A micro-solid phase extraction technique was developed using a novel polypyrrole-polyamide nanofiber sheet, fabricated by electrospinning method. The applicability of the new nanofiber sheet was examined as an extracting medium to isolate malathion as a model pesticide from aqueous samples. Solvent desorption was subsequently performed in a microvial, and an aliquot of extractant was injected into gas chromatography-mass spectrometry. Various parameters affecting the electrospinning process including monomer concentration, polyamide content, applied voltage, and electrospinning time were examined. After fabricating the most suitable preparation conditions, influential parameters on the extraction and desorption processes were optimized. The developed method proved to be rather convenient and offers sufficient sensitivity and good reproducibility. The limit of detection (S/N = 3) and limit of quantification (S/N = 10) of the method under optimized conditions were 50 and 100 ng L(-1), respectively. The relative standard deviation at concentration level of 1 ng mL(-1) was 2% (n = 3). The calibration curve of analyte showed linearity in the range of 0.1-1 ng mL(-1) (R (2) = 0.9975). The developed method was successfully applied to tap and Zayanderood river water samples, while the relative recovery percentages of 98% and 96% were obtained, respectively. The whole procedure showed to be conveniently applicable and quite easy to be manipulated.
A novel method based on microextraction in packed syringe (MEPS) as sample preparation technique coupled off-line with gas chromatography-mass spectrometry was developed using electrospun nanofibers as sorbent. For electrospinning of polypyrrole/polyamide-based nanofiber, a homogeneous solution containing nylon 6, ferric chloride and pyrrole monomer was prepared and then was drawn into a 2.5-mL syringe. By applying a voltage of 13 kV between the needle of the syringe and an aluminum-foil collector, the nanofibers could be formed on the surface of the collector. The prepared sheet was used as the sorbent for MEPS to analyze some selected organophosphorous pesticides. Important parameters influencing the extraction and desorption processes were optimized. Limits of detection were in the range of 0.04-0.1 ng/mL using time scheduled selected ion monitoring mode, and the relative standard deviation (RSD %) values with four replicates were in the range of 3.7-11.8% at a concentration level of 5 ng/mL. The linearity of the method was in the range of 0.5-500 ng/mL for diazinon and fenithrothion and 0.5-200 ng/mL for the rest of the analytes. The developed method was successfully applied to Zayandeh-roud river water samples, whereas the matrix factors were in the range of 0.87-0.98.
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