柱前电化学衍生-高效液相色谱法测定鱼肉中结晶紫和隐性结晶紫  

Determination of crystal violet and leucocrystal violet residues in fish by HPLC with pre-column coulometric electrochemical derivation

作　　者：胡江涛[1,2] 俞凌云[1] 于刚[1] 帅培强[1] 张莹 吴孟茹 张琴[1] 

机构地区：[1]四川出入境检验检疫局检验检疫技术中心,成都610041 [2]食品安全检测(四川省)重点实验室,成都610041 [3]宜宾出入境检验检疫局,宜宾644000

出　　处：《分析试验室》2016年第3期297-300,共4页Chinese Journal of Analysis Laboratory

基　　金：国家质检总局科技计划项目(2014IK137)资助

摘　　要：建立了柱前电化学氧化还原衍生-高效液相色谱测定鱼肉中结晶紫（CV）及隐性结晶紫（LCV）残留量的方法。试样用体积分数0.5%乙酸乙腈溶液提取,酸性氧化铝吸附剂净化,乙腈和乙酸铵缓冲液（78∶22,V/V）等度洗脱,柱前库仑检测器500 m V电压下LCV衍生为CV,588 nm波长检测。CV,LCV含量在0.010～0.50 mg/L范围内线性良好（γ〉0.998）,检出限为2.0μg/kg,定量限为5.0μg/kg。加标回收率为86.0%～91.0%。方法精密度、正确度和检出限等性能指标均达到兽残分析的要求,可用于水产品中CV,LCV测定。A new high performance liquid chromatographic method with pre-column coulometric electrochemical derivation was developed for the analysis of crystal violet（ CV） and leucocrystal violet（ LCV） Residues in Fish.Sample was extracted by 0. 5% acetic acid and acetonitrile solution. Alumina-A clean-up was performed. LCV in the eluate was on-line derivatized by pre-column Coulometric Electrochemical Detector. LCV was transferred to CV at 500 m V,and detected at 588 nm. Under the optimized conditions,the calibration curve of CV and LCV showed good linearity in the range of 0. 010-0. 50 mg / L with correlation coefficient of 0. 998. The limit of detection was 2 μg / kg. The limit of quantitation was 5 μg / kg. The average recoveries ranged from 86% ～ 91%.The performance of the method such as precision,accuracy and the limits of detection meets the requirements of residues of veterinary drug analysis,and the method can be applied to the practical analysis of crystal violet and leucocrystal violet residues in fish.

关 键 词：柱前电化学衍生 结晶紫 隐性结晶紫 高效液相色谱 

分 类 号：TS207.3[轻工技术与工程—食品科学]