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目的:研究了水产品中氯霉素残留量的ECD-气相色谱分析方法。方法:水产品中的氯霉素用乙酸乙酯提取、浓缩后用正己烷抽提脱脂。样液经C18固相萃取小柱净化,BSTFA+TMCS衍生后,用配有电子捕获检测器(ECD)的气相色谱仪测定,外标法定量,气相色谱-质谱法进行确证。结果:方法的最低检出浓度达到0.02μg/kg(S/N=3),在2.5～5000.0ng/ml浓度范围内,线性关系良好,相关系数r=0.9995,加标水平为1.0～10.0μg/kg时,回收率在86.3%～95.3%,相对标准偏差(RSD)为5.02%～9.04%。结论:该方法具有灵敏度高,样品提取简单等特点。
Objective: To study the method of ECD-GC for the determination of chloramphenicol residues in aquatic products. Methods: Chloramphenicol in aquatic products was extracted with ethyl acetate, concentrated and degreased with n-hexane. The sample was purified by C18 solid phase extraction cartridges. After BSTFA + TMCS derivatization, the sample was determined by gas chromatography with electron capture detector (ECD) and quantified by external standard method and confirmed by gas chromatography-mass spectrometry. Results: The minimum detectable concentration was 0.02μg / kg (S / N = 3). The calibration curve was linear in the range of 2.5-5000.0ng / ml, with a correlation coefficient of 0.9995 and a spiked level of 1.0-10.0μg / kg, the recoveries ranged from 86.3% to 95.3% and the relative standard deviations (RSDs) ranged from 5.02% to 9.04%. Conclusion: The method has the characteristics of high sensitivity and simple sample extraction.