摘要
本实验以QuEChERS作为样品前处理手段,采用高效液相色谱-串联质谱(HPLC-MS/MS)检测技术,建立了适用于禽饲料中59种杀虫剂残留同时检测的方法。禽饲料样品均由1%(V/V)乙酸酸化乙腈提取,经0.30 g C18+0.30 g中性氧化铝(ALN)分散萃取净化,采用Venusil MP C18色谱柱分离,以0.1%(V/V)甲酸水溶液和乙腈为流动相梯度洗脱,电喷雾电离(ESI)源、正负离子交替扫描方式进行检测,基质匹配标准溶液定量。结果表明:59种杀虫剂在0.0050~2.000 mg/L范围内线性良好,相关系数大于0.99;加标回收率为71.0%~109.0%,相对标准偏差为4.0%~10.5%,检出限为0.004~0.040 mg/kg。该法灵敏度、准确度和精密度均符合相关杀虫剂残留测定的技术要求。
A effective method was developed for the determination of 59 pesticide residues in poultry feed by modified QuEChERS and high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS).The target compounds were extracted with 1%(V/V)acetic acid-acetonitrile,and purified by 0.30 g C18 and 0.30 g neutral alumina(ALN).The 0.1%(V/V)formic acid aqueous solution and acetonitrile were used as the mobile phases.The extracts were separated on a Venusil MP C18 chromatographic column.The positive electrospray ion and negative electrospray ion(ESI)source,ion monitoring(SIM)mode were used.The analytes were quantified by the matrix match standard solutions.The good linearities were obtained in the range of0.005~2.000 mg/L,and the correlation coefficients were all greater than 0.99.The average recoveries of the 59 pesticide residues ranged from 71.0%~109.0%,and RSDs were in the range of 4.0%~10.5%.The limits of detection were 0.004~0.040 mg/kg.The method was sensitive,accurate and precise,and could meet the technical requirements for the determination of insecticide residues.
作者
林绪
蓝梦哲
李金连
王海鸣
曹小彦
LIN Xu;LAN Mengzhe;LI Jinlian;WANG Haiming;CAO Xiaoyan(Guangzhou GRG Metrology&Test CO.,LTD.,Guangzhou,Guangdong Prvoince 510000,China)
出处
《中国饲料》
北大核心
2020年第1期56-63,共8页
China Feed
关键词
高效液相色谱-串联质谱
QUECHERS
杀虫剂残留
禽饲料
high performance liquid chromatography-tandem mass spectrometry
QuEChERS
insecticide residues
poultry feed
作者简介
通讯作者:曹小彦。
