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

Determination of Six Kinds of Antibiotic Residues in Eggs by High Performance Liquid Chromatography-Tandem Mass Spectrometry

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。

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 0.4~20.0μg·kg^(-1),and amoxicillin in the mass fraction range of 4~200μg·kg^(-1),with r>0.998.The detection limits were between 0.1μg·kg^(-1)and 2.0μg·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 10μg·kg^(-1),and the spiked levels of amoxicillin was 10,20 and 50μg·kg^(-1).The proposed method is simple,fast,low-cost,accurate and reliable,which is suitable for rapid determine of various antibiotics in eggs.