UPLC-MS/MS法检测动物性食品中肝脏、肾脏组织中氯霉素残留量

Determination of Chloramphenicol Residuesin Liver and Kidney Tissue of Edible Animal by UPLC-MS/MS

关键词:  动物肝脏、肾脏  氯霉素  残留  超高效液相色谱-串联质谱

Key words:  liver and kidney tissue  chloramphenicol  residue  UPLC - MS /MS

摘要:

建立了动物性食品中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0.1g/kg,定量限为0.2 g /kg。本方法氯霉素在0.2 μg/kg、0.4 μg/kg、2 μg/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%。该方法具有简便快捷、灵敏度高、定性准确等特点。

Abstract:

Anultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was established for the determination of chloramphenicol in Liver and Kidney Tissue of Edible Animal. The sample was hydrolysised by β-glucuronidase enzyme, extracted with ethyl acetate, purified by C18 (500mg/3cc) solid phase extraction (SPE), measured by internal standard method with negative ion mode of liquid chromatography-tandem mass spectrometry determination.The calibration curves were good linear between the peak areas and the concentrations of 0.5～10.0ng/mL, and the correlation coefficients (r) were more than 0.990. The limit of detection of chloramphenicol was 0.1g/kg,and the limit of quantification was 0.2 g/kg. The average recoveries o f chloramphenicol ranged from 70% to 120 % . The RSD of method was less than 20%.