固相萃取-液相色谱法测定水产品中孔雀石绿结晶紫及其代谢产物  

DETERMINATION OF MALACHITE GREEN,GENTIAN VIOLET AND THEIR METABOLITES IN AQUATIC PRODUCTS BY SPE-HPLC

作　　者：张林田[1] 陈小雪[1] 梁希扬[1] 罗惠明[1] 苏建晖[1] 张胜举[1] 

机构地区：[1]汕头出入境检验检疫局,广东汕头515031

出　　处：《检验检疫科学》2006年第3期8-10,共3页Inspection and Quarantine Science

摘　　要：[目的]建立水产品中孔雀石绿、结晶紫及其代谢产物隐性孔雀石绿、隐性结晶紫的高效液相色谱分析方法。[方法]样品以乙酸钠-乙腈为提取剂,经二氯甲烷反提取、再经SPE柱净化、氰基柱分离和柱后衍生化、等度洗脱、HPLC-DAD测定、外标法定量。[结果]各标准曲线相关系数均≥0.999,2μg/kg、4μg/kg浓度水平加标回收率为70.0%～87.7%,RSD为4.9%～8.1%,检测低限均为2μg/kg。[结论]本法简便、快速,具有良好的重现性和准确性。A new SPE-HPLC method for the determination of the malachite green,gentian violet and their metabolites leucomalachite green, leucogentian violetin in aquatic products. Residues in sample were extracted with an acetonitrile-sodium acetate buffer mixture, further purified with methylene chloride and was cleaned up on SPE column. The compounds were separated on an LC cyano column and a PbO2 post-column for derivation, equal-gradient eluted, then determined by HPLC-DAD, quantified by external standard method. All the calibration curve＇s correlation coefficients were higher than 0.996with the average recoveries of 2μg/kg, 4μg/kg, spiked recoveries of 70.0%～87.7%,BSD of 4.9%～8.1%,the limit of detection of all compounds was less than 2μg/kg. The method is validated with respect to its simplicity, sensitivity with good repeatability and reproducibility.

关 键 词：液相色谱 SPE 水产品 孔雀石绿 结晶紫 

分 类 号：TQ225.23[化学工程—有机化工] S948[农业科学—水产养殖]