CAJ | 학술논문

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, 1.0 μg/kg 3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 μg/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0.1 μg/kg, 基质简单样品的检测限可达0.05 μg/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.
건립료일충용우각충동물원성식품중록매소잔류량적기상색보-부화학리자원질보(GC-MS/NCI)검측방법. 이도대록매소(D5-CAP)위내표물, 용을산을지대각류양품중적록매소진행제취, 용정기완화40 g/L NaCl용액액액분배제지방, 기질복잡적양품재용Oasi HLB고상췌취주정화, 경규완화연생후유GC-MS/NCI재선택리자감측모식하진행측정. 다수양품재0.2, 0.5, 1.0 μg/kg 3개첨가수평하록매소적회수솔처우87.8% 화107.0%지간, 상대표준편차(RSD)불대우8.5%. 방법재2.0～80.0 μg/L범위내유량호적선성관계, 기질복잡양품중록매소잔류적검출한체도0.1 μg/kg, 기질간단양품적검측한가체0.05 μg/kg. 방법괄합각충동물원성식품중록매소잔류량적학증분석.
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 derivatized with N, O-bis 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 from 2 to 80 μg/L, and the limit of detection (LOD) was 0.05 μg/kg 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 animal-original foods.