固相微萃取-高效液相色谱法测定己烯雌酚【毕业设计】.doc

- PAGE I - （20 届） 本科毕业设计 固相微萃取-高效液相色谱法测定己烯雌酚 Determination of DES by Solid-Phase Microextraction Coupled and High Performance Liquid Chromatography 所在学院 专业班级 化学 学生姓名 学号 指导教师 职称 完成日期 年 月 PAGE XVIII PAGE 4 摘 要 【摘要】建立应用固相微萃取（SPME）-高效液相色谱（HPLC）法测定食品中的己烯雌酚（DES）的分析方法。探讨了萃取纤维、萃取时间、解吸时间和离子强度对DES萃取效率的影响，并采用正交试验，以解析液组成、萃取液pH和搅拌速度为3因素筛选出了最佳固相微萃取条件。结果表明，在室温下，采用85μm聚酰胺(PA)萃取纤维头，萃取原液中不添加盐（NaCl）且不做任何pH处理，搅拌速度为600r/min，萃取时间为30min，解吸时间为10min时，对DES萃取效果最佳。本方法对DES测定的线性范围为0.02～2.00μg/mL，工作曲线线性良好，线性相关系数为0.9961，方法检出限（S/N=3）为0.006μg/mL，测定结果的变异系数小于5%。将该法用于鸡肉和牛奶中DES的测定，不同加标水平的回收率为84.6～91.3%和81.9～93.1%。 【关键词】固相微萃取；高效液相色谱；己烯雌酚；食品 Determination of DES by Solid-Phase Microextraction Coupled and High Performance Liquid Chromatography Abstract 【ABSTRACT】A novel method for the determination of DES by SPME-HLPC was developed in food. Discussed the influence of extraction fiber,extraction time,desorption time and ionic strength to DES extracted efficiency, and using the orthogonal test, taking analyzed liquid 、extracted liquid pH and the mixing speed as 3 factors filtered the best SPME .The result indicated that under the room temperature,adopting 85μm gathers the amide (PA) extraction fiber head，no an addition of the salt (NaCl) and no pH processing in the extraction original fluid,the solution being srirred at 600r/min,extraction time at 30 minutes，desorption time at 10 minutes，witch was the best for the extraction effect of DES .The method is linear for DES over the range assayed from 0.02 to 2.00μg/mL with the detection limits（S/N=3）of 0.006μg/mL and the correlation coefficients of 0.9961.This determ- ination result of the coefficient variation was smaller than 5%. The method was applied to the determination of DES in chicken as food and milk power，and the different recovery rates of detected samples Respectively were 84.6~91.3% and 81.9~93.1%. 【KEYWORDS】solid-phase