通过式固相萃取-超高效液相色谱-串联质谱法测定鱼体中10种三嗪类除草剂残留  

Analysis of 10 Triazine Herbicide Residues in Fish Using Ultra High Performance Liquid Chromatography-Tandem Mass Spectrometry with Pass-Through Solid Phase Extraction

作　　者：魏伟 郝永 亓林敏 张玲 WEI Wei;HAO Yong;QI Linmin;ZHANG Ling(Binzhou Testing Center,Binzhou 256600,China)

机构地区：[1]滨州市检验检测中心,山东滨州256600

出　　处：《食品科技》2024年第12期322-327,共6页Food Science and Technology

基　　金：2022年滨州市农社领域科技创新政策引导计划项目(2022SHFZ049)。

摘　　要：文章建立了基于通过式固相萃取净化的鱼体中10种三嗪类除草剂的超高效液相色谱-串联质谱(Ultra high performance liquid chromatography-tandem mass spectrometry,UPLC-MS/MS)检测方法。样品经乙腈提取,采用PRiME HLB固相萃取柱以通过式固相萃取的方式进行净化,经ACQUITY BEH C_(18)(100 mm×2.1 mm,1.7μm)色谱柱分离、梯度洗脱,采用UPLC-MS/MS在正离子电喷雾、多反应监测模式下进行测定。结果表明,在0.2~40μg/L线性范围内,10种三嗪类除草剂线性相关系数为0.993~0.999。扑草净的方法检出限为0.2μg/kg,方法定量限为0.5μg/kg;其余9种待测物质的方法检出限为0.5μg/kg,方法定量限为1.0μg/kg。样品添加回收率为66.3%~103.2%,相对标准偏差为0.5%~9.7%(n=6)。该方法灵敏度和准确度较高,且操作简便,能够用于实际样品的准确定量。A detection method for 10 triazine herbicide residues in fish was developed using ultra high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)with pass-through solid-phase extraction.The samples were extracted with acetonitrile,cleaned up by pass-through solid-phase extraction approach using PRiME HLB column.The separation was performed on an ACQUITY BEH C_(18)column(100 mm×2.1 mm,1.7μm)with gradient elution,and detection was carried out in positive ion electrospray mode with multiple reaction monitoring(MRM).The 10 triazine herbicides exhibited good linearity in the range of 0.2μg/L to 40μg/L,with correlation coefficients ranged from 0.993 to 0.999.The limit of detection for the method of prometryn was 0.2μg/kg,and the limit of quantitation was 0.5μg/kg,while the limits of detection for the method of the other 9 analytes were 0.5μg/kg,and the limits of quantitation were 1.0μg/kg.The recovery rates of the spiked samples were in the ranges of 66.3%to 103.2%,with relative standard deviation between 0.5%and 9.7%(n=6).The method has high sensitivity and accuracy,and is easy to operate,making it suitable for precise quantification of real samples.

关 键 词：超高效液相色谱-串联质谱法 通过式固相萃取 三嗪类除草剂 鱼体 

分 类 号：TS207.5*3[轻工技术与工程—食品科学]