在线固相萃取结合高效液相色谱-电喷雾式检测器测定鸡粪中红霉素残留  

Determination of Erythrocin in Chicken Manure by High Performance Liquid Chromatography-Corona-Charged Aerosol Detection Coupled with On-line Solid Phase Extraction

作　　者：周茜[1] 陈满堂[1] 朱丽华[1] 丁耀彬[2] 

机构地区：[1]华中科技大学化学与化工学院,武汉430074 [2]中南民族大学化学与材料科学学院,武汉430074

出　　处：《分析化学》2014年第12期1838-1841,共4页Chinese Journal of Analytical Chemistry

基　　金：国家高技术研究发展计划(863计划)(No.2012AA06A304)资助项目~~

摘　　要：将在线固相萃取（ online SPE）与高效液相色谱（ HPLC）-通用型电喷雾检测器（ CAD）结合,建立了集约养殖业常用抗生素红霉素的分析方法。5.0 g鸡粪样品与硅藻土混合后,置于34 mL萃取池中,以热水为萃取剂,在70℃、10.4 MPa条件下,用快速溶剂萃取仪提取样品中的红霉素。利用双三元液相色谱仪,采用在线富集进样方式,经Acclaim 120 C18色谱柱,以乙腈-0.1％甲酸溶液为流动相分离后,用CAD进行检测。红霉素在21～2000μg/kg范围内线性关系良好（r≥0.99）,检出限为6.3μg/kg,加标回收率为79.2％～87.5％。A novel HPLC-CAD method coupled with on-line solid phase extraction （SPE） for the determination of erythrocin which was widely used in livestock farming was developed. After mixed with diatomite, 5.0 g manure sample was put into the cell and extracted with hot water at 70 ℃ and 10.3 MPa. An on-line SPE methodology was applied to pre-treat the sample, and the sample was seperated on an Acclaim 120 ClS column and analyzed by corona CAD detector using acetonitrile and 0. 1% formic acid as mobile phase. Good linearity for erythrocin was obtained in the range of 21-2000 μg/kg. The detection limit was 6.3 μg/kg. The average recoveries were 79.2% -87.5%.

关 键 词：高效液相色谱 电喷雾式检测器 在线固相萃取 红霉素 快速溶剂萃取 

分 类 号：S859.84[农业科学—临床兽医学] O657.72[农业科学—兽医学]