自制萃取头固相微萃取测定水中的有机磷杀虫剂  

Determination of organophosphorus pesticides in water samples by solid-phase microextraction using home-made fiber

作　　者：冯喜兰[1] 田孟魁[1] 荆瑞俊[1] 

机构地区：[1]河南科技学院,新乡453003

出　　处：《河南科技学院学报》2010年第2期107-112,共6页Journal of Henan Institute of Science and Technology(Natural Science Edition)

基　　金：河南省教育厅科技攻关项目(2010A150010)

摘　　要：以多壁碳纳米管(MWCNTs)为涂层制作了固相微萃取(SPME)萃取头,用自制的萃取头SPME技术与GC-TSD联用测定了水中的4种有机磷杀虫剂(甲拌磷、甲基对硫磷、毒死蜱和对硫磷).优化了影响萃取效率的各种因素.方法的线性范围为0.1～50μg·L^(-1),相关系数(r)为0.996 3～0.999 7,检出限(LODs,S/N=3)为1.9～24.3ng·L^(-1),相对标准偏差(RSD,n=6)小于8.8%.与商用的PDMS(7μm)萃取头比较,MWCNTs涂层的萃取头具有使用寿命长、灵敏度高等优点,自制的萃取头用于测定水样中的有机磷杀虫剂,在2和20μg·L^(-1)两个加标浓度的回收率分别为74.6%～96.8%和91.1%～102.6%.A novel fiber coated with multiwalled carbon nanotube （MWCNTs） was prepared for use with headspace solid-phase mieroextraetion （HS-SPME） combined with gas chromatography and thermionic specific detector （TSD）, which was applied in order to determine four organophosphorus pesticides （phorate, methyl parathion, chlopyrifos and parathion） in water sample. Various parameters affecting the extraction efficiency were optimized. The developed method has a linear range of 0.1-50 μg.L^-1 for all analytes, with coefficients of correlation （r） ranging from 0.996 3 to 0.999 7. The limits of detection （LODs） ranged from 1.9 to 24.3 ng. L^-1 （S/N = 3）, and relative standard deviation （RSD%） in the range of 5.9%-8.8%（n = 6）. Compared with the commercial PDMS （7 μm） fiber, the MWCNTS fiber has honger lifespan and higher sensitivity.The novel fiber was applied to determine organophosphorus pesticides in fiver water sample, the recoveries obtained at 2 μg.L^-1and 20 μg· L^-1 spiking level were in the range of 74.6%- 96.8% and 91.1%-102.6%, respectively.

关 键 词：多壁碳纳米管 有机磷杀虫剂:固相微萃取 

分 类 号：O657.7[理学—分析化学]