This study introduces a green approach to sample preparation by applying natural deep eutectic solvents (NADES) to determine phthalates in carbonated soft drinks using high-performance liquid chromatography with diode array detector (HPLC-DAD). The method employs hollow fiber-microporous membrane liquid-liquid microextraction combined with a 96-well plate system, utilizing fatty-acid-based DES in the pores of the membranes. This methodology substantially reduces the use of organic solvents, and its efficiency is comparable to or better than conventional methods.
View Article and Find Full Text PDFThis study utilized cork powder as a green alternative for extractor phase using the parallel-disposable pipette extraction (Pa-DPX) method for the determination of pesticides such as atrazine, carbofuran, diuron, and simazine from aqueous environmental samples. The separation/detection was performed by HPLC-DAD. Optimization experimental conditions was achieved through univariate and multivariate designs, resulting in the following parameters: 15 mg of cork as extractor phase, 7 extraction cycles with 7.
View Article and Find Full Text PDFThis work describes the development of a new automated parallel dispersive tip microextraction method (Au-Pa-DPX) for the determination of eleven polycyclic aromatic hydrocarbons (PAHs) in four samples of Brazilian sugarcane spirit beverages, with separation and detection done by the HPLC-DAD. The results obtained with the Au-Pa-DPX approach were also compared with those obtained via the conventional parallel manual DPX method with the same samples and optimized extraction process. Desorption solvent and cycles of desorption, cleaning and extraction were optimized using response surface methodology and univariate approaches.
View Article and Find Full Text PDFHerein, we report a KIO-catalyzed oxidative coupling of thiols to their corresponding disulfides in water, in a short time and at ambient temperature. The reaction has a broad scope and exhibits good functional group tolerance, resulting in the desired products in excellent yields. This approach allows the reuse of the reaction system in multiple cycles and scale-up.
View Article and Find Full Text PDFIn this study, different polyanilines were synthesized and evaluated for the determination of three hormones, including 17-β-estradiol, 17-α-ethinylestradiol, and estrone, in urine using a novel methodology based on thin film solid-phase microextraction technique, employing the sampling well plate system. The extractor phases, designated as polyaniline doped with hydrochloric acid, polyaniline doped with oxalic acid, polyaniline-silica doped with hydrochloric acid, and polyaniline-silica doped with oxalic acid, were characterized by electrical conductivity measurements, scanning electron microscopy, and Fourier transform infrared spectroscopy. The optimized extraction conditions were composed of 1.
View Article and Find Full Text PDFThis manuscript describes the development of magnetic restricted-access carbon nanotubes (M-RACNTs) for use as SPME sorbent to determine cannabidiol (CBD) and delta-9-tetrahydrocannabinol (THC) in human plasma samples by UHPLC-MS/MS. The adsorptive phase was immobilized on an SPME device by electromagnetic interactions between the M-RACNTs and a cylindrical neodymium magnet (3-mm diameter x 8-mm height) attached to a stainless-steel rod (3-mm diameter x 40-mm height). The M-RACNTs were synthesized by incorporating FeO magnetic nanoparticles (MNPs) into commercial carbon nanotubes (CNTs); then the surface of the resulting sorbent was further coated with a layer of bovine serum albumin (BSA).
View Article and Find Full Text PDFJ Chromatogr B Analyt Technol Biomed Life Sci
September 2022
In this work, hollow-fiber microporous membrane liquid-liquid extraction (HF-MMLLE) was associated with a 96-well plate system for the determination of estrone, 17-β-estradiol, estriol and 17-α-ethinylestradiol in urine samples. This method exhibited some advantages, such as low cost, easy application, high-throughput and environmentally-friendly aspects. The type of organic solvent to fill the membrane, ionic strength effect, sample dilution, extraction and desorption time, and desorption solvent were examined.
View Article and Find Full Text PDFA simple and rapid methodology was developed using hollow fiber membrane microporous and a 96-well plate system for a high throughput multiclass determination of endocrine disruptors in human urine (diclofenac, diazepam, carbamazepine, ibuprofen, naproxen, carbofuran, methyl parathion, 17-α-ethynyl estradiol, bisphenol A and benzophenone). The quantification and detection of the chemicals were carried out by an HPLC-diode array detector. The fixed conditions for carrying out the method optimization were 1.
