摘要
采用两相中空纤维液相微萃取(LPME)技术结合高效液相色谱(HPLC)法,对水环境中残留的毒死蜱农药进行了富集和测定。通过研究萃取剂、萃取剂相pH、搅拌速率和萃取时间等对萃取效率的影响,确定了最优化的LPME条件为:以磷酸三丁酯为萃取剂,萃取剂相pH值为7,搅拌速率为1 000 r/min,萃取时间为20 min。然后采用高效液相色谱法对毒死蜱进行了定性和定量测定,结果表明,本法线性范围宽,相关系数r2=0.997,检出限为0.03μg/mL,相对标准偏差为4.2%,且毒死蜱的富集倍数可达97倍,大大提高了检测的灵敏度。用于实际样品分析时,结果稳定、可靠,平均回收率达87.3%~94.0%。
Using the method of two-phase hollow fiber liquid phase microextraction( LPME) combined with high performance liquid chromatography( HPLC) to enrich and detect residual pesticide of chlorpyrifos in water environment. By studying the influences of extraction agent,the pH of provider phase,stirring rate and extraction time on extraction efficiency,the optimum conditions were determined: using TBP as extractant,the pH of provider phase was 7,the stirring rate was 1000 r / min and the extraction time was 20 min. Then HPLC was used for quality and quantitative analysis of chlorpyrifos. The results showed that this method provided a wide linear range with a correlation coefficient( r2) of 0. 997,the limit of detection was 0. 03 μg/mL and the relative standard deviation was 4. 2%. The enrichment ratio of chlorpyrifos reached 97 times,which greatly improving the detection sensitivity. The result was stable and reliable when the method was applied to the determination of actual samples, and the average recoveries rate were within the range of 87. 3% ~ 94. 0%.
出处
《东华理工大学学报（自然科学版）》
CAS
2013年第S1期96-100,共5页
Journal of East China University of Technology(Natural Science)
基金
江西省科技计划项目(20121BBG70011)
关键词
中空纤维
两相液相微萃取
毒死蜱
hollow fiber
two phase liquid-phase microextraction
chlorpyrifos
