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.
作者
吴虎虎
彭麟
季辉
刘晓晓
滕佩
江善祥
WU Huhu, PENG Lin, JI Hui, LIU Xiaoxiao ,TENG Pei ,JIANG Shanxiang(College of Veterinary Medicine, Nanjing Agricultural University, Nanjing 210095, Chin)
出处
《南京农业大学学报》
CAS
CSCD
北大核心
2018年第2期377-381,共5页
Journal of Nanjing Agricultural University
