固相萃取净化高效液相色谱法测定玉米中吡虫啉  

Determination of imidacloprid residuals in corn with HPLC and SPE cleanup method

作　　者：王凤池[1] 高文惠[2] 吕红英[1] 罗敏[2] 孟慧[2] 

机构地区：[1]河北出入境检验检疫局,石家庄050071 [2]河北科技大学生物科学与工程学院,石家庄050018

出　　处：《食品科技》2006年第8期259-262,共4页Food Science and Technology

基　　金：河北省博士基金项目(06547003D-3);河北省科技攻关项目(04213036);河北省教育厅项目(Z2005202)

摘　　要：研究采用固相萃取-高效液相色谱法测定玉米中吡虫啉的残留。样品中吡虫啉经乙腈提取,采用刚活化后弗罗里硅土对其进一步净化提纯,洗脱液为丙酮;将洗脱液用氮吹浓缩、定容、过滤后,供液相色谱测定;采用安捷伦XDB-C18(250mm×4.6mm)色谱柱,柱温40℃,甲醇-乙腈-水(10∶10∶80)为流动相,检测波长270nm;该方法的检测限为0.2μg/mL,线性范围0.2～5μg/mL,线性相关系数为0.9993,回收率达84.2%。结果表明,该分析方法不仅操作简便,分析周期短,而且方法准确度高,色谱分离效果好。A combination method of SPE and HPLC were used to determine imidacloprid residuals in corn. Imidacloprid was extracted with acetonitrile from the sample and the extraction was further purified with fresh activated Florisil. Acetone was used as eluent. Eluent was concentrated with nitrogen and diluted to volume and filtrated. The chromatographic conditions were： Agilent XDB-C18（250mm×4.6mm） column at 40℃, MeOH/ CH3CN/H2O（10：10：80） as mobile phase, UV detector at 270nm. Detection limit of the method was 0.2μg/mL, linear range and linearly dependent coefficient were 0.2-5μg/mL and 0.9993 respectively, average recovery is 84.2%. The result showed that this method is easy to operate, with greatly shortened analytical time, greatly enhanced accuracy, and obviously improved separation results.

关 键 词：高效液相色谱 固相萃取 吡虫啉 玉米 

分 类 号：TS207.53[轻工技术与工程—食品科学]