文档介绍：凝胶渗透色谱和固相萃取净化-气相色谱-负化学源质谱
测定羊肠衣中的氯霉素残留量
李锋格窦辉全晓盾姚伟琴
(新疆出入境检验检疫局技术中心,乌鲁木齐 830063)
摘要:[目的]建立了羊肠衣中氯霉素残留含量的分析方法。[方法]羊肠衣样品用乙酸乙酯提取,凝胶渗透色谱和固相萃取净化,净化后的提取物用BSTFA+TMCS衍生化,气相色谱-负化学源-质谱法(GC-NCI-MS)选择离子定量检测,内标法定量,间位氯霉素为内标物。[结果] %-%之间,%-%之间。检出限(LOD) ,测定低限(LOQ)。[结论]该法简便省时,自动化程度高,可以满足欧盟委员会决议2002/657/EC和2003/181/EC的要求。
关键词气相色谱-负化学源-质谱,凝胶渗透色谱,固相萃取,氯霉素,羊肠衣
Determination of Chloramphenicol residues in Sheep Casing by Gas Chromatography Negative Chemical Ionization Mass Spectrometry with Purification of Gel Permeation Chromatography and Solid Phase Extraction
Li Fengge Dou Hui Quan Xiaodun Yao Weiqin
(Xinjiang Entry-Exit Inspection and Quarantine Bureau of the Peopleˊs Republic of China,Urumqi,Xinjiang,830063,China)
Abstract: A method for analysis of Chloramphenicol(CAP) residues in sheep casing has been was extracted from samples with ethyl acetate and cleaned-up by Gel Permeation Chromatography(GPC) and Solid Phase Extraction(SPE).The extracts of purified were derivatised with BSTFA+TMCS .CAP was detection by Gas Chromatography negative chemical ionization(NCI)/selected ion monitoring (SIM) mode, quantitative analysis was carried out by using meta-CAP as internal mean recoveries of 5 standard fortified levels were between % and % with relative standard deviations between % and %.The limit of detection (LOD)was , and the limit of quantitation(LOQ) for CAP in sheep casing samples was
μg/ proposed method was simple, saving time and automatization .The method can be satisfied the latest EU requirements mission Decision 2002/657/EC and 2003/181/EC.
Key words: Gas Chromatography Negative Chemical Ionization Mass Spectrometry; Gel Permeation Chromatography;Solid Phase Extraction; Chloramphenicol; Sheep Casing
氯霉素(Choramphenicol,CAP)是一种广谱抗菌素,1947年第一次从链霉菌中分离,1949年人工合成。常用于人类及动物各种传染病的治疗,对多种病原菌有较强的抑制作用。氯霉素存在严重的毒副作用,能抑制人体骨髓造血功能,引起人类的再生障碍性贫血、粒状白细胞缺乏症、新生儿灰色综合症等疾病,因此动物源食品中的氯