超高效液相色谱-串联质谱法测定鸡肉和鸡蛋中氯霉素和甲硝唑  

Rapid determination of chloramphenicol and metronidazole in chicken and egg by ultra performance liquid chromatography-tandem mass spectrometry

作　　者：徐飞[1] 刘峰[1] 张亚军[1] 关光玉[1] 

机构地区：[1]宁夏回族自治区疾病预防控制中心,宁夏银川750004

出　　处：《中国食品卫生杂志》2016年第6期759-762,共4页Chinese Journal of Food Hygiene

基　　金：宁夏自然科学基金资助项目(NZ14226)

摘　　要：目的建立超高效液相色谱-串联质谱法检测鸡肉和鸡蛋中的氯霉素和甲硝唑。方法鸡肉和鸡蛋样品经乙腈沉淀蛋白,乙酸乙酯和乙腈同时提取,Oasis MCX柱净化,以乙腈-水为流动相,采用ACQUITY BEH C18（2.1 mm×100 mm,1.7μm）色谱柱分离,分别以电喷雾负离子和正离子模式进行质谱测定,内标法定量。结果分别以鸡肉和鸡蛋为加标基质,三个加标水平下氯霉素和甲硝唑的平均回收率为96.3%~110.5%,相对标准偏差小于7.0%,氯霉素和甲硝唑的检出限（S/N=3）为0.1μg/kg,定量限（S/N=10）为0.3μg/kg。结论该方法操作快速简单、重现性好,可用于鸡肉和鸡蛋中氯霉素和甲硝唑的含量测定。Objective To develop a rapid method for determination of chloramphenicol and metronidazole in chicken and egg by ultra performance liquid chromatography-tandem mass spectrometry（ UPLC-MS / MS） and provide analytical methodology for chicken and egg in Ningxia. Methods Samples of chicken and eggs were protein precipitated with acetonitrile,then extracted by ethyl acetate and acetonitrile,and cleaned up by Oasis MCX column. Chloramphenicol and metronidazole were separated on ACQUITY BEH C18 chromatographic column（ 2. 1 mm × 100 mm,1. 7 μm） with mobile phase of acetonitrile-water on gradient elution,then determined and quantified by mass spectrometry. Results Average recoveries of chloramphenicol and metronidazole at three spiked levels were 96. 3%-110. 5% with relative standard deviations less than 7. 0%. The limit of detection（ LOD） and limit of quantification（ LOQ） for both chloramphenicol and metronidazole were 0. 1 μg / kg and 0. 3 μg / kg. Conclusion The method was accurate,reliable,and could be used as a quality control method for chloramphenicol and metronidazole in chicken and egg.

关 键 词：超高效液相色谱-串联质谱 鸡肉 鸡蛋 氯霉素 甲硝唑 食品污染物 兽药残留 食品安全 

分 类 号：R155.5[医药卫生—营养与食品卫生学] O657.63[医药卫生—公共卫生与预防医学]