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Determination of chlorinated hydrocarbons in milk samples using sol-gel based polymer coated silica sorbent for stir-bar supported micro-solid-phase extraction coupled with gas chromatography mass-spectrometry
Authors:Khalid Alhooshani
Affiliation:Department of Chemistry, King Fahd University of Petroleum and Minerals, Dhahran 31261, Saudi Arabia
Abstract:
In this work, sol-gel reaction chemistry was utilized to create 3-(trimethoxysilyl)propyl methacrylate-poly (propylene glycol) polymer coating on amorphous silica. The synthesized sorbent was characterized using energy dispersive X-ray spectrometry, field emission scanning electron microscopy, and thermogravimetric analysis. The sorbent was then used for membrane protected stir-bar supported micro-solid-phase extraction (SB-µ-SPE) of chlorinated hydrocarbons (CHCs) in milk samples and analyzed using gas chromatography mass spectrometry. Sorbent suitability, sorbent quantity, solvent for desorption, solvent volume, time for extraction, time for desorption, and ionic strength were all optimized for extraction. This method resulted in a wide linear range for all tested CHCs with an r2 up to 0.9992. The lower limits of detection ranged between 0.2 and 2.8 ng mL?1. Reproducibility of the method was also determined at three different concentrations ranging between 3.8 and 7.3%. The relative recoveries in milk samples were found to be between 85.1 and 104.3%.
Keywords:Chlorinated hydrocarbon  Sol-gel chemistry  Gas chromatography mass-spectrometry  Micro-solid phase extraction  Milk samples
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