New magnetic graphene-based inorganic-organic sol-gel hybrid nanocomposite for simultaneous analysis of polar and non-polar organophosphorus pesticides from water samples using solid-phase extraction.
A new graphene-based tetraethoxysilane-methyltrimethoxysilane sol-gel hybrid magnetic nanocomposite (Fe3O4@G-TEOS-MTMOS) was synthesised, characterized and successfully applied in magnetic solid-phase extraction (MSPE) for simultaneous analysis of polar and non-polar organophosphorus pesticides from several water samples. The Fe3O4@G-TEOS-MTMOS nanocomposite was characterized using Fourier transform-infrared spectroscopy, energy-dispersive X-ray spectroscopy, field emission scanning electron microscopy and X-ray diffraction. Separation, determination and quantification were achieved using gas chromatography coupled with micro electron capture detector. Adsorption capacity of the sorbent was calculated using Langmuir equation. MSPE was linear in the range 100-1000 pg mL-1for phosphamidon and dimethoate, and 10-100 pg mL-1for chlorpyrifos and diazinon, with limit of detection (S/N = 3) of 19.8, 23.7, 1.4 and 2.9 pg mL-1for phosphamidon, dimethoate, diazinon and chlorpyrifos, respectively. The LODs obtained is well below the maximum residual level (100 pg mL-1) as set by European Union for pesticides in drinking water. Acceptable precision (%RSD) was achieved for intra-day (1.3-8.7%, n = 3) and inter-day (7.6-17.8%, n = 15) analyses. Fe3O4@G-TEOS-MTMOS showed high adsorption capacity (54.4-76.3 mg g-1) for the selected OPPs. No pesticide residues were detected in the water samples analysed. Excellent extraction recoveries (83-105%) were obtained for the spiked OPPs from tap, river, lake and sea water samples. The newly synthesised Fe3O4@G-TEOS-MTMOS showed high potential as adsorbent for OPPs analysis.
Separation Science and Technology Group, Department of Chemistry, Faculty of Science, Universiti Teknologi Malaysia, 81310 UTM, Johor Bahru, Johor, Malaysia.
Hamid
H
Rashidi Nodeh
Separation Science and Technology Group, Department of Chemistry, Faculty of Science, Universiti Teknologi Malaysia, 81310 UTM, Johor Bahru, Johor, Malaysia; Centre for Sustainable Nanomaterials, Ibnu Sina Institute for Scientific and Industrial Research, Universiti Teknologi Malaysia, 81310 UTM, Johor Bahru, Johor, Malaysia. Electronic address: wanaini@kimia.fs.utm.my.
Wan Aini
WA
Wan Ibrahim
Separation Science and Technology Group, Department of Chemistry, Faculty of Science, Universiti Teknologi Malaysia, 81310 UTM, Johor Bahru, Johor, Malaysia.
Muhammad Afzal
MA
Kamboh
Separation Science and Technology Group, Department of Chemistry, Faculty of Science, Universiti Teknologi Malaysia, 81310 UTM, Johor Bahru, Johor, Malaysia; Centre for Sustainable Nanomaterials, Ibnu Sina Institute for Scientific and Industrial Research, Universiti Teknologi Malaysia, 81310 UTM, Johor Bahru, Johor, Malaysia.
Mohd Marsin
MM
Sanagi
D000327:Adsorption; D002138:Calibration; D004390:Chlorpyrifos / Q000032:analysis; D002849:Chromatography, Gas; D003976:Diazinon / Q000032:analysis; D004117:Dimethoate / Q000032:analysis; D005290:Ferric Compounds / Q000737:chemistry; D006108:Graphite / Q000737:chemistry*; D060106:Lakes / Q000032:analysis; D057230:Limit of Detection; D008280:Magnetics; D053761:Nanocomposites / Q000737:chemistry*; D009930:Organic Chemicals / Q000737:chemistry; D010087:Oxides / Q000737:chemistry; D010573:Pesticide Residues / Q000032:analysis*; D010575:Pesticides / Q000032:analysis*; D044367:Phase Transition; D010707:Phosphamidon / Q000032:analysis; D010758:Phosphorus / Q000737:chemistry; D045483:Rivers; D012821:Silanes; D052616:Solid Phase Extraction / Q000379:methods*; D012997:Solvents / Q000737:chemistry; D017550:Spectroscopy, Fourier Transform Infrared; D014961:X-Ray Diffraction
D005290:Ferric Compounds; D009930:Organic Chemicals; D010087:Oxides; D010573:Pesticide Residues; D010575:Pesticides; D012821:Silanes; D012997:Solvents; C071718:methyltrimethoxysilane; D010707:Phosphamidon; C000499:ferric oxide; D010758:Phosphorus; C040733:tetraethoxysilane; D006108:Graphite; D004390:Chlorpyrifos; D004117:Dimethoate; D003976:Diazinon
Graphene; Magnetic solid phase extraction; Organophosphorus pesticides; Sol-gel hybrid; Water samples