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高效液相色谱-串联质谱法快速测定鸡蛋中六种抗生素残留

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开发了一种高效液相色谱-串联质谱法(UPLC-MS/MS)快速检测鸡蛋中6种抗生素残留量的方法.样品分别用乙腈、1%甲酸乙腈和80%乙腈水(含1%甲酸)进行提取,提取液在40℃下氮气吹干后用50%乙腈水(含0.1%甲酸)溶液复溶,采用C18色谱柱分离,以电喷雾离子源在正、负离子多反应监测模式下进行测定.结果表明:6种抗生素用80%乙腈水(含1%甲酸)作为提取溶剂时回收率较高;甲硝唑、恩诺沙星、环丙沙星、替米考星、氟苯尼考在0.4~20.0μg·kg-1以及阿莫西林在4~200μg·kg-1的质量分数范围内与峰面积呈现良好的线性关系,r均大于0.998,检出限范围为0.1~2.0μg·kg-1;甲硝唑、恩诺沙星、环丙沙星、替米考星、氟苯尼考加标水平为2、5、10μg·kg-1以及阿莫西林加标水平为10、20、50μg·kg-1时,回收率为85.3%~115.0%,相对标准偏差为1.5%~4.0%.该方法前处理简单、快速,成本低,结果准确可靠,适用于鸡蛋中多种抗生素的快速测定.
Determination of Six Kinds of Antibiotic Residues in Eggs by High Performance Liquid Chromatography-Tandem Mass Spectrometry
A high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was developed for the fast detection of six antibiotic residues in eggs. Samples were extracted with acetonitrile, 1% formic acid acetonitrile and 80% acetonitrile water (containing 1% formic acid) respectively. The extract was dried by nitrogen at 40 ℃ and then redissolved with 50% acetonitrile water (containing 0.1% formic acid) solution. The samples were separated by C18 column and monitored by Tandem mass spectrometry with electrospray ion in positive and negative ion multi-reaction monitoring mode. The results showed that the recoveries of six antibiotics were higher when 80% acetonitrile water (containing 1% formic acid) was used as extraction solvent. Metronidazole, enrofloxacin, ciprofloxacin, tilmicosin and florfenicol showed a good linear relationship between mass concentration and peak area in the mass fraction range of 0.4 ~ 20.0 μg·kg-1, and amoxicillin in the mass fraction range of 4 ~ 200 μg·kg-1, with r > 0.998. The detection limits were between 0.1 μg·kg-1 and 2.0 μg·kg-1. The recoveries were ranged from 85.3% to 115.0% with the relative standard deviations of 1.5% ~ 4.0% when the spiked levels of metronidazole, enrofloxacin, ciprofloxacin, tilmicosin and florfenicol were 2, 5 and 10 μg·kg-1, and the spiked levels of amoxicillin was 10, 20 and 50 μg·kg-1. The proposed method is simple, fast, low-cost, accurate and reliable,which is suitable for rapid determine of various antibiotics in eggs.

Ultra performance liquid chromatography-tandem mass spectrometryAntibioticsEggs

董曼曼、王苑桃、孙晓、饶雅琨、李敏、王涛、李旸、孙闽子、梁静茹

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西安市食品药品检验所,陕西西安 710000

高效液相色谱-串联质谱 抗生素 鸡蛋

陕西省市场监督管理局项目陕西省市场监督管理局项目

2022KY132023KY17

2024

当代化工
中国石油抚顺石化公司,中国石化抚顺石油化工研究院,沈阳市医药和化工行业联合会

当代化工

CSTPCD
影响因子:0.412
ISSN:1671-0460
年,卷(期):2024.53(5)
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