View Article and Find Full Text PDFAnalytical chemistry has always been evolving towards techniques that are increasingly simple and effective and that conform to green principles. Disposable pipette extraction (DPX, also known as dispersive pipette tip solid phase extraction) is a recent technique that has become an interesting tool in sample preparation methodologies. The principle is based on a dynamic mixture between the matrix and the sorbent which allows rapid and effective extraction of analytes and provides vigorous clean-up of the samples.
View Article and Find Full Text PDFSynthetic drugs for recreational purposes are in constant evolution, and their consumption promotes a significant increase in intoxication cases, resulting in damaging public health. The development of analytical methodologies to confirm the consumption of illicit drugs in biological matrices is required for the control of these substances. This work exploited the development of an extraction method based on homogenous liquid-liquid microextraction with switchable hydrophilicity solvent (SHS) as extraction phase for the determination of the synthetic drugs 3,4-methylenedioxymethamphetamine, 3,4-methylenedioxyamphetamine and N-methoxybenzyl-methoxyphenylethylamine derivates (25B, 25C and 25I) in postmortem blood, followed by liquid chromatography coupled to mass spectrometry in tandem.
View Article and Find Full Text PDFCarbendazim (CBZ) is a fungicide employed in grape crop disease controls, and its maximum residue limit in food is regulated by specialized agencies. This study aimed to determine the CBZ content in the grape juices in a semi-quantitative classification model based on portable Ultraviolet-Visible spectroscopy and partial least squares with discriminant analysis. The sensitivity and specificity of the obtained model ranged from 83 to 100%, with the external validation set.
View Article and Find Full Text PDFClean water is one of the sustainable development goals set by the United Nations for 2030. The development of effective but worldwide affordable strategies is essential to guarantee this achievement. Photocatalysis technology fulfills these criteria whenever the photocatalyst is sustainable and nontoxic.
View Article and Find Full Text PDFIn this study, a biosorbent material with characteristics for the adsorption of organic compounds was used for a cork pellet-based bar adsorptive microextraction technique, as a new greener alternative for the determination of organochlorine compounds. Aldrin, chlordane, dieldrin, endrin, lindane, 4,4-DDD, 4,4-DDE, 4,4-DDT, α-endosulfan and β-endosulfan were analyzed in water samples (drinking water, stream water and river water) with separation/detection by gas chromatography and electron capture detection (GC/ECD). The parameters that can affect the sample preparation efficiency such as desorption solvent and time as well as extraction time and ionic strength were evaluated by multivariate and univariate designs.
View Article and Find Full Text PDFThis study presents a novel method for fluorine quantification determination by microwave-induced plasma optical emission spectrometry (MIP-OES). Due to the low temperature of this plasma, atomic emission of fluorine could not be measured, instead CaF molecular emissions were measured by using a calcium solution mixed in the spray chamber with the sample using a T-piece. Several wavelengths were studied to find the best signal to noise ratio for fluorine determination and 530.
View Article and Find Full Text PDFIn this study, a lab-made parallel single-drop microextraction methodology using the magnetic ionic liquid trihexyltetradecylphosphonium tetrachloromanganate (II) as extraction solvent was developed to determine the pesticides tebuconazole, pendimethalin, dichlorodiphenyltrichloroethane, and dichlorodiphenyldichloroethylene in human urine samples. The experimental setup consisted of a 96-well plate system containing a set of magnetic pins that allowed for the manipulation of up to 96 samples simultaneously, providing an enhanced drop stability compared to traditional single-drop microextraction approaches. The optimal conditions employed 5.
View Article and Find Full Text PDFThe development and application of alternative green solvents in analytical techniques consist of trends in sample preparation, since this subject represents an important step toward sustainability in experimental procedures. This review is focused on the main theoretical aspects related to deep eutectic solvents (DES), switchable hydrophilicity solvents (SHS) and supramolecular solvents (SUPRAS). Recent applications are highlighted, particularly for the extraction of different analytes from environmental, biological and food matrices.
