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

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。

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

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.