色谱

色谱 ›› 2014, Vol. 32 ›› Issue (4): 419-425.DOI: 10.3724/SP.J.1123.2014.01016

• 庆祝《色谱》创刊三十周年暨卢佩章院士九十华诞专刊-研究论文 • 上一篇    下一篇

改进的QuEChERS方法用于鱼肉中孔雀石绿、隐色孔雀石绿、结晶紫和隐色结晶紫的快速检测(英文)

朱程云1,2, 魏杰2, 董雪芳2, 郭志谋2, 刘名扬1,2, 梁鑫淼2   

  1. 1. 大连交通大学环境与化学工程学院, 辽宁 大连 116028;
    2. 中国科学院大连化学物理研究所 分离分析化学重点实验室, 辽宁 大连 116023
  • 收稿日期:2014-01-08 修回日期:2014-03-06 出版日期:2014-04-08 发布日期:2014-03-28
  • 通讯作者: 刘名扬, 梁鑫淼
  • 基金资助:

    National Natural Science Foundation of China (21177040).

Fast analysis of malachite green, leucomalachite green, crystal violet and leucocrystal violet in fish tissue based on a modified QuEChERS procedure

ZHU Chengyun1,2, WEI Jie2, DONG Xuefang2, GUO Zhimou2, LIU Mingyang1,2, LIANG Xinmiao2   

  1. 1. College of Environment and Chemistry Engineering, Dalian Jiaotong University, Dalian 116028, China;
    2. Key Laboratory of Separation Science for Analytical Chemistry, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Dalian 116023, China
  • Received:2014-01-08 Revised:2014-03-06 Online:2014-04-08 Published:2014-03-28

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摘要：

孔雀石绿（MG）和结晶紫（CV）具有抗菌等活性，常被违法用于水产养殖业。但MG、CV及其代谢产物隐色孔雀石绿（LMG）、隐色结晶紫（LCV）具有致癌性。所以水产品中染料的残留检测是食品安全分析的重要问题。由于水产品基质复杂，样品前处理尤为重要。本文发展了一种基于QuEChERS技术与高效液相色谱联用的方法，用于鱼肉中4种染料的同时检测。对QuEChERS方法中提取剂体积、提取次数以及分散固相萃取材料进行了优化。结果表明反相/强阴离子交换材料（C18SAX）能有效提高回收率。在最优条件下，4种染料在0.5~100 mg/L范围内线性良好，相关系数均大于0.998。该方法在鱼肉中的回收率为73%~91%，RSD为0.66%~5.41%。结果表明该方法简单、高效，适合于鱼肉中染料的快速检测。

关键词: QuEChERS, 高效液相色谱, 结晶紫, 孔雀石绿, 隐色结晶紫, 隐色孔雀石绿, 鱼肉组织

Abstract:

Triphenylmethane dyes malachite green (MG) and crystal violet (CV) have been used as antimicrobial, antiparasitic and antiseptic agents in aquaculture. However, MG and CV, as well as their metabolites leucomalachite green (LMG) and leucocrystal violet (LCV) are potential mutagens and carcinogens. Thus, the efficient determination of dye residues is of great concern. Considering the complexity of the aquatic products, the sample pretreatment is significant for decreasing matrix interference and improving detection sensitivity. In this study, a simple and rapid QuEChERS procedure was developed and combined with HPLC analysis for the simultaneous determination of the four dyes in fish tissue. An XCharge C18 column was applied in HPLC analysis to achieve good peak shape and selectivity. The pretreatment method involved the extraction of dyes from fish tissue and further clean-up with dispersive solid phase extraction (d-SPE) material. The extraction volume, extraction time as well as d-SPE materials were systematically optimized. The results indicated that reversed-phase/strong anion exchange (C18SAX) adsorbent in the d-SPE procedure could effectively improve the recovery compared with conventional C18 or C18 incorporated with primary secondary amine (PSA) material. Under optimized conditions, good linearity was achieved in the concentration range of 0.5-100 mg/L with R2 greater than 0.998. The recoveries were 73%-91% and the precisions were 0.66%-5.41%. The results demonstrated the feasibility and efficiency of QuEChERS procedure incorporated with HPLC for dye monitoring.

Key words: crystal violet, fish tissue, high performance liquid chromatography (HPLC), leucocrystal violet, leucomalachite green, malachite green, QuEChERS

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