Silica aerogel modified electrospun polyacrylonitrile as a sorbent for thin-film microextraction of chlorpyrifos from real samples coupled with corona discharge ion mobility spectrometry detection.

In this paper, modified polyacrylonitrile/silica aerogel fibers were prepared and used as an adsorbent for thin-film microextraction of chlorpyrifos. The extracted analyte was analyzed by corona discharge ion mobility spectrometry. The electrospinning method was applied for the preparation of polyacrylonitrile fibers. The alkaline hydrolyzation technique was used to modify the electrospun film surface. Silica aerogel was synthesized on the surface of modified electrospun polyacrylonitrile fibers by the in situ growth technique. To access a high extraction yield, effective synthesis and extraction parameters such as NaOH concentration, reaction temperature and time, thin-film pretreatment, gelation time, solution pH, ionic strength, and extraction time were studied. The linearity range and the limit of detection of the method were 1-100 µg L-1 and 0.3 µg L-1, respectively. The precision of the method was 4 and 12% for the concentration levels of 5 and 60 µg L-1, respectively. Chlorpyrifos was successfully determined by the method in well water, river water, agricultural wastewater, and tangerine samples.

In situ growth of copper-based metal-organic framework on a helical shape copper wire as a sorbent in stir-bar sorptive extraction of fenthion followed by corona discharge ion mobility spectrometry.

In this paper, a helical copper wire, coated with copper-benzene-1,4-dicarboxylic acid metal-organic framework (Cu-BDC) was used as a sorbent for stir-bar sorptive extraction of fenthion from water and fruit samples. The homogenous coating was fabricated through two simple and fast steps. The chemical conversion of copper substrate to copper hydroxide nanotubes (Cu(OH)2 NTs) was performed in an alkaline solution and then Cu-BDC was formed through a neutralization reaction. Corona discharge ion mobility spectrometry in positive mode was applied for the detection of fenthion. To improve the sensitivity of the method, some synthesis and extraction parameters affecting the extraction efficiency such as benzene-1,4-dicarboxylic acid concentration, ionic strength, sample pH, stirring rate, extraction temperature, and extraction time were investigated. The linear dynamic range between 0.5 and 80 µg L-1 and detection limit of 0.1 µg L-1 were obtained under optimal conditions. The intra- and inter-day relative standard deviations were less than 6.4 and 8.6%, respectively. The applicability of the method was examined for the analysis of different samples (i.e., well water, agricultural wastewater, and orange). The recovery for the determination of fenthion in spiked samples varied from 88 to 111%.

Centrifuge-free dispersive liquid-liquid microextraction coupled with thin-film microextraction for the preconcentration of molinate in real samples by ion mobility spectrometry.

A tandem microextraction method, centrifuge free dispersive liquid-liquid microextraction and thin-film microextraction (DLLME-TFME), was used for analyzing molinate in environmental samples by ion mobility spectrometry (IMS). Considering the IMS as a competitive detection system, coupling these two popular sample preparation methods reduces the effect of solvent interference and improves the sensitivity of the technique. Trichloromethane and methanol were used as the extraction, and dispersive solvents for the DLLME method and electrospun polyacrylonitrile/copper-benzene-1,4-dicarboxylic acid fibers were used as a sorbent in the TFME method. Some effective experimental variables influencing the extraction efficiency of an analyte such as type and volume of dispersive and extraction solvents, solution pH, ionic strength, sonication time, and extraction time were studied. The linear dynamic range of 0.5-50 µg L-1 and the limit of detection of 0.1 µg L-1 were obtained under optimized conditions. The relative standard deviations for intra-and inter-day analysis were calculated less than 10%. The present method was used for the determination of molinate in different real samples such as agricultural wastewater, well water, river water, and apple, and the recovery was obtained between 82% and 113%, for the spiked samples.

Mg-Al-CO3 layered double hydroxide reinforced polymer inclusion membrane as an extractant phase for thin-film microextraction of cyanide from environmental water samples.

In this paper, a flexible and efficient nano-reinforced polymer inclusion membrane (PIM) was fabricated and used for cyanide (CN-) extraction from water samples. Aliquat 336 (a liquid anion exchanger) was embedded in poly(vinyl chloride) (PVC) support as the extractant. Mg-Al-CO3 layered double hydroxide (LDH) with high surface area and anion exchange ability was applied to promote the extraction efficiency of PIM. A PIM comprising 56% PVC, 40% Aliquat 336, and 4% Mg-Al-CO3 LDH showed the best extraction efficiency. A single beam ultraviolet-visible spectrophotometer was used for the detection of cyanide. Surface morphology of the PIM was studied by field emission scanning electron microscopy. The experimental parameters influencing the extraction process were investigated and optimized. The intra- and inter-day relative standard deviations at two different concentrations were in the range of 2.8-7.6%. The dynamic range of the method was in the range of 5-500 µg L-1, and the detection limit was 1.4 µg L-1. The LDH reinforced PIM showed proper characteristics for the extraction of cyanide from real water and wastewater samples with recoveries between 82 and 115%.