Sol-Gel Hybrid Cyanopropyltriethoxysilane-methyltrimethoxysilane as Adsorbent for Dispersive-Micro Solid Phase Extraction of Selected Organophosphorus Pesticides in Water Samples

2014 ◽  
Vol 71 (5) ◽  
Author(s):  
Norfazilah Muhamad ◽  
Wan Aini Wan Ibrahim ◽  
Mohd Marsin Sanagi
Keyword(s):  
Solid Phase Extraction ◽  
Water Samples ◽  
Solid Phase ◽  
Organophosphorus Pesticides ◽  
Sol Gel ◽  
Polar Compounds ◽  
Gas Chromatography Mass Spectrometry ◽  
Phase Extraction ◽  
Pesticides In Water ◽  
Spe Method

Commercial solid phase extraction (SPE) sorbents normally used for organophosphorus pesticides (OPPS) analysis is C18.  However, it show low retention for polar compounds and is rather expensive. The limitations are overcome through the development of a new sol-gel hybrid material, cyanopropyltriethoxysilane-methyltrimethoxysilane (CNPrTEOS-MTMOS). Sol-gel hybrid CNPrTEOS-MTMOS was successfully synthesized and applied as an adsorbent for dispersive-micro-SPE (D-µ-SPE) of three selected OPPs from several water samples. Extracted analytes were analyzed using gas chromatography-mass spectrometry.  Under the optimum conditions (100 mg CNPrTEOS-MTMOS as adsorbent, 10 mL water samples, 7 min extraction time, 300 µL methanol as desorption solvent and 3 min desorption time), the method showed excellent detection limits (0.01-0.004 µg L-1  at S/N = 3) and linear range achieved were 0.01-10 µg L-1. The CNPrTEOS-MTMOS sorbent offers an alternative sorbent material for the extraction of OPPs of various polarity. The developed D-µ-SPE method was successfully applied for the simultaneous analysis of OPPs in several water samples and results were compared with published results.  Sol-gel hybrid CNPrTEOS-MTMOS showed high potential as an alternative adsorbent for D-µ-SPE technique for OPPs.

Selective and Simultaneous Solid Phase Extraction of Polar and Non–Polar Organophosphorus Pesticides Using Sol–Gel Hybrid Silica–Based Sorbent

2013 ◽  
Vol 62 (3) ◽  
Author(s):  
Wan Aini Wan Ibrahim ◽  
Wan Norfazilah Wan Ismail ◽  
Mohd Marsin Sanagi
Keyword(s):  
Solid Phase Extraction ◽  
Water Samples ◽  
Extraction Efficiency ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Organophosphorus Pesticides ◽  
Sol Gel ◽  
Phase Extraction ◽  
Hybrid Silica ◽  
Hybrid Sorbent

A new sol–gel hybrid silica–based sorbent, methyltrimethoxysilane–cyanopropyltriethoxysilane (MTMOS–CNPrTEOS) produced in our laboratory was used for highly selective and simultaneous solid phase extraction (SPE) of two polar organophosphorus pesticides (OPPs) and four non–polar OPPs from water samples. The two polar OPPs used as test analytes are dicrotophos and methamidophos while the four non–polar OPPs are diazinon, malathion, methidathion, and chlorpyrifos. Analysis of OPPs was performed using gas chromatography–mass spectrometry in scan mode. Extraction efficiency (based on peak area response) of the new sol–gel hybrid MTMOS–CNPrTEOS was superior to commercial C18 SPE sorbent. The new sorbent showed higher selectivity towards the polar dicrotophos and methamidophos and it was also able to simultaneously extract the four non–polar OPPs with higher extraction efficiency. The limit of detection at S/N=3 for the new sol–gel hybrid sorbent is 5–9× lower and similar accuracy for the six OPPs compared to commercial C18 SPE sorbent. The new sol–gel hybrid material showed high potential as an alternative sorbent material for solid phase extraction of OPPs of wide polarity. It was successfully applied to the selective and simultaneous extraction the six OPPs from tap water and lake water samples.

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