Journal
TALANTA
Volume 189, Issue -, Pages 560-567Publisher
ELSEVIER SCIENCE BV
DOI: 10.1016/j.talanta.2018.07.044
Keywords
Organophosphorus pesticides; Mesoporous silica; Solid-phase extraction; Gas chromatography; Water samples; Preconcentration
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Funding
- MINECO of Spain
- FEDER [MAT2015-64139-C4-2-R]
- Generalitat Valenciana [PROMETEO/2016/145]
- MEC [FPU16/02358]
- Universitat de Valencia [INV_PREDOC17F1-540310]
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A novel sorbent based on a UVM-7 mesoporous silica doped with Ti has been synthesized and used for solid phase extraction of several organophosphorus pesticides in environmental water samples followed by gas chromatography coupled to a nitrogen-phosphorus selective detector. Thus, mesoporous silica materials doped with Ti and Fe as well as immobilized cyclodextrin silica-based supports were prepared and morphologically characterized by several techniques such as transmission electronic microscopy, nitrogen adsorption-desorption and X-ray diffraction. These sorbents were comparatively evaluated, and Ti25-UVM-7 material was selected as the best solid phase. After optimization of extraction parameters such as amount of solid-phase, type and volume of eluent, pH and ionic strength and breakthrough volume, recoveries between 81% and 104.5% were achieved, with RSD values below 7.8% and 12% for infra-day and inter-day repeatability respectively. Moreover, limits of quantification in the range 0.5-4.4 mu g L-1 were achieved for all target compounds using mass spectrometry detector. In addition, the developed method was applied for analysis of real water samples and it was validated with commercial C18 cartridges. Matrix effect was demonstrated in complex environmental matrices and the good reusability of synthesized material was also proved.
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