改良QuEChERS结合高效液相色谱-串联质谱法检测饲料中的7种镇静剂

Determination of seven sedatives in feed by modified QuEChERS combined with high-performance liquid chromatography-tandem mass spectrometry

本实验旨在建立以改良的QuEChERS作为前处理技术,结合高效液相色谱-串联质谱技术(HPLC-MS/MS)检测饲料中7种镇静剂的检测方法。样品加入乙腈提取,提取液经增强型基质去脂吸附剂(EMR-Lipid)脱脂,盐析后经PSA和C18吸附剂进一步净化浓缩,然后用高效液相色谱-串联质谱方法检测分析。结果表明:7种镇静剂为1~100μg/L时线性关系良好,相关系数均大于0.99,检出限为1.1~2.8μg/kg,定量限为3.7~9.3μg/kg。分别对配合饲料、浓缩饲料和预混合饲料进行3个水平的加标回收实验,平均回收率为84.7%~96.5%,相对标准偏差为3.2%~10.8%。该方法前处理方法快速、简便、灵敏度高,适用于饲料中多种残留镇静剂的同时测定。

A analytical method for determining seven sedatives in feed was developed by modified -QuEChERS coupled with high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS).The samples were extracted with acetonitrile,the extract acquired was degreased by enhanced matrix removal(EMR-lipid) material.After the process of salting-out,PSA and C18 adsorbent was further purified and concentrated.Then the analytes were detected and analyzed by HPLC-MS/MS.The results demonstrated that the linear range of this method was from 1 ~ 100 μg/L with good correlation coefficients of R >0.99.The limits of detection and quantification were 1.1 ~ 2.8 μg/kg and 3.7 ~ 9.3μg/kg,respectively.The average recoveries of the seven sedatives spiked in three feed matrixes(the complete formula feed,the concentrated feed and the compound premix feed)at three spiked levels were 84.7%~ 96.5% with the relative standard deviations (RSDs) of 3.2%~ 10.8%.The proposed method was simple,sensitive and accurate.It was applicable for the determination of sedatives in feed.