Sustainable and green microextraction of organophosphorus flame retardants by a novel phosphonium‐based deep eutectic solvent (original) (raw)

Development of a dispersive liquid–liquid microextraction method for organophosphorus flame retardants and plastizicers determination in water samples

Journal of Chromatography A, 2007

Aerobic biodegradation behavior of nonylphenol propoxylates was investigated using dispersive liquidliquid microextraction as a simple and fast technique for sample preparation. The developed method proved to be efficient for the isolation and concentration of nonylphenol propoxylates before their quantification with the use of high performance liquid chromatography. The primary biodegradation of nonylphenol propoxylates was approximately 80 % by 10 days after the beginning of the test. However, the biodegradation products which were identified with the use of mass spectrometric detection persisted for many days.

On-line determination of organophosphorus pesticides in water by solid-phase microextraction and gas chromatography with thermionic-selective detection

Journal of High Resolution Chromatography, 1997

This paper describes the extraction of 49 organophosphorus pesticides (OPPs) from water samples using solid-phase microextraction (SPME). Three fibers, including a 15-km XAD-coated fiber, a 85ym polyacrylate-coated fiber, and a 30-km polydimethylsiloxane-coated fiber (PDMS), were evaluated here. The effects of stirring and the addition of NaCl to the sample were examined for the polyacrylate-coated fiber. The precision of the technique was examined for all three fibers and the extraction kinetics were investigated using the XAD-and polyacrylate-coated fibers. With some exceptions, the XAD-and polyacrylate-coated fibers performed better than the PDMS-coated fiber. The superiority of the XAD-and polyacrylate-coated fibers over the PDMS-coated fiber can be attributed to the aromatic functionalities of the XAD and the polar functionalities in the polyacrylate. The relatively high percent RSDs indicate that the SPME technique needs to be further refined before it can be used for anything other than screening. A more effective form of agitation than mechanical stirring may be necessary to reduce variability and achieve a faster equilibrium between the sample and the SPME fiber. I) New address: Roche BioScience, Palo Alto, California J. High Resol. Chromatogr.

Development of a solid-phase microextraction method for the analysis of phenolic flame retardants in water samples

Journal of chromatography. A, 2006

A solid-phase microextraction (SPME) method has been developed for the determination of pentachlorophenol (PCP) in paper and board samples. The analytical procedure involves direct extraction of PCP from paper and board samples and determination by gas chromatography with electron capture detection (GC-ECD). Two kinds of commercially available fibres; 100 m polydimethylsiloxane (PDMS), apolar, and 85 m polyacrylate (PA), quite polar, were evaluated to determine the extraction efficiency of pentachlorophenol. Parameters affecting the extraction process, such as temperature and time, were studied. Moreover, time of desorption and the effect of addition of salt were also investigated. The optimized procedure was applied to the analysis of pentachlorophenol (PCP) in five samples of virgin and recycled paper and board. The PCP content was determined by GC-ECD. To evaluate the effectiveness of the proposed method, it was compared with conventional extraction method with liquid-liquid extraction and derivatization. Detection limit of 0.015 g/g for PCP in paper was achieved with a RSD of 14%.

Comparison of the extractability of organophosphorus flame retardants in landfill media using organic and green solvents

