QEChERS提取与高效液相色谱-电喷雾电离串联质谱联用法快速检测食品中氯霉素类物质的残留量

Quick Determination of Chloramphenicols Residues in Foods by QuEChERS Extraction and High Performance Liquid Chromatography-mass/Mass Spectrometry

本文建立一种QuEChERS提取与高效液相色谱-串联质谱法(high performance Liquid chromatography-mass/mass spectrometry,HPLC-MS/MS)快速测定食品中氯霉素类物质残留量的方法。样品经酸性乙腈提取,经C18色谱柱分离,甲醇-5 mmol乙酸铵溶液梯度洗脱,采用电喷雾负离子模式多反应监测,内标法定量。氯霉素的浓度在0.1~200μg·L^-1以内与峰面积呈线性关系,检测定量限可低至0.1μg·kg^-1。取空白样品在0.01,0.05,0.1μg·kg^-1三个标准加入水平下进行了加标回收和精密度测试试验,回收率在81%~120%范围之间,相对标准偏差在1.5%~3.8%范围之间。该方法快速简便,准确性强,灵敏度高,适合实验室大批量食品中氯霉素类物质残留量的测定。

A quick method by high performance Liquid chromatography-mass/mass spectrometry was established for determining chloramphenicols in foods.Chloramphenicols residues were extracted with acid acetonitrile,purified by QuEChERS adsorbent and separated by C18 chromatographic column with gradient elution using the mobile phase made up of methanol and 5mmol ammonium acetate.The identification and quantification analysis was carried out in negative electro-spray ionization(ESI-),and the quantification analysis was performed by internal standard method.The calibration curve of chloramphenicol showed a good linearity in the concentration range of 0.1~200μg·L^-1 and the quantification limit was as low as 0.1μg·kg^-1.The recoveries at the three spiked levels of 0.01,0.05,0.1μg·kg^-1 were in the range of 81%~120%and the relative standard deviations were between 1.5%and 3.8%.This method is quick,simple,effective and sensitive,and it is suitable for mass determination works of chloramphenicols residues in foods.