超高效液相色谱-串联质谱法测定鸡组织中氯苯胍残留

Determination of robenidine residue in chicken tissues by ultra performance liquid chromatography- tandem mass spectrometry

关键词:  氯苯胍  残留  超高效液相色谱-串联质谱法

Key words:  robenidine  residues  UPLC-MS/MS

摘要:

研究建立了鸡组织中氯苯胍残留的超高效液相色谱-串联质谱检测方法。样品经酸化乙腈提取后,分别经中性氧化铝柱和HLB固相萃取柱净化,C₁₈柱分离,超高效液相色谱-串联质谱测定,外标法定量。氯苯胍在10 ng/mL～500 ng/mL的浓度范围内呈线性相关,相关系数为0.994以上。本方法对氯苯胍在鸡组织中的检测限为5μg/kg,定量限为10μg/kg；鸡肉、鸡肝和鸡肾在添加50μg/kg～200μg/kg浓度范围内,其回收率为76.7%～107.6%,鸡脂肪和鸡皮在添加100μg/kg～400μg/kg浓度范围内, 其回收率为81.2%～106.8%, 批内变异系数均在1.4%～19.5%之间,批间变异系数在2.5%～12.8%之间。本方法快速、灵敏、重现性好,各项技术指标均满足国内外相关法规要求,适用于鸡组织中氯苯胍的残留检测。

Abstract:

A method based on ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was developed for the determination of robenidine residues in chicken tissues. The analyte was extracted with acidic acetontrile, and purified by neutral Alumina and HLB solid phase extraction cartridge. Quantification of the analyte was achieved by UPLC-MS/MS with multiple reaction monitoring (MRM) using external standard method. Limit of detction is 5μg/kg ,and the limits and quantification is10μg/kg.The overall recovery varies from 76.7%～107.6% at the spiked level of 50μg/kg～200μg/kg in muscle, liver and kindey, and from 81.2%～106.8% at the spiked level of 100μg/kg～400μg/kg in fat and skin, the intra-and inter-batch coefficients was from 1.4%～19.5% and from 2.5%～12.8%, respectively. The method was reliable, sensitive and reproducibility, its performance can meet the requirements of the domestic and international legislation．The method adapts to the determination of robenidine residues in chicken products.