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1.
Zhongguo Zhong Yao Za Zhi ; 45(16): 3952-3960, 2020 Aug.
Artigo em Chinês | MEDLINE | ID: mdl-32893594

RESUMO

A method of ultra-high performance liquid chromatography coupled with quadrupole/electrostatic field Obitrap high-resolution mass spectrometry(UHPLC-Q-Exactive MS) was established to comprehensively identify the metabolites of carnosic acid in rats. After oral gavage of carnosic acid CMC-Na suspension in rats, urine, plasma and feces samples were collected and pretreated by solid phase extraction(SPE). Acquity UPLC BEH C_(18 )column(2.1 mm×100 mm, 1.7 µm) was used with 0.1% formic acid solution(A)-acetonitrile(B) as the mobile phase for the gradient elution. Biological samples were analyzed by quadrupole/electrostatic field Obitrap high-resolution mass spectrometry in positive and negative ion mode. Based on the accurate molecular mass, fragment ion information, and related literature reports, a total of 28 compounds(including carnosic acid) were finally identified in rat samples. As a result, the main metabolic pathways of carnosic acid in rats are oxidation, hydroxylation, methylation, glucuronide conjugation, sulfate conjugation, S-cysteine conjugation, glutathione conjugation, demethylation, decarbonylation and their composite reactions. The study showed that the metabolism of carnosic acid in rats could be efficiently and comprehensively clarified by using UHPLC-Q-Exactive MS, providing a reference for clarifying the material basis and metabolic mechanism of carnosic acid.


Assuntos
Abietanos , Extração em Fase Sólida , Animais , Cromatografia Líquida de Alta Pressão , Espectrometria de Massas , Ratos
2.
Chemosphere ; 254: 126872, 2020 Sep.
Artigo em Inglês | MEDLINE | ID: mdl-32957284

RESUMO

The distribution of 20 personal care products (PCPs), including seven preservatives, six UV filters, five anticorrosion agents, and two antimicrobials, were determined in 40 swimming pools using solid phase extraction followed by liquid chromatography-tandem mass spectrometry. Among 14 targets detected, 1H-benzotriazole and triclocarban were observed in all samples. The detected concentrations of preservatives, UV filters, anticorrosion agents, and antimicrobials were in the ranges of not detected (nd)-179 ng L-1, nd-289 ng L-1, nd-58.4 ng L-1, and nd-56.9 ng L-1, respectively. The presence of preservatives, UV filters and antimicrobials in pool waters might be mainly brought in by human activities while anticorrosion agents were mainly from the source water. Furthermore, the concentrations of methylparaben, ethylparaben, 1H-benzotriazole, 5-methyl-1H-benzotriazole, 5-chloro-1H-benzotriazole, and 5,6-dimethyl-1H-benzotriazole in indoor pools were found higher than those in outdoor pools. The longer opening time and weaker light intensity for indoor pools might cause the difference. The redundancy analysis showed significantly negative correlations between the concentrations of parabens and the contents of residual chlorine in the pool waters. A higher chlorine residue may promote the decomposition of parabens. Health risk assessment showed that skin penetration would be the main approach for the intake of PCPs by swimmers while swimming. Compared with the non-athletic swimmers, the athletic swimmers might be more sensitive, but the health risks for both groups of swimmers could be negligible.


Assuntos
Cosméticos/análise , Monitoramento Ambiental , Poluentes Químicos da Água/análise , Carbanilidas , Cloro/análise , Cromatografia Líquida , Humanos , Parabenos , Medição de Risco , Extração em Fase Sólida , Natação , Piscinas , Triazóis
3.
Environ Monit Assess ; 192(9): 583, 2020 Aug 15.
Artigo em Inglês | MEDLINE | ID: mdl-32803620

RESUMO

In this study, a new analytical strategy was developed to determine trace cadmium in aqueous samples with high sensitivity and accuracy. A combination of magnetic nickel nanoparticles (Ni-MNPs) based dispersive solid-phase extraction (DSPE) and flame atomic absorption spectrometry fitted with a slotted quartz tube (SQT-FAAS) lowered the detection limit of cadmium. The magnetic Ni nanoparticles were synthesized, characterized, and thoroughly optimized in a stepwise approach. The quartz tube was custom cut in the laboratory to suit the specifics of the flame burner. Using the optimized conditions, a limit of detection value of 0.58 µg/L and limit of quantification value of 1.93 µg/L were obtained. To demonstrate accuracy and applicability of the developed method, well water samples were analyzed for their Cd content, and matrix effect on the extraction yield was investigated. The percent recovery results calculated ranged from 93.8 to 108.2%, with corresponding standard deviation values ranging from 1.7 to 7.7. These results established the developed method as sensitive, accurate, and precise for determination of cadmium at trace levels.


Assuntos
Microextração em Fase Líquida , Poluentes Químicos da Água/análise , Cádmio/análise , Monitoramento Ambiental , Fenômenos Magnéticos , Quartzo , Extração em Fase Sólida , Espectrofotometria Atômica
4.
J Chromatogr A ; 1626: 461324, 2020 Aug 30.
Artigo em Inglês | MEDLINE | ID: mdl-32797817

RESUMO

Sorption of PFASs onto surfaces of laboratory materials has been frequently reported. Due to the often complex and poorly understood nature of such sorption, workarounds have often included use of whole samples only, accompanied by sample vessel rinsing to desorb active surfaces. The resulting methods tend to require considerable sample preparation times and preclude typical activities such as aliquoting and dilution of water samples prior to extraction. This manuscript reports an approach for PFAS analysis which uses subsampling of water matrices from vessels including centrifuge tubes and autosampler vials, through the optimized use of solvent to reduce PFAS retention on subsampling vessels. Online solid phase extraction (SPE) using a weak anion exchange resin is then used to concentrate sample aliquots to improve sensitivity and allow for removal of matrix interferences. With the technique of ultra performance liquid chromatography (UPLC) coupled to isotope dilution tandem mass spectrometry, statistically based quantitation limits ranged from sub ng/L to single digit ng/L for carboxylate, sulfonate, and sulfonamide PFASs analytes from C4 to C12. Linear calibration ranges were from 0.25 to 4000 ng/L. Matrix effects relevant for drinking water treatment studies, such as cations, organic carbon, and competing PFAS compounds, were evaluated and found to not impact method performance within QC criteria consistent with study data quality objectives.


