加压毛细管电色谱法测定鳗鱼中5种磺胺类药物残留  

Simultaneous Determination of Five Sulfonamide Residues in Eel Products by Pressurized Capillary Electrochromatography

作　　者：董洁莹[1] 欧阳小琨[1] 曹国洲[2] 朱晓艳[2] 王阳光[1] 杨立业[1] 

机构地区：[1]浙江海洋学院食品与药学学院,浙江舟山316004 [2]宁波出入境检验检疫局,浙江宁波315012

出　　处：《浙江海洋学院学报（自然科学版）》2011年第5期392-396,共5页Journal of Zhejiang Ocean University(Natural Science Edition)

基　　金：浙江省科技厅科技计划项目(2009C14024;2011C22073);浙江省自然科学基金(Z3100533;Y2111223);十一五国家科技支撑计划(2009BADB9809-2);舟山市科技计划项目(10245);浙江省科技厅新苗计划

摘　　要：建立了加压毛细管电色谱(pCEC)法同时测定鳗鱼中磺胺嘧啶、磺胺间甲氧嘧啶、磺胺喹噁啉、磺胺甲噁唑、磺胺二甲异噁唑5种磺胺类药物残留的分析方法。样品均质后经乙酸乙酯提取,无水硫酸钠脱水,HLB固相萃取柱净化,最后利用加压毛细管电色谱进行检测。通过优化有机相的比例,流动相中的盐浓度和电压等色谱条件,使5种药物的出峰时间控制在6.5 min内。结果表明:5种磺胺类药物在0.5～5μg/mL浓度范围内线性关系良好(R>0.999 0),磺胺嘧啶、磺胺间甲氧嘧啶检出限为0.02 mg/kg;磺胺喹噁啉的检出限为0.03 mg/kg;磺胺甲噁唑、磺胺二甲异噁唑的检出限为0.04 mg/kg。在鳗鱼空白样本中加标浓度分别为2 mg/kg、5 mg/kg,5种药物相应的回收率在71%～82%之间,该法快速、准确,能够满足日常检测需要。A pressurized capillary electrochromatography（pCEC） method was developed for the determination of five sulfonamides,including a sulfadiazine,sulfamonomethoxine sodium,sulfachinoxalin,sulfamethoxazole,sulfisoxazole in products of eel.The sample was extracted by ethyl acetate.The extracts were dehydrated with sodium sulphate anhydrous.After the ethyl acetate extraction was purified and concentrated by HLB cartridges,then determined by pCEC.The effects of ratio of organic phase,mobile phase salt concentration and separation voltage on separation efficiency were investigated,respectively;the peak flowing out time could control within 6.5 minutes.The calibration curve of simultaneous was lined under the content of 0.5-5 μg/mL,with correlation higher than 0.999 0.The limit of detection（LOD） for sulfadiazine,sulfamonomethoxine sodium was 0.02 mg/kg,for sulfachinoxalin was 0.03 mg/kg and that for sulfamethoxazole,sulfisoxazole was 0.04 mg/kg.The mean recoveries varied from 71% to 82% at two spiked levels of 2 and 5 mg/kg.This method is accurate,rapid and able to meet the testing requirements.

关 键 词：加压毛细管电色谱 磺胺 鳗鱼 

分 类 号：O651.8[理学—分析化学]