Functionalized Organosilicate Materials As A Novel Fiber Coating In Headspace Solid Phase Microextraction Of Phthalate Esters

Sample preparation is common in many analyses and is developed to improve a specific analysis. This step may be the most time-consuming in analysis and affects significantly the analytical information [۱]. Solid phase microextraction (SPME) was developed by Pawliszyn and his coworkers in the last decade. It has become an attractive sampling technique and gained widespread acceptance in many areas [۲]. a new porous material was used as a coating in solid phase microextraction for extraction and determination of phthalate esters in complex matrices such as environmental and biological samples. The prepared nanomaterial was immobilized on a stainless steel wire for fabrication of the SPME fiber. The fiber was evaluated for the extraction of some phthalate esters from aqueous sample solutions and saliva in combination with the GC-FID instrument. The extraction efficiency of SPME increases by using mesoporous silicas adsorbents due to its high surface area [۳]. The resultant material was characterized by scanning electron microscopy, transmission electron microscopy, infrared spectroscopy, X-ray diffraction, and BET/BJH surface area/porosity, N۲ adsorption-desorption measurements. Key parameters affecting the extraction efficiencies, including extraction temperature, extraction time, ionic strength, and desorption temperature and time. Under optimum conditions, the repeatability for one fiber (n = ۷), expressed as relative standard deviation (R.S.D.%), was between ۴.۸% and ۸.۷% for the extracted compounds. The limits of detection for the studied compounds were between ۰.۲۵ and ۱ μgL-۱. The relative recovery was between ۸۲ and ۱۱۰%. The calibration curve was linear in the concentration range from ۰.۰۵ to ۳۰۰ μgL-۱. The results showed suitable correlation coefficients (R > ۰.۹۹) for all of the analytes in the studied calibration range. The developed method offers the advantage of being simple to use, with shorter analysis time, lower cost of equipment, the thermal stability of fiber, and high relative recovery in comparison to conventional methods of analysis.