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超高效液相色谱-三重四极杆/线性离子阱复合质谱法测定鸡蛋中黏菌素残留的研究
尹晖,王亦琳,叶妮,孙红洋,孙雷
0
(中国兽医药品监察所)
摘要:
建立了鸡蛋中黏菌素残留检测的超高效液相色谱-三重四极杆/线性离子阱复合质谱方法(UPLC -QTRAP)。样品用25%甲醇提取后,正己烷去脂,固相萃取柱净化,上机测试。液相色谱条件:色谱柱为BEH C18(50 mm×2.1 mm,1.7 μm),流动相为0.5%甲酸水溶液+0.5%甲酸乙腈溶液,梯度洗脱,流速为0.4 mL/min,柱温为30 ℃,进样量为5 μL。质谱条件:电喷雾正离子源(ESI+),采用多反应监测-信息依赖扫描-增强子离子扫描(MRM-IDA-EPI)方式采集。结果表明:在鸡蛋中,黏菌素A和黏菌素B在20~800 ng/kg基质匹配标准溶液浓度范围内均呈现良好的线性关系,相关系数(R2)大于0.990;鸡蛋中黏菌素A和黏菌素B的定量限均为30 μg/kg,检测限为10 μg/kg。鸡蛋中黏菌素A和黏菌素B在30、150和300 μg/kg三个添加浓度平均回收率都在67.2%~106%之间,批内、批间RSD均小于20%。该方法定性准确、灵敏度高、简便快捷,回收率和精密度满足残留检测要求。
关键词:  黏菌素  鸡蛋  残留  液相色谱-三重四极杆/线性离子阱复合质谱
DOI:
投稿时间:2020-08-28修订日期:2021-05-27
基金项目:
Determination of Colistin Residue in Eggs by LC-QTRAP
(China Institute of Veterinary Drug Control)
Abstract:
A LC-QTRAP method was established for the determination of Colistin residue in Eggs. The samples were extracted by water(25% methanol), the fat was removed by hexane, and purified with C18 SPE. LC conditions were as follows: the chromatography column is BEH C18 column of 50 mm×2.1 mm, 1.7 μm;mobile phase is water(0.5% formic acid)and acetonitrile(0.5% formic acid); flow rate is 0.4 mL/min; column temperature is 30 ℃; injection volume is 5 μL. Mass spectrometry conditions were ESI+ and Multi-reaction Monitoring-Information Dependent Acquisition-Enhanced Product Ion (MRM -IDA - EPI) mode. The calibration curve of Colistin were good linear from 20 to 800 ng/kg in Eggs with the correlation coefficient R2 over 0.990. The limit of quantification was 30 μg/kg,and the limit of detection was 10 μg/kg. The average recoveries of Colistin from spiked Eggs at three concentrations of 30, 150 and 300 μg/kg were between 60%~120%, and intra- and inter-batch RSD were <20%.
Key words:  Colistin  Eggs  Residue  LC-QTRAP

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