢溴酸常山酮含量。[Objectives]A solid-phase extraction and reversed-phase high performance liquid chromatography（SPE-RP HPLC） method for determination of halofuginone hydrobromide in chicken feeds was developed.[Methods]The chicken feed added to halofuginone hydrobromide was alkalization by 100 g·L^-1 sodium carbonate solution and then was successively extracted by ethyl acetate,0.125 mol·L^-1 ammonium acetate buffer liquid-liquid extracted,and was cleaned up via HLB column before detection by HPLC.The mobile phase consisted of acetonitrile,0.25 mol·L^-1 of ammonium acetate buffer and water（the volume ratio is 5 ∶ 3 ∶ 12）,adjusted to pH value equal to 4.3 with glacial acetic acid.Halofuginone hydrobromide was monitored by UV detector at 243 nm.[Results]The result showed that,the limit of detection and quantification was 0.05 μg·g^-1 and 0.2 μg·g^-1,respectively.Among the concentration range from 0.2 to 15 μg·g^-1,the correlation coefficient is greater than 0.999,a good linear relation.At 0.2,1.0,5.0,15.0 μg·g^-1 levels,the rate recoveries of 87%-113% were obtained,and within-day and between-day cofficents of variation were 1.1%-17% and 7.1%-12%,respectively.[Conclusions]This method can meet the requirements of sensitivity,precision and accuracy,which can be applied for quick and efficient determination of halofuginone hydrobromide in chicken feeds.

关 键 词：氢溴酸常山酮 鸡饲料 反相高效液相色谱法 

分 类 号：S816.75[农业科学—饲料科学]