Preparation of an acryloyl β‐cyclodextrin‐silica hybrid monolithic column and its application in pipette tip solid‐phase extraction and HPLC analysis of methyl parathion and fenthion. Issue 18 (19th September 2018)

• Record Type: Journal Article
• Authors: Chen, Ling; Dang, Xueping; Ai, Youhong; Chen, Huaixia
• Is Part Of: Journal of separation science. Volume 41:Issue 18(2018)
• Page Start: 3508
• Page End: 3514
• Publication Date: 2018-09-19
• Subjects: cyclodextrin -- fenthion -- methyl parathion -- monolithic columns -- pipette tip solid‐phase extraction; Separation (Technology) -- Periodicals; Chromatographic analysis -- Periodicals; 543.089
• DOI: 10.1002/jssc.201701273
• Languages: English
• ISSNs: 1615-9306

Abstract

Abstract: An acryloyl β‐cyclodextrin‐silica hybrid monolithic column for pipette tip solid‐phase extraction and high‐performance liquid chromatography determination of methyl parathion and fenthion has been prepared through a sol–gel polymerization method. The synthesis conditions, including the volume of cross‐linker and the ratio of inorganic solution to organic solution, were optimized. The prepared monolithic column was characterized by thermogravimetric analysis, scanning electron microscopy, and Fourier transform infrared spectroscopy. The eluent type, volume and flow rate, sample volume, flow rate, acidity, and ionic strength were optimized in detail. Under the optimized conditions, a simple and sensitive pipette tip solid‐phase extraction with high‐performance liquid chromatography method was developed for the determination of methyl parathion and fenthion in lettuce. The method yielded a linear calibration curve in the concentration ranges of 15–400 μg/kg for methyl parathion and 20–400 μg/kg for fenthion with correlation coefficients of above 0.9957. The limits of detection were 4.5 μg/kg for methyl parathion and 6.0 μg/kg for fenthion, respectively. The recoveries of methyl parathion and fenthion spiked in lettuce ranged from 96.0 to 104.2% with relative standard deviations less than 8.4%.