Dispersive magnetic solid phase extraction combined with gas chromatography negative chemical ionization mass spectrometry for the determination of pyrethroids in aqueous samples

• Main Authors: Guang-Ping Niu, 牛光平
• Other Authors: Youn-Yuen Shu
• Format: Others
• Language: zh-TW
• Published: 2016
• Online Access: http://ndltd.ncl.edu.tw/handle/46577939245070508755

碩士 === 國立高雄師範大學 === 化學系 === 104 === A novel dispersive magnetic solid phase extraction coupled with gas chromatography-negative ion chemical ionization mass spectrometric method (GC-MS-NCI) was developed for the determination of six pyrethroids ( including fenpropathrin, λ-cyhalothrin, cypermethrin, flucythrinate, fenvareate and deltamethrin ) in environmental aqueous samples. A prepared core/shell Fe3O4@nSiO2@mSiO2 magnetic particle was used for the extraction. The optimum extraction conditions was obtained by using Taguchi’s Orthogonal Arrays: 50 mL aqueous sample was adjusted to pH 2 with the 0.15 g magnetic sorbent for 20 minutes extraction. The analytes extracted on magnetic sorbent was then desorbed with 1.5 mL acetone for 20 minutes. Desorption solvent was withdrawn and with subsequent evaporation to dryness and reconstituted to 50 mL prior to GC-MS analysis. Under the optimum conditions, good linearity were obtained in a range of 0.05-35.0 ng/mL for the six analytes with correlation coefficients g2> 0.992 and concentration factors between 237 and 468. The method detection limits were between 6.7-72 pg/mL. The recoveries of six pyrethroids at spiked levels were in the range of 78%-95%. The developed DMSPE-GCMS method is a simple and viable for the determination of pyrethroids in environmental samples with high enrichment factor.