分子印迹固相萃取—高效液相色谱法检测鱼肉中的孔雀石绿和结晶紫  

Determination of malachite green and crystal violet in fish

作　　者：肖琴[1] 林一[1] 郑琳[1] 廖勇[1] 张奎[1] 

机构地区：[1]中山大学公共卫生学院,广东广州510080

出　　处：《粮油食品科技》2011年第6期31-34,共4页Science and Technology of Cereals,Oils and Foods

基　　金：广东省医学科学技术研究基金项目资助(B2008021)

摘　　要：将分子印迹固相萃取和高效液相色谱法联用,建立一种检测鱼肉中孔雀石绿和结晶紫及其代谢产物残留的新方法。以孔雀石绿为模板分子,甲基丙烯酸为功能单体,乙二醇二甲基丙烯酸酯为交联剂,本体聚合法合成分子印迹聚合物。并制成分子印迹固相萃取柱,优化分子印迹固相萃取的实验条件。鱼肉样品经过超声提取后,采用分子印迹固相萃取富集净化,用高效液相色谱法测定孔雀石绿和结晶紫及其代谢产物的残留量。该方法的线性范围孔雀石绿和结晶紫均为0.01～5μg/mL,隐色孔雀石绿和隐色结晶紫均为0.01～10μg/mL,相关系数为0.9943～0.9993,具有较好的线性关系;检出限孔雀石绿为0.12 ng/mL,结晶紫0.02 ng/mL,隐色孔雀石绿0.26 ng/mL,隐色结晶紫0.25 ng/mL。该方法对鱼肉样品的回收率为97.06%～111.83%,RSD为1.54%～10.49%。所建立的新方法简单快速、准确可行,而且有机溶剂用量少,被成功地应用于鱼肉中孔雀石绿和结晶紫及其代谢产物残留的测定。A new method of molecularly imprinted solid phase extraction （MISPE） combined with high performance liquid chromatography （HPLC） was developed for detecting malachite green （MG）, crystal violet （CV） and their metabolites leucomalachite green （LMG）, leucocrystal violet （LCV） in fish. Using MG as template molecule, methacrylic acid as functional monomer, ethylene glycoldimethacrylate as cross -linking agent, molecularly imprinted polymers were synthesized by bulk polymerization and made into extraction column. The significant parameters affecting MISPE were optimized. The fish samples were extracted with acetonitrile by ultrasonic extraction, and cleaned up on MISPE column. Then the residues of MG, CV, LMG and LCV were detected by HPLC. The result showed that linear response data were obtained in the concentration range of 0.01 - 5 p,g/mL for MG, CV and 0.01 - 10 ug/mL for LMG, LCV with correlation coefficients from 0. 9943 to 0. 9993. The limits of detection were 0.12 ng,/mL for MG, 0.02 ng/mL for CV,0.26 ng/mL for LMG and 0.25 ng/mL for LCV. The recovery rate of the fish samples was 97.06% -111.83% ,with the relative standard deviations ranging from 1.54% - 10.49%. The new established method is simple and fast, accurate and feasible, which can be successfully applied for the determination of MG, CV in fish and their metabolin with low solvent consumption.

关 键 词：分子印迹固相萃取 高效液相色谱法 鱼肉 孔雀石绿 结晶紫 

分 类 号：TS201.3[轻工技术与工程—食品科学] R115[轻工技术与工程—食品科学与工程]