Scientific Reports, 2022

Organic solvents are mainly used in the extraction of organophosphorus flame retardants (OPFRs) because of their availability and having been tested as good extracting solvents for most environmental pollutants. However, organic solvents are toxic, flammable, and costly. Hence, there is an ongoing quest for less hazardous chemicals such as green deep eutectic solvents (DES) that are cheap, recyclable, non-toxic and degradable in the environment, which can be used to extract organic pollutants such as OPFRs in environmental samples. This study assessed the extractability of OPFRs in municipal landfill leachate and sediment, using organic solvents and DES. Of the fourteen targeted OPFRs, 11 (80%) and 7 (50%) were detected in the leachate and sediment samples, using hexane; whereas 14 (100%) and 13 (90%) OPFRs were detected in the same order of samples using DES. The concentrations of OPFRs obtained for the leachate using optimum organic and DES ranged from below the limit of quantification (< LOQ)-516 ± 8.10 ng/L and < LOQ-453 ± 8.10 ng/L respectively. Correspondingly, the concentrations of OPFRs in sediment samples ranged from < LOQ-135 ± 2.89 ng/g dw and < LOQ-395 ± 2.24 ng/g dw, respectively. The results from this study, therefore, highlight the potential of DES to extract more OPFR from complex matrices such as landfill leachate and sediment. This finding infers that green hydrophilic DES can serve as good replacement for organic solvents such as hexane in liquid-liquid extraction (LLE) and solid-liquid extraction (SLE) techniques for landfill leachate and sediment. Flame retardants are organic chemicals that are added to materials, to reduce the rate at which materials catch fire, thereby giving people more time to escape 1. With the gradual discontinuation of the use of flame retardants such as polybrominated diphenyl ethers (PBDEs), the demand for replacements increased and organophosphorus flame retardants were introduced as suitable replacements. However, research on these chemicals has re-emerged as they have been identified as not being quite suitable substitutes for the phased-out commercial penta-and octa-BDE formulations because of their toxicity 2. Due to the application of organophosphorus flame retardants (OPFRs) in several household and industrial products, these products are the primary sources of OPFRs 3,4. Hence, they can reach the environment via industrial emissions during manufacturing, and by leaching out of OPFRs-treated materials into the environment when disposed into municipal landfill sites 5. In South Africa, consumer products inclusive of OPFRs-treated products are usually disposed of into landfill sites as general waste at the end of their life cycle. It is, therefore, important to monitor the presence of OPFRs in the landfill environment since groundwater contamination is most likely to occur also if no geomembrane liner is provided in the landfill 6. OPFRs have a wide range of polarities, and the reported studies in landfill leachate and water samples have used organic solvents that are polar 7-10 ; a mixture of equal ratios of polar and non-polar organic solvents 11-14 ; and unequal variations of polarities 13,15,16. Only a few studies have reported the extraction of OPFRs from landfill sediment or soil samples, however, the use of polar 8,17,18 ; and unequal variations of organic solvents were reported 14,15,19. The use of organic solvents for extraction is owed to their availability and having been tested as good extracting solvents for most organic environmental pollutants 20. However, it is a well-known fact that these solvents are toxic, flammable, and costly 21. Hence, there is an ongoing quest for less hazardous chemicals with a high extracting potential that can be used to extract organic pollutants such as OPFRs in environmental samples. Several studies have reported the use of deep eutectic solvents to extract flame retardants or pesticides in environmental matrices. For example, Solaesa et al. 22 reported the extraction of PBDEs in fish oils using choline

Determination of Organophosphorus Pesticides in Juice and Water by Modified Continuous Sample Drop Flow Microextraction Combined with Gas Chromatography–Mass Spectrometry

2020

In this paper, the technique of continuous sample drop flow microextraction (CSDF-ME) is developed by the addition of a narrow-necked conical vessel. In the developed technique, an organic solvent denser than water is used for the extraction of organophosphorus pesticides (OPPs) from fruit juice and river water, followed by analysis with GC-MS. Eight milliliters of the sample solution is pumped at 0.5 mL min −1 flow rate into 12.0 μL extraction solvent (chloroform) and placed in the narrow-necked conical vessel for extraction and pre-concentration processes. Under optimal condition, the enrichment factor (EF) and linearity are found to be in the range of 102–380 and 500.0 μg L −1 with correlation coefficient greater than 0.98, respectively. The detection limit is in the range of 0.3–1.0 μg L −1 and LOQ ranged from 2.0–5.0 μg L −1 . The relative standard division (RSD) of six replicate measurements for three different concentrations (i.e., 15.0, 50.0, 150.0 μg L −1 ) is 3.8–8.4%, 2.6...

Determination of organophosphorus pesticide residues in human tissues by capillary gas chromatography–negative chemical ionization mass spectrometry analysis

Journal of Chromatography B, 2002

In the present work, a novel dispersive microextraction technique based on acetonitrile/water-coated Fe 3 O 4 was proposed to determine the organophosphorus pesticides (OPP) including phorate, diazinon, chlorpyrifosmethyl, pirimiphos-methyl and chlorpyrifos in edible oils. In the method, acetonitrile coated bare Fe 3 O 4 was used as the extractant, Fe 3 O 4 served as the supporter of acetonitrile, a trace amount of water acted as a crosslinking agent between acetonitrile and bare Fe 3 O 4 . The analytes adsorbed A/W-Fe 3 O 4 can be easily collected and isolated from the sample solution using a magnet before gas chromatography-mass spectrometry (GC-MS) analysis. Several dominant parameters affecting extraction efficiency were investigated and optimized. Under the optimal conditions, the limits of detection and limits of quantification for the five OPP were 1.1-6.7 and 4.8-18.3 ng/g, respectively. The recoveries in spiked real oil samples were in the range of 63.8-102.7 % with RSD between 4.9 and 14.3 %. The proposed simple, rapid and solvent-saving method was successfully applied to detect OPP in edible oils.