摘要
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 for the determination of chloramphenicol (CAP) residues in aquatic products by ECD gas chromatography.Methods:The CAP residue was extracted from aquatic products which with ethyl acetate and defatted by n-hexane after concentrated.The sample solution was cleaned up by solid phase extraction C 18 column, derived with BSTFA+TMCS(99+1) and analyzed by electron capture detector gas chromatography using external standard quantitation. At last validated by GC/MS.Results:The detection limit of this method was 0.02 μg/kg(S/N=3).The results showed a good linear (r=0.9995) in the concentration range of 2.5～ 5 000.0 ng/ml,the average recoveries(n=3) for spiked standards(1.0～ 10.0 μg/kg) were 86.3%～95.3%,the relative standard deviations were 5.02%～9.04%.Conclusion:The method is sensitive and simple.
出处
《中国卫生检验杂志》
CAS
2005年第6期672-674,共3页
Chinese Journal of Health Laboratory Technology
基金
珠海市科技计划项目(PC200310045)
