CE-UV-Vis法测定鲫鱼中结晶紫.pdf

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CE-UV-Vis法测定鯽鱼中结晶紫
肖虎鹏2,周小理,韩生,何忠义2,熊丽萍2
(1.上海应用技术学院新能源材料研究室,上海200225;2.华东交通大学,江西南昌330013)
摘要:用毛细管电泳(CE)-紫外可见(UV-Vis)检测法测定鱼中结晶紫残留量的新方法。样品
中的结晶紫用硼氢化钾还原为其代谢产物隐色结晶紫;鱼样品用乙腑提取,二甲烷革取,浟编
净化后用毛细管电泳进样检测,外标法定量。結果表明:该方法能有效用于卿鱼中结晶紫的分析检
测。其最佳测定条件为:流动相,100mmol/L磷酸一磷酸二氢钠變冲溶液(pH4.0);紫外检测波长
267nm;分离电压为12kV。结晶紫标准工作液浓度范国为1~32ug/mL时线性关系良好,相关
系数为0.942。方法检出限和定量检出限均为2.9xg/kg。空白样品结晶紫添加水平为5、10、20
g/mL时平均回收率分别为83.97%、109.55%和88.45%,相对标准偏差分别为3.22%、5.05%
和2.09%。
关键词:毛细管电泳;结晶紫;隐色结晶紫;鱼
中图分类号:0657.8
文献标志码:A
文章编号:0367-6358(2012)01-0019-05
Determination of Crystal Violet in Carp by Capillary
Electrophoresis with Ultraviolet Visible Detection
XIAO Hu-peng'=, ZHOU Xiao-li, HAN Sheng*, HE Zhong yi?, XIONG Li-ping
(1. New Energy Material Lab, Shanghai Institute of Technology, Shanghai 200235, Chinas
2. School of Basic Science, East Chira Jiaotong University, Jianxi Nanchang 330013, China)
Abstract: A new method was established to analysis crystal violet(CV) residues in carp. Crysai violet in
samples was reduced to its metabolite leuco-crysial violet with potassium borohydride. The carp samples
were firstly extracted with acetonitrile and dichhoromethane in sequence, then followed by concentration
and purification, finally detected with capillary electrophoresis(CE) using external standard method for
quantitative analysis. The results show that CE-UV-VIS could effectively analyse crystal violet in carp. The
optimum conditions were as follow: mobile phase, 100 mmol/L phosphate-sodium dihydrogen phosphate
buffer solution (PH4. 0); UV detection wavelength, 267 nm; separation voltage of 12 kv. The linear
relationship was good when the crystal violet concentration range of standard working liquid was between 1
and 32 mg/ml, and the correlation coefficien was 0. 9942. The detection threshold(CC) and the detection
capability (CC ) were both 2.9 pg/kg. The precision of the method, expressed as RSD (n=6) values for
the within-laboratory reproducibility, at the three add levels of LCV(5, 10 and 20 ug/kg), were.22%
05% and 2.09%, respectively, and the average recoveries were.97%, 109.55% and 83.45%
respectively.
Key words: capillary electrophoresis(CE); crystal violet(CV); leuco-crystal violet(LCV); gentian violet
(GV); leuco-gentian violet(GV); carp
收稿日期:2011-03-04;修回日期:2011-09-23
基金项目:國家自然科学基金资助(2011976105);上海市科学技术委员会资助(09QT1400600
作者简介;肖虎鹏(1985~),男,湖北天门人,硕士生。-mail:xiaohupeng2@163.com*联系人:Tel:021-64941192,E
hansheng654321(@sina.com