超声波萃取-PSA净化-气相色谱法测定水产品中氯霉素

Determination of Chloramphenicol and Florfenicol in Fishery Products by Gas Chromatography Combined with Ultrasonic Extraction and PSA Purification

建立了测定水产品中氯霉素的气相色谱电子捕获检测方法（GC-ECD）。样品通过乙酸乙酯超声波萃取,正己烷初步净化后,经过适量的N-丙基乙二胺（PSA）固相吸附剂进一步净化,硅烷化试剂衍生,再采用GC-ECD法检测,外标法定量。结果表明,氯霉素在1.5-100μg/L浓度范围内,组分含量与峰面积呈线性相关,相关系数分别为0.9996,检出限为0.1μg·kg-1。氯霉素在不同基质的水产品（鳗鲡、鳜鱼、大管鞭虾）中不同浓度水平的加标回收率分别为92%-103%、86%-108%和78%-99%,相应的相对标准偏差（RSDs）分别为3.5%-4.2%、3.1%-4.6%和2.6%-3.9%（n=5）。本方法简单快速,基体干扰小,线性范围宽,灵敏度、准确度、精密度能满足水产品中氯霉素的含量分析。

A simple, efficient, sensitive, and low matrix interference method for determination of chloram- phenicol（CAP） in fishery products using gas chromatography-electron capture detector（GC-ECD） has been developed. The samples were treated by ultrasonic extraction with ethyl acetate and n-hexane purification. Further purification of the extracts was processed by a moderate amount of primary secondary amine （PSA） sot-bent. Then the purified solutions were derivatized with slilyl reagents. The linearity of the method ranged from 1.5 to 100 μg/L for CAP, with correlation coefficient of 0.999 6. The limits of detection was 0.1 μg·kg-1. The recoveries of spiked CAP with external calibration method at different concentration levels in different matrix of samples （eel, mandarin fish, and Solenocera melantho） were 92%-103%, 86%-108%. and 78%-99%. respectively, and with relative standard deviations of 3.5%-4.2%, 3.1%-4.6%, and 2.6%-3.9%（n=5）, respectively. It is concluded that this method can be successfully applied for the determination of CAP in fishery products.