GC-MS/NCI稳定同位素稀释技术检测动物源性食品中氯霉素的残留量  

Determination of chloramphenicol residue in animal-original foods by gas chromatography-negative chemical ionization mass spectrometry using stable isotope dilution technique

作　　者：潘玉香[1] 董静[1] 吕建霞[1] 孙军[1] 张靖[1] 任芳[1] 马小杰[1] 

机构地区：[1]潍坊出入境检验检疫局,潍坊261041

出　　处：《分析试验室》2010年第2期105-110,共6页Chinese Journal of Analysis Laboratory

摘　　要：建立了一种用于各种动物源性食品中氯霉素残留量的气相色谱-负化学离子源质谱（GC-Ms／NcI）检测方法。以氘代氯霉素（D5．CAP）为内标物，用乙酸乙酯对各类样品中的氯霉素进行提取，用正己烷和40g/LNaCl溶液液液分配除脂肪，基质复杂的样品再用OasiHLB固相萃取柱净化，经硅烷化衍生后由GC．MS／NCI在选择离子监测模式下进行测定。多数样品在0．2，0．5，1．0μg／kg3个添加水平下氯霉素的回收率处于87．8％和107．0％之间，相对标准偏差（RSD）不大于8．5％。方法在2．0～80．0耐L范围内有良好的线性关系，基质复杂样品中氯霉素残留的检出限达到0．1μg／ks，基质简单样品的检测限可达0．05μg／kg。方法适合各种动物源性食品中氯霉素残留量的确证分析。A method is developed for the determination of chloramphenicol residue in diverse animal foods/animal-original foods by gas chromatography-negative chemical ionization mass spectrometry （GC-MS/NCI） with/using deuterium chloramphenicol （D5-CAP） as an internal standard. Chloramphenicol residue was extracted with ethyl acetate from different animal-original foods, the fat was removed with n-hexane and NaCl, the Oasi HLB cohmm was used to clean the more complex sample extract. After the sample extract was derivatized with N, O-bis （trimetlysilyl） trifluoroacetamide-trimethylchlorosilane （99：1） and determined by GC-MS/NCI in selected ions monitoring mode. The recoveries of chloramphenicol were in the range from 87.8% to 107.0% at three spiked levels, 0.2 μg/kg, 0.3 μg/kg and 0.5 μg/kg, and the relative standard deviations （RSDs） were below 8.5%. The linearity of the method is good from2 to 80μg/L, and the limit of detection （LOD） was O. 05μkg for the simple samples, and 0.10 μg/kg for the complex samples. The method is suitable for the determination and validation of chloramphenicol residue in all kinds of animaloriginal foods.

关 键 词：气相色谱-质谱联用 负化学离子源 氯霉素 动物源性食品 

分 类 号：O557.63[理学—热学与物质分子运动论]