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
发布时间:2018-06-02 07:37
本文选题:超高效液相色谱-串联质谱 + 禽蛋 ; 参考:《分析试验室》2016年12期
【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。
[Abstract]:A method for the simultaneous determination of chloramphenicol, sulfoxamphenicol and fluorsulfoxide in poultry eggs was established by using ultra-high performance liquid chromatography-triple quadrupole tandem mass spectrometry and multi-reaction monitoring mode. Chloramphenicol -d5 was added as internal standard for quantitative analysis. The sample was extracted by ethyl acetate, deproteinized by trichloroacetic acid, salted out, separated, and then removed by n-hexane. The detection limits of chloramphenicol, sulfoxamphenicol and flursulfoxamphenicol were 0.03 and 0.015 "g / kg, respectively, and the quantification limits were 0.100.10 and 0.05" g / kg 路kg ~ (-1), respectively. The average recoveries of the three compounds were 90.5% and 103.5%, respectively. The relative standard deviation was between 2.1% and 6.0%. Methods the chloramphenicol compounds in poultry eggs were detected and analyzed.
【作者单位】: 青岛市食品药品检验研究院;
【分类号】:TS253.7;O657.63
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