摘要
目的:建立超高效液相色谱-串联质谱法(UPLC-MS/MS)对鸡蛋中氯霉素和氟苯尼考残留量检测方法。方法鸡蛋中的氯霉素、氟苯尼考残留物通过制备、提取、净化、氮吹、复溶,过滤后进液相色谱-串联质谱仪进行分析测定。采用C18色谱柱,以水-乙腈溶液为流动相梯度洗脱分离目标物,氯霉素采用内标法定量,氟苯尼考采用外标法定量。结果:通过测试氯霉素、氟苯尼考检出限(LOD)为:0.05μg/kg,定量限(LOQ)为:0.1μg/kg。在鸡蛋中添加1×LOQ,2×LOQ,10×LOQ等3个浓度的两种物质,平均回收率在85.3%~105.8%,相对标准偏差范围为3.90%~9.45%,线性范围为:0.5~250ng/mL。结论:通过改进和优化,本方法更加简便、快捷、准确的测定鸡蛋中的氯霉素、氟苯尼考。
Objective:A method for determination of chloramphenicol and florfenicol residues in eggs by UPLC-MS/MS was established.Methods:Chloramphenicol and florfenicol residues in eggs were determined by liquid chromatography-tandem mass spectrometry after preparation,extraction,purification,nitrogen blowing,redissolution and filtration.The target substances were separated by gradient elution on C18 column with water and acetonitrile solution as mobile phase.Chloramphenicol was quantified by internal standard method and florfenicol was quantified by external standard method.Results:The lowest detection concentration(LOD)of chloramphenicol and florfenicol was 0.05μg/kg,and the limit of quantification(LOQ)was 0.1μg/kg.Two compounds were added to eggs at three concentrations:1×LOQ,2×LOQ and 10×LOQ,the average recovery was 85.3~105.8%,the relative standard deviation was 3.90%~9.45%,and the linear range was 0.5~250 ng/mL.Conclusion:Through improvement and optimization,this method is more simple,rapid and accurate for the determination of chloramphenicol and florfenicol in eggs.
作者
刘洋
邢海艳
苏晶
吴旭
吴义春
孙丽
LIU Yang;XING Hai-yan;SU Jing;WU Xu;WU Yi-chun;SUN Li(Huai′an Institute for Food and Drug Control,Huai′an 223300)
出处
《中国食品添加剂》
CAS
北大核心
2021年第5期101-106,共6页
China Food Additives
关键词
氯霉素
氟苯尼考
液相色谱-串联质谱法
鸡蛋
残留
chloramphenicol
florfenicol
liquid chromatography-tandem mass spectrometry
eggs
residues