固相萃取-高效液相色谱-荧光检测法测定水体中孔雀石绿

食品科学 ›› 2012, Vol. 33 ›› Issue (14): 150-153.

固相萃取-高效液相色谱-荧光检测法测定水体中孔雀石绿

邓建朝，李来好，杨贤庆*，岑剑伟，辛少平，魏涯，吴燕燕

中国水产科学研究院南海水产研究所，国家水产品加工技术研发中心，农业部水产品加工重点实验室

收稿日期:2012-04-07 修回日期:2012-06-18 出版日期:2012-07-25 发布日期:2012-07-27
通讯作者: 杨贤庆 E-mail:yxqgd@163.com
基金资助:
国家农业科技成果转化资金项目;国家农业科技成果转化资金项目;国家现代农业产业技术体系;广东省海洋渔业科技推广项目;广东省海洋渔业科技推广项目;中央级公益性科研院所基本科研业务费专项资金项目

Determination of Malachite Green in Water Using Solid Phase Extraction-High Performance Liquid Chromatography with Fluorescence Detection

Deng Jian-Ming Laihao LIXianqing YANG WU Yan-Yan Sheng-Jun CHEN²

Received:2012-04-07 Revised:2012-06-18 Online:2012-07-25 Published:2012-07-27
Contact: Xianqing YANG E-mail:yxqgd@163.com

摘要/Abstract

摘要： 应用固相萃取-高效液相色谱-荧光检测法建立环境水体中痕量孔雀石绿的分析方法。水样中的孔雀石绿用硼氢化钾还原为其相应的代谢产物隐色孔雀石绿，通过MCX固相萃取柱富集、净化后用0.25mol/L乙酸铵-甲醇溶液洗脱，以Agilent C18反相色谱柱为分析柱，0.05mol/L的乙酸铵(pH4.5)-乙腈(20:80，V/V)为流动相，采用荧光检测器分析，外标法定量。结果表明：孔雀石绿在0.005～0.5μg/mL范围内线性良好，检出限为0.05μg/L。以池塘水、江水和海水作为基底，加标质量浓度分别为0.200、1.00、5.00μg/L时，孔雀石绿的平均加标回收率分别为91.7%～92.6%、87.4%～94.6%和84.1%～92.6%，相对标准偏差分别为4.5%～5.9%、2.8%～4.1%和5.4%～6.5%。该方法灵敏度高、重现性好、杂质干扰小，适用于批量样品的测定。

关键词: 孔雀石绿, 固相萃取, 高效液相色谱, 水体

Abstract: A simple method based on solid phase extraction (SPE) coupled to high performance liquid chromatography with fluorescence detection was developed for the determination of malachite green (MG) in water samples. MG in water samples was reduced completely to leucomalachite green (LMG) with KBH4. The water samples were purified and enriched with MCX solid-phase extraction cartridges. MG was successfully separated on an Agilent C18 analytical column using a mobile phase consisting of 0.05 mol/L ammonium acetate and acetonitrile (20:80,V/V). Under the optimal conditions, the developed calibration curve was linear in the range of 0.005－0.5 μg/mL for MG with a detection limit of 0.05 μg/L. The mean average recoveries for MG at spike levels of 0.200, 1.00 μg/L and 5.00 μg/L were in the ranges of 91.7%－92.6% in pool water, 87.4%－94.6% in river water, 84.1%－92.6% in sea water, with relative standard deviations (RSD) of 4.5%－5.9%, 2.8%－4.1% and 5.4%－6.5%, respectively. The results show that this method is sensitive, accurate and suitable for the determination of MG residues in water samples.

Key words: malachite green, solid phase extraction, high performance liquid chromatography, water

中图分类号:

O 657.7+2

邓建朝，李来好，杨贤庆*，岑剑伟，辛少平，魏涯，吴燕燕. 固相萃取-高效液相色谱-荧光检测法测定水体中孔雀石绿[J]. 食品科学, 2012, 33(14): 150-153.

Deng Jian-Ming Laihao LI Xianqing YANG WU Yan-Yan Sheng-Jun CHEN. Determination of Malachite Green in Water Using Solid Phase Extraction-High Performance Liquid Chromatography with Fluorescence Detection[J]. FOOD SCIENCE, 2012, 33(14): 150-153.

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