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

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。

Simultaneous determination of residues of chloramphenicol,thiamphenicol and florfenicol in aquatic products by gas chromatographic method with electron capture detection

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.