Saraji Mohammad, Esteki Nafise
Department of Chemistry, Isfahan University of Technology, Isfahan, 84154-83111, Iran.
Anal Bioanal Chem. 2008 Jun;391(3):1091-100. doi: 10.1007/s00216-008-2087-8. Epub 2008 Apr 16.
Single-drop microextraction (SDME) followed by gas chromatography-mass spectrometry detection was used for the determination of some carbamate pesticides in water samples. The studied pesticides were thiofanox, carbofuran, pirimicarb, methiocarb, carbaryl, propoxur, desmedipham and phenmedipham. Two alternative sample introduction methods have been examined and compared; SDME followed by cool on-column injection (without derivatization) and SDME followed by in-microvial derivatization and splitless injection. Acetic anhydride was used as derivatization reagent. Parameters that affect the derivatization reaction yield and the extraction efficiency of the SDME method were studied and optimized. The analytical performances and possible applications of both approaches were investigated. Relative standard deviations for the studied compounds ranged from 3.2 to 8.3%. The detection limits obtained by the derivatization method were found to be in the range 3-35 ng/L. Using cool on-column injection (without derivatization), the detection limits were between 30 and 80 ng/L.
采用单滴微萃取(SDME)结合气相色谱-质谱检测法测定水样中的某些氨基甲酸酯类农药。所研究的农药有涕灭威、克百威、抗蚜威、甲硫威、西维因、残杀威、甜菜宁和苯胺灵。考察并比较了两种进样方法;SDME结合冷柱头进样(不衍生化)以及SDME结合微瓶内衍生化和不分流进样。使用乙酸酐作为衍生化试剂。研究并优化了影响衍生化反应产率和SDME方法萃取效率的参数。考察了两种方法的分析性能和可能的应用。所研究化合物的相对标准偏差范围为3.2%至8.3%。衍生化方法获得的检测限在3至35 ng/L范围内。采用冷柱头进样(不衍生化)时,检测限在30至80 ng/L之间。