HPLC-MS/MS测定猪肉和猪肝中氯霉素残留量的研究

建立高效液相色谱-串联质谱法(HPLC-MS/MS)检测猪肉和猪肝中氯霉素药物残留的分析方法。样品经4%的氯化钠溶液和乙腈提取并沉淀蛋白质,正己烷脱脂净化,乙酸乙酯液液萃取,再浓缩定容,上HPLC-MS/MS仪器,用Syncronis C18柱分离,以乙腈-水(40∶60)作为流动相,采用电喷雾离子源(ESI),负离子模式,多反应监测(MRM)方式检测,用氯霉素-D5作内标物来定量。在该试验条件下,氯霉素在1～15ng/mL浓度呈良好的线性关系,r=0.999 2,最低检出浓度为0.1μg/kg,样品的加样回收率在90.0%～110.0%,重复性好RSD<3.0%。该方法能对猪肉和猪肝中氯霉素残留进行定性及定量分析,方法精密度较好、准确度较高、选择性好,结果满意。

Determination of chloramphenicol residues in pork and pig liver by LC-MS/MS

A method of determination of chloramphenicol in pork and pork liver by High Liquid chromatography-Tandem Mass Spectrometry(HPLC-MS/MS) was developed.Samples were extracted with acetonitrile and 4% sodium chloride solution,and precipitation protein at the same time,defatted by hexane,and Ethyl acetate liquidliquid extraction,then concentrated and constanted volume.Samples were detected by LC-MS/MS and isolated with Syncronis C 18 and the liquid phase was acetonitrile and water(40∶60),The electrospray ionization(ESI) mass spectrometry was run in negative ion multiple reaction monitoring mode,taking the chloramphenicol-D5as internal standard.At these experimental conditions,chloramphenicol had a good liner relatively(r=0.999 2) between 1～15ng/mL.recovery rate of samples ranged from 90.0%～110.0%,with LOD of 0.1 μ g/kg,and replicability was RSD<3.0%.This method could detect the chloramphenicol residue in pork and pork liver,and with a better precision,higher accuracy,better specificity,and the result was satisfied.