分散固相萃取净化-气相色谱法测定水产品中氯霉素和氟苯尼考

Determination of Chloramphenicol and Florfenicol in Fishery Products by Using Dispersive Solid Phase Extraction and Gas Chromatography

建立测定水产品中氯霉素和氟苯尼考的气相色谱-电子捕获检测方法.样品通过乙酸乙酯萃取、正己烷初步净化后,经过分散固相萃取进一步净化、硅烷化试剂衍生,再采用气相色谱-电子捕获法检测、外标法定量.结果表明：氯霉素、氟苯尼考分别在1.5～100 μg/L、6～400 μg/L范围内,组分含量与峰面积呈线性相关,相关系数分别为0.998 1和0.999 7,检出限分别为0.1、0.3 μg/kg.氯霉素和氟苯尼考在不同基质的水产品（鲫鱼、青蟹、南美白对虾）中不同加标水平回收率分别为82％～106％、87％～111％和91％～98％,相对标准偏差分别为2.3％～4.9％、2.4％～4.5％和1.4％～4.1％（n=5）.本方法基体干扰小、线性范围宽,灵敏度、准确度、精密度能满足水产品中氯霉素类药物的含量分析.

An efficient,sensitive,and low matrix interference method for the determination of chloramphenicol （CAP） and florfenicol （FF） in fishery products using gas chromatography-electron capture detector （GC-ECD） has been developed.Samples were treated by extraction with ethyl acetate and n-hexane purification.Further cleanup of the extracts was processed by a modified dispersive solid phase extraction procedure.Then,the purified solutions were derivatized with slilyl reagents.The linearity of the method ranged from 1.5 to 100 μg/L for CAP,and from 6 to 400 μg/L for FF,with correlation coefficients ranging between 0.998 1 and 0.999 7.The limits of detection were 0.1-0.3 μg/kg.The recoveries of spiked CAP and FF with external calibration method at different concentration levels in different sample matrixes （crucian,blue crab,and Penaeus vannawei） were 82％-106％,87％-111％,and 91％-98％,respectively,with relative standard deviations of 2.3％-4.9％,2.4％-4.5％,and 1.4％-4.1％ （n =5）,respectively.Thus it is concluded that this method can be successfully applied for the determination of choramphenicols （CAPs） in fishery products.