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.
出处
《分析试验室》
CAS
CSCD
北大核心
2010年第2期105-110,共6页
Chinese Journal of Analysis Laboratory
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
Gas chromatography-mass spectrometry （GC-MS）
Negative chemical ionization （NCI）
Chlommpheni- col
Animal-original foods
