食品与发酵工业 >

2024 , Vol. 50 >Issue 13: 290 - 297

DOI: https://doi.org/10.13995/j.cnki.11-1802/ts.039025

分析与检测

多壁碳纳米管净化-液相色谱-串联质谱法测定水产品中19种含氯苯酚类化合物残留

  • 陈彦宏 ,
  • 胡凌 ,
  • 王宇 ,
  • 钱振杰 ,
  • 刘佳 ,
  • 毛新武 ,
  • 蔡伟谊 ,
  • 钟玉心
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  • 1(广州市食品检验所,广东 广州,511400)
    2(中共广东省委党校,广东 广州,510000)
第一作者:学士,工程师(毛新武正高级工程师为通信作者,E-mail:xinwumao@163.com)

收稿日期: 2024-02-29

  修回日期: 2024-03-20

  网络出版日期: 2024-08-02

基金资助

广州市市场监督管理局科技项目(2022kj36);广东省自然科学基金项目(2019B1515210025)

收起

Determination of 19 chlorinated phenol residues in aquatic products by multi-walled carbon nanotubes purification-liquid chromatography-tandem mass spectrometry

  • CHEN Yanhong ,
  • HU Ling ,
  • WANG Yu ,
  • QIAN Zhenjie ,
  • LIU Jia ,
  • MAO Xinwu ,
  • CAI Weiyi ,
  • ZHONG Yuxin
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  • 1(Guangzhou Institute for Food Inspection, Guangzhou 511400, China)
    2(Party School of the Guangdong Provincial Committee of CPC, Guangzhou 510000, China)

Received date: 2024-02-29

  Revised date: 2024-03-20

  Online published: 2024-08-02

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摘要

该研究基于多壁碳纳米管吸附材料,对提取条件、净化条件等进行了研究和优化,建立了一种操作简便、重现性好、可同时测定水产品中19种含氯苯酚类化合物残留的多壁碳纳米管净化-液相色谱-串联质谱法。试样经磷酸氢二钠-柠檬酸缓冲液、乙腈提取,加入无水MgSO4、NaCl盐析,有机层经无水MgSO4、MWCNTs和C18净化,氮吹浓缩后,以甲醇和10 mmol/L乙酸铵溶液为流动相,使用Phenomenex Kinetex C18色谱柱分离,LC-MS/MS测定。结果表明,19种含氯苯酚类化合物在0.2~5 000 μg/L线性关系良好,相关系数r≥0.996,方法定量限为1~500 μg/kg。在低、中、高不同加标水平下,回收率为80%~96%,相对标准偏差为2.4%~8.9%,方法准确度和精密度良好,可适用于水产品中19种含氯苯酚类化合物残留的高通量确证分析。

关键词： 含氯苯酚类; 多壁碳纳米管; 液相色谱-串联质谱法; 水产品

本文引用格式

陈彦宏 , 胡凌 , 王宇 , 钱振杰 , 刘佳 , 毛新武 , 蔡伟谊 , 钟玉心 . 多壁碳纳米管净化-液相色谱-串联质谱法测定水产品中19种含氯苯酚类化合物残留[J]. 食品与发酵工业, 2024 , 50(13) : 290 -297 . DOI: 10.13995/j.cnki.11-1802/ts.039025

Abstract

In this study, the extraction conditions and purification conditions were investigated and optimized based on multi-walled carbon nanotube adsorbent materials.A multi-walled carbon nanotubes purification-liquid chromatography-tandem mass spectrometry method was developed for the simultaneous determination of 19 chlorinated phenol residues in aquatic products with simple operation and good reproducibility.The sample was extracted by disodium hydrogen phosphate-citric acid buffer and acetonitrile, then added with anhydrous magnesium sulfate and sodium chloride for salting out.The organic layer was aspirated and cleaned up by anhydrous magnesium sulfate, MWCNTs and C18, concentrated by nitrogen blowing, and then separated on a Phenomenex Kinetex C18 column with methanol and 10 mmol/L ammonium acetate solution as the mobile phases for the determination of 19 chlorinated phenols by LC-MS/MS.The results showed that the linear relationship of 19 chlorinated phenols was good in the range of 0.2-5 000 μg/L with the correlation coefficients r≥0.996, and the limits of quantification were in the range of 1-500 μg/kg.The recoveries of 19 chlorinated phenols were in the range of 80%-96% at different spiked levels of low, medium, and high, and the RSDs were in the range of 2.4%-8.9%, which indicated that the method were accurate and precise, and it could be applied to high-throughput confirmation analysis of 19 chlorinated phenol residues in aquatic products.

Key words： chlorinated phenols; multi-walled carbon nanotubes; liquid chromatography-tandem mass spectrometry; aquatic products

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