摘要
为了检测氯霉素在家禽组织中的残留量,本文建立了一种超高效液相色谱-串联质谱（UPLC-MS/MS）分析方法.通过对肌肉和鸡蛋样品采用碱性乙酸乙酯提取,20％甲醇水饱和正己烷液萃取净化,对鸡的肝脏和肾脏样品采用β-葡萄糖醛酸苷酶酶解后采用乙酸乙酯提取,C18固相萃取柱（500 mg/3cc）净化,进行液相色谱-串联质谱负离子模式测定.结果表明,氯霉素在0.5～10.0 ng/mL范围内均呈现良好的线性关系,相关系数（r）均大于0.990;样品中氯霉素的检测限为0.1μg/kg,定量限为0.2μg/kg.UPLC-MS/MS对氯霉素在0.2、0.4、2μg/kg范围内的平均回收率均为70％～ 120％,相列标准偏差均小于20％.
High performance liquid chromatography-tandem mass spectrometry （UPLC-MS/MS）method was established by optimized conditions for determination of chloramphenicol residues in chicken tissues. Muscle and eggs samples were extracted with ethyl acetate and purified by hexane saturated 20% methanol, liver and kidney samples were hydrolysised by β-glucuronidase enzyme,extracted with ethyl acetate,purified by C18 solid phase extraction column （500mg/3cc）, then they were measured by internal standard method with negative ion mode of performance liquid chromatography-tandem mass spectrometry determination.The calibration curves were good linear between the concentrations of 0.5 to 10.0 ng/mL, and the correlation coefficients （r） were more than 0.990. The detection limit of chloramphenicol was 0.1 μg/kg,and the quantification limit was 0.2 μg/kg. The average recoveries of chloramphenicol were ranged from 70% to 120%. The RSD of method was less than 20%.
出处
《中国家禽》
北大核心
2014年第14期30-34,共5页
China Poultry
基金
山东省自主创新专项(2013CXC90202)
