气相色谱-质谱法测定饲料中的二氢吡啶

Determination of Diludine in Feed by Gas Chromatography-mass Spectrometry

本文建立一种气相色谱-质谱法(GC-MS)测定饲料产品中二氢砒啶含量的方法。采用避光的环境,在饲料样品中添加保护剂降低二氢砒啶的光化学反应,采用乙腈提取待测物,经浓缩和固相微萃取净化,采用BSTFA进行衍生,衍生物通过GCMS气化分离以及选择离子监测(SIM)模式进行检测。对二氢吡啶衍生物的电子轰击(EI)质谱碎片进行解析,特征碎片离子(m/z)206、178、251、151、150、195为定性离子,206为定量离子。该分析方法中二氢吡啶在3~150 mg/kg范围内呈良好线性关系,样品分析精密度RSD<3%,样品中二氢吡啶的检出限0.3 mg/kg。结果表明,这项方法灵敏、稳定、可靠,有效避免了饲料中二氢吡啶在处理过程中的降解,并有效排除了主要杂质的干扰,适用于饲料产品中二氢吡啶的定量分析与确证。

This paper presents a method for the determination of 3,5-Diethoxycarbonyl-2,6-dimethylpyridine in feed products by gas chromatography-mass spectrometry(GC-MS).In the dark environment,the protective agents were added to the feed to reduce the photochemical reaction,and the analyte was extracted with acetonitrile,extracted,concentrated and purified,then derivatized with BSTFA,and the derivative was detected by GCMS.The mass spectra of diludine derivative was analyzed.The characteristic fragment ions m/z 206,178,251,151,150,195 was qualitative ion and 206 was quantitative ion.This analytical method of diludine showed a good linear in the range of 3 mg/kg-150 mg/kg,the precision of the method RSD was less than 3%,and the detection limit of diludine in the sample was 0.3 mg/kg.The results show that this analytical method is sensitive,stable,reliable and effective to avoid the degradation of diludine in the sample process and effectively eliminate the interference of impurities.This method is suitable for the analysis of diludine in feed products.