摘要
建立了动物性食品中肝脏、肾脏组织氯霉素残留检测的超高效液相色谱-串联质谱(UPLC-MS/MS)分析方法。样品用β-葡萄糖醛酸苷酶酶解后乙酸乙酯提取,C18(500mg/3cc)固相萃取柱净化,液相色谱-串联质谱负离子模式测定,内标法定量。结果表明:氯霉素在0.5~10.0ng/mL的系列浓度范围内均呈良好线性关系,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。本方法氯霉素在0.2、0.4、2μg/kg的添加浓度范围内,平均回收率均为70%~120%,相对标准偏差(RSD)均小于20%。该方法具有操作简便快捷、结果灵敏度高、准确度高等优点。
Anuhra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was established for the determination of chloramphenicol in liver and kidney tissues of animal derived food.The sample was hydrolysised by β-glucuronidase enzyme, extracted with ethyl acetate, purified by C18 (500mg/3cc) solid phase extraction and measured by internal standard method with negative ion mode of liquid chromatography- tandem mass spectrometry determination. The calibration curves was good linear between the peak areas and the concentrations of 0.5- 10.0 ng/mL, and the correlation coefficients (r) was more than 0.990. The limit of detection of chloramphenicol was 0.1 μg/kg, and the limit of quantification was 0.2 μg/kg. The average recoveries of chloramphenicol ranged from 70% to 120% . The RSD of method was less than 20%.
出处
《中国兽药杂志》
2014年第4期43-47,共5页
Chinese Journal of Veterinary Drug
基金
农业行业标准制定与修订[(2013)91]