质量安全与检验检测2024,Vol.34Issue(2) :1-7.

QuEChERS-HPLC-MS/MS法检测蚕砂中氯霉素残留量

Determination of chloramphenicol residues in silkworm excrement-high performance liquid chromatography-tandem mass spectrometry method with QuEChERS

梁香 崔凤云 朱绍华 付善良 成婧 陆静 焦艳娜
质量安全与检验检测2024,Vol.34Issue(2) :1-7.

QuEChERS-HPLC-MS/MS法检测蚕砂中氯霉素残留量

Determination of chloramphenicol residues in silkworm excrement-high performance liquid chromatography-tandem mass spectrometry method with QuEChERS

梁香 1崔凤云 2朱绍华 1付善良 1成婧 1陆静 1焦艳娜1
扫码查看

作者信息

  • 1. 长沙海关技术中心&食品安全科学技术湖南省重点实验室 湖南长沙 410004
  • 2. 中国海关科学技术研究中心
  • 折叠

摘要

本文建立了一种QuEChERS和C18固相萃取柱净化结合液相色谱串联质谱方法测定蚕砂中氯霉素残留.经乙酸乙酯提取,GCB和C18固相萃取柱净化,以甲醇和水为流动相梯度洗脱,C18柱(2.1 mm×100mm,1.7μm)分离,在电喷雾离子源(ESI)负离子模式下采用液相色谱-串联质谱仪测定,内标法定量.结果显示,在0.02μg/L~5.00μg/L,氯霉素具有良好的线性关系,相关系数为1.000.氯霉素在4个加标水平(0.1 μg/kg、0.3 μg/kg、1.0 μg/kg、2.0 μg/kg)下回收率范围为74.7%~103.0%,RSD在4.36%~9.64%.该方法操作快速简单,且灵敏度与回收率高,可用于蚕砂中氯霉素残留的检测分析.

Abstract

A method for the determination of chloramphenicol residues in silkworm excrement based on QuEChERS-High Performance liquid chromatography-tandem mass spectrometry was developed.The method was extracted by ethyl acetate,pu-rified by GCB and C18 solid phase extraction column,eluted by methanol and water as mobile phase gradient,separated by C18 column(2.1 mm×100mm,1.7 μm),determined by liquid chromatography tandem mass spectrometry under the negative ion mode of electric spray ion source(ESI),and quantified by internal standard method.The results showed that chloramphenicol had a good linear relationship between 0.02 μg/L-5.00 μg/L with a correlation coefficient of 1.000.The recoveries of chlo-ramphenicol at four supplemental levels(0.1 μg/kg,0.3 μg/kg,1.0 μg/kg,2.0 μg/kg)ranged from 74.7%-103.0%,and the RSD ranged from 4.36%-9.64%.The method is quick,simple,sensitive and has high recovery rate,so it can be used for the de-tection and analysis of chloramphenicol residues in silkworm excrement.

关键词

蚕砂/氯霉素/QuEChERS/固相萃取/液相色谱-串联质谱

Key words

Silkworm excrement/Chloramphenicol/QuEChERS/Solid phase extraction/High performance liquid chromatogra-phy-tandem mass spectrometry

引用本文复制引用

基金项目

海关总署科研项目(2023HK078)

出版年

2024
质量安全与检验检测
中国检验检疫科学研究院

质量安全与检验检测

影响因子:0.399
ISSN:2096-8876
参考文献量32
段落导航相关论文