View Article and Find Full Text PDFIn this work, a novel and high-throughput parallel-dispersive droplet extraction (Pa-DDE) based on in situ formation of the hydrophobic MILs ([Co(CIM)]2[NTf], [Ni(CIM)]2[NTf] and [Ni(BeIM)]2[NTf]) is demonstrated, for the first time, for the determination of benzophenone, metolachlor, triclocarban, pendimethalin, 4-methylbenzylidene camphor, and 2-ethylhexyl-4-methoxycinnamate from aqueous environmental samples. This experimental setup is comprised of a 96-well plate system containing a set of magnetic pins which were used to collect the MIL droplet after in situ formation. This consolidated system enabled simultaneous extraction of up to 96 samples and MIL production in one step.
View Article and Find Full Text PDFSci Total Environ
March 2021
DDT (1,1,1-trichloro-2,2-bi(p-chlorophenyl)-ethane) and its metabolites (DDD, 1,1-dichloro-2,2-bis-(4'-chlorophenyl)ethane, and DDE, 1,1-dichloro-2,2-bis-(4'-chlorophenyl)ethylene) are persistent organic pollutants that can be catalytically degraded into a less toxic and less persistent compound. In this work, ecofriendly methodologies for catalyst synthesis, catalytic degradation of DDT and reaction monitoring have been proposed. Three types of Pd-based nanoparticles, NPs, (Pd, Au-on-Pd and Cu-on-Pd) were synthesized and used for catalytic hydrodechlorination of DDT and its metabolites.
View Article and Find Full Text PDFIn widespread use in commercial products as plasticizers, phthalic acid esters (phthalates) have worried researchers and society in general, given the negative impacts on living organisms, especially human health. Since they are not chemically linked to the polymeric matrix, their migration is evident for samples that come into contact with plastics that contain them, such as water, food and saliva. In this work, a new strategy is described, named parallel-disposable pipette extraction (Pa-DPX), in a fast, efficient and robust analytical method using five simultaneous extractions for the determination of migration of 6 phthalates from common plastic materials (children's toys, school supplies, dog toys and oral contact items) to saliva simulant, using gas chromatography-mass spectrometry (GC-MS).
View Article and Find Full Text PDFBisphenol A is a synthetic compound widely used in industry, in the production of polycarbonate, epoxy resins, and thermal paper, among others. Its annual production is estimated at millions of tons per year, demonstrating its importance. Despite its wide application in various everyday products, once in the environment (due to its disposal or leaching), it has high toxicity to humans and animal life, and this problem has been well known for years.
View Article and Find Full Text PDFThis study reports a novel and environmentally friendly method based on bar adsorptive microextraction (BAμE) with cork pellet as extraction phase for the determination of methylparaben, ethylparaben, propylparaben and butylparaben in river water samples. This natural approach consists of a cork pellet recycled from wine stoppers used as biosorbent material to replace the traditional BAμE device. The analytical determinations were performed using a high-performance liquid chromatography-diode array detector (HPLC-DAD).
View Article and Find Full Text PDFThis study reports the use ofa natural deep eutectic solvent (NADES) with hollow fiber-microporous membrane liquid-liquid microextraction (HF-MMLLE) for the multiclass determination of 11 compounds classified as emerging contaminantsin water. Different deep eutectic solvents were synthetized and Thymol: Camphor (1:1 molar fraction) wasused as extraction solvent. The Thymol:Camphor was impregnated into the polypropylene membrane porous for 10 min, replacing commonly used solvents (ex.
View Article and Find Full Text PDFEnviron Sci Pollut Res Int
December 2020
The evaluation of the concentration of pesticides in drinking water presents a real concern. In this study, a simple and rapid method based on solid-phase microextraction (SPME) followed by gas chromatography-mass spectrometry and electron capture detectors was developed aiming at multiclass determination of 23 pesticides regulated by the Brazilian legislation. The extraction was carried out by direct immersion mode (DI-SPME) using DVB/Car/PDMS fiber coating.
View Article and Find Full Text PDFIn this study, a novel and straightforward analytical methodology was proposed for the determination of cocaine (COC) and its main metabolites benzoylecgonine (BZE) cocaethylene (CE) and hydroxy‑cocaine (COCOH) in urine samples. This approach consisted of a high-throughput and semiautomated configuration based on hollow-fiber renewal liquid membrane extraction (HFRLM) coupled to a 96-well plate system, which was proposed for the first time to analyze complex biological samples such as urine. The analytical determinations were performed using ultra-high performance liquid chromatography coupled to quadrupole time-of-flight-mass spectrometry (LC-ESI-QTOF-MS).
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