超高效液相色谱-串联质谱法测定禽蛋中氯霉素、甲砜霉素和氟甲砜霉素  

Determination of chloramphenicol,thiamphenicol and florfenicol in eggs using ultra-high performance liquid chromatography-tandem mass spectrometry

作　　者：杨洁 杨钊 于宙 李新荣 张军宁 张辉珍 

机构地区：[1]青岛市食品药品检验研究院,青岛266071

出　　处：《分析试验室》2016年第12期1463-1467,共5页Chinese Journal of Analysis Laboratory

摘　　要：采用超高效液相色谱-三重四极杆串联质谱,用多反应监测模式定量,建立了禽蛋中氯霉素、甲砜霉素和氟甲砜霉素同时测定的分析方法。添加氯霉素-d5作为内标进行定量,试样经过乙酸乙酯提取,三氯乙酸去蛋白,盐析,分离,再经正己烷去脂肪,省去固相萃取净化步骤,直接上机测定。氯霉素、甲砜霉素和氟甲砜霉素的检出限分别为0.03,0.03和0.015＂g/kg,定量限分别为0.10,0.10和0.05＂g/kg,3种化合物的加标平均回收率在90.5%-103.5%,相对标准偏差在2.1%-6.0%之间。方法能对禽蛋中的氯霉素类化合物进行检测分析。A method for the determination of chloramphenicol, thiamphenicol and florfenicol in eggs using ultrahigh performance liquid chromatography-Tandem Mass Spectrometry was described. Samples were spiked with chloramphenicol-d5 as internal standard and extracted with ethyl acetate. After the proteins were removed by trichloroacetic acid and the lipids were removed by n-hexane, the samples were directly detected without the requirement of solid phase extraction clean-up. The detection limits for chloramphenicol, thiamphenicol and florfenicol were 0.03,0.03 and 0.015 μg/kg, and the quantitative limits were 0.10,0.10 and 0.05 μg/kg, respectively. The spike recoveries were between 90.5% and 103.5 %, with relative standard deviations （ RSDs, n = 6） within 2.1% - 6.0%. This method has the advantages of easy operation, high sensitivity and accuracy.

关 键 词：超高效液相色谱-串联质谱 禽蛋 氯霉素 甲砜霉素 氟甲砜霉素 

分 类 号：TS207.3[轻工技术与工程—食品科学]