摘要
基于微波辅助-顶空液相微萃取联用(MAE-HS-LPME)这一样品前处理方法,采用高效液相色谱法(HPLC)对水样中的敌敌畏残留量进行了测定。对影响萃取的因素如萃取剂、微波辐射功率、萃取时间、离子强度和样品基质的pH值等进行了考察。萃取条件为:选用二甲苯作萃取剂,萃取时间为15min,微波辐射功率300W,NaCl含量为5%,pH为2.5。在最佳条件下,敌敌畏的检出限(信噪比为3时)为0.96μg/L,定量限(信噪比为10时)为3.20μg/L,萃取富集倍数为54,实际水样的加标回收率为87.4%~103%。与传统的前处理方法相比,本方法具有简便、快速、高效、节省溶剂、选择性好、应用范围广的特点。
A novel method for the determination of dichlorvos in environmental water samples has been developed using microwave-assisted-headspace-liquid-phase microextraction(MAE-HS-LPME) coupled with high performance liquid chromatography(HPLC).The influences of extraction parameters in the sample matrix were investigated.Under optimized experimental conditions,the detection limit(S/N=3),the quantification limit(S/N=10) and the enrichment factor of the proposed method for the target analyte were 0.96 μg/L,3.20 μg/L and 54,respectively.The recoveries of target analyte spiked in real water samples were 87.4%-103%.The extraction performance of MAE-HS-LPME to the target analyte was also compared with liquid-liquid extraction(LLE).The results indicated that the developed method is simple,rapid,efficient,solvent-saving,highly selective and widely applicable.
出处
《色谱》
CAS
CSCD
北大核心
2010年第12期1200-1203,共4页
Chinese Journal of Chromatography
基金
中央高校基本科研业务费项目(No.CDJXS10220004)
重庆市科学委员会自然科学基金项目(No.CSTC2008BB9266)
重庆市教育委员会科学技术研究项目(No.KJ100102)
关键词
微波辅助萃取
顶空液相微萃取
高效液相色谱
敌敌畏
环境水样
microwave-assisted extraction(MAE)
headspace-liquid-phase microextraction(HS-LPME)
high performance liquid chromatography(HPLC)
dichlorvos
environmental waters