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

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。%Triphenylmethane dyes malachite green(MG)and crystal violet(CV)have been used as antimicro-bial,antiparasitic and antiseptic agents in aquaculture. However,MG and CV,as well as their metabolites leu-comalachite 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 analy-sis 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 recov-ery 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 R 2 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.