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

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40 g/L NaCl溶液液液分配除脂肪,基质复杂的样品再用Oasi HLB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2.0~80.0μg/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/kg,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。

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

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 column was used to clean the more complex sample extract.After the sample extract was derivatize...