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毛细管电子捕获气相色谱法同时测定水产品中氯霉素、甲砜霉素和氟甲砜霉素残留
引用本文:吴明媛,杨姝丽,黎小正,韦信贤.毛细管电子捕获气相色谱法同时测定水产品中氯霉素、甲砜霉素和氟甲砜霉素残留[J].广西农业科学,2009,40(5):567-570.
作者姓名:吴明媛  杨姝丽  黎小正  韦信贤
作者单位:广西水产研究所,南宁,530021
基金项目:广西水产品药物残留监控项目 
摘    要:采用乙酸乙酯提取目标物,正己烷脱脂,微波辅助衍生化,建立了能同时测定水产品中氯霉素、甲砜霉素和氟甲砜霉素残留量的毛细管电子捕获气相色谱法(GC—ECD)。加标回收实验结果显示,氯霉素在1.0-200.0μg/L范围内、甲砜霉素和氟甲砜霉素在5.0~200.0μg/L范围内成良好的线性,相关系数均大于0.996;氯霉素、甲砜霉素和氟甲砜霉素的检出限分别为0.1、0.2和0.2μg/kg,回收率在79.2%-88.0%之间,相对标准偏差在2.0%-4.1%之间。表明该方法定性定量准确、检出限低、重现性好、省时省力,可以满足水产品中3种氯霉素类药物的多残留安全检测。

关 键 词:水产品  氯霉素  甲砜霉素  氟甲砜霉素  残留量  气相色谱

Simultaneous determination of residues of chloramphenicol,thiamphenicol and florfenicol in aquatic products by gas chromatographic method with electron capture detection
WU Ming-yuan,YANG Shu-li,LI Xiao-zheng,WEI Xin-xian.Simultaneous determination of residues of chloramphenicol,thiamphenicol and florfenicol in aquatic products by gas chromatographic method with electron capture detection[J].Guangxi Agricultural Sciences,2009,40(5):567-570.
Authors:WU Ming-yuan  YANG Shu-li  LI Xiao-zheng  WEI Xin-xian
Institution:Guangxi Fishery Research Institute;Nanning 530021;China
Abstract:A capillary gas chromatographic method with electron capture detection (GC-ECD) was developed for simultaneous determination of residues of chloramphenicol(CAP), thiamphenicol(TAP) and florfenicol(FF) in aquatic products. Samples were extracted with ethyl acetate, defatted with n-hexane and microwave oven was used for microwave-assisted derivatization of CAP, TAP and FF with BSTFA-TMCS. The analysis results of recovery demonstrated that the standard curves were linear in the ranges of 1.0-200.0 μg/L for CAP, and 5.0-200.0 μg/L for TAP and FF, respectively, and the correlation coefficients were r≥0.996. The detection limits were 0.1 μg/kg, 0.2 μg/kg and 0.2 μg/kg for CAP, TAP and FF, respectively, and the recovery was 79.2%-88.0% and the relative standard deviations were 2.0%-4.1%. These results indicated that GC-ECD had the characteristics of high sensitivity, low detection limits, good repeatability, saving time and labor, and could quantitate exactly with a relatively rapid and simple procedure, so it could meet the safe detection of residues of the three phenicols in aquatic products.
Keywords:aquatic products  CAP  TAP  FF  residue  gas chromatography  
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