Assuntos
Fluorcarbonetos/análise , Indicadores e Reagentes/análise , Espectrometria de Massas em Tandem/métodos , Cromatografia Líquida de Alta Pressão , Fluorcarbonetos/isolamento & purificação , Água Doce/análise , Indicadores e Reagentes/isolamento & purificação , Marcação por Isótopo , Sais/química , Extração em Fase Sólida , Poluentes Químicos da Água/análise , Poluentes Químicos da Água/isolamento & purificação
5.
J Chromatogr A ; 1626: 461359, 2020 Aug 30.
Artigo em Inglês | MEDLINE | ID: mdl-32797838

RESUMO

The enantiomeric determination of chiral drugs in the environment is of emerging concern since their enantiomers often exhibit stereoselectivity in environmental occurrence, fate and toxicity. In this study a method based on solid-phase extraction followed by chiral liquid chromatography and high-resolution mass spectrometry has been developed for the enantiomeric determination of a group of cathinones in river water and effluent wastewater. The enantioseparation was carried out using a Chiralpak CBH column in reversed-phase mode, and optimised by evaluating the effects of flow rate, buffer concentration and organic modifier. Under optimal conditions, good enantioseparations (Rs ≥1.2) were achieved for all the analytes. Two mixed-mode cation-exchange sorbents (Oasis WCX and Oasis MCX) in solid-phase extraction were evaluated in river water. Oasis MCX sorbent showed better performance with apparent recoveries ranging from 57 to 91% and matrix effect ranging from -10 to 15%. It is worth noting that a shifting of retention times and loss of enantioresolutions in environmental water samples was observed for all the analytes when the Oasis WCX sorbent was used. The method was validated with river water and effluent wastewater samples and its overall performance was satisfactory. The method quantification limits for all the analyte enantiomers ranged from 1.0 to 2.9 ng/L in river water, and from 2.3 to 6.0 ng/L in effluent wastewater. The repeatability and reproducibility values, expressed as% relative standard deviation (n = 5) were less than 15%. The method was then applied to the analysis of river water and effluent wastewater. The racemic methylone and methedrone (EF=0.49 and 0.46, respectively) were detected at low ng/L in some of the river water samples.


Assuntos
Alcaloides/análise , Cromatografia Líquida/métodos , Espectrometria de Massas/métodos , Alcaloides/química , Alcaloides/isolamento & purificação , Reprodutibilidade dos Testes , Rios/química , Extração em Fase Sólida/métodos , Estereoisomerismo , Águas Residuárias/química , Poluentes Químicos da Água/análise , Poluentes Químicos da Água/química , Poluentes Químicos da Água/isolamento & purificação
6.
J Chromatogr A ; 1626: 461362, 2020 Aug 30.
Artigo em Inglês | MEDLINE | ID: mdl-32797841

RESUMO

Exploring new material as adsorbent for the efficient enrichment of pollutants is always of great significance in analytical chemistry. In this work, a magnetic azobenzene framework (labeled as MAzo) was constructed as a magnetic solid phase extraction (MSPE) adsorbent by a simple and environmentally benign strategy. The MAzo exhibited the attractive features of strong magnetism, outstanding adsorption performance, as well as good reusability. Combining MAzo-based MSPE with high performance liquid-phase chromatography, a simple and effective method was developed for simultaneous determination of four phenylurea herbicides in pear juice and apple juice samples. Under optimized experimental conditions, the method offered low limits of detection of 0.05-0.15 ng mL-1, high recoveries of 86.7-109.2% with RSD less than 7%. Density functional theory calculation indicated that the good adsorption performance of MAzo for PUHs can be ascribed to the strong H-bonding forces and weak π-π interactions. The facile, green, low-cost synthesis method together with the excellent adsorption performance endows the MAzo great application prospect in sample preparation.


Assuntos
Compostos Azo/química , Poluentes Ambientais/análise , Herbicidas/análise , Compostos de Fenilureia/análise , Extração em Fase Sólida/métodos , Adsorção , Cromatografia Líquida de Alta Pressão , Poluentes Ambientais/isolamento & purificação , Sucos de Frutas e Vegetais/análise , Herbicidas/isolamento & purificação , Fenômenos Magnéticos , Malus , Estruturas Metalorgânicas , Compostos de Fenilureia/isolamento & purificação , Pyrus
7.
J Chromatogr A ; 1626: 461364, 2020 Aug 30.
Artigo em Inglês | MEDLINE | ID: mdl-32797843

RESUMO

A new type of restricted access media-imprinted nanomaterials (RAM-MIPs) were successfully prepared on the surface of metal-organic framework by reversible addition fragmentation chain transfer polymerization technology. Then it was applied as a dispersed solid phase extraction (DSPE) material in analysis of fluoroquinolones (ofloxacin, pefloxacin, norfloxacin, enrofloxacin and gatifloxacin) in untreated milk and river water by HPLC-UV detection. The resulted material has a good binding amounts (60.81 mg g-1), rapid binding kinetic (15 min) and satisfactory selectivity as well as has a good ability to eliminate matrix interference. Several major factors affecting DSPE efficiency, pH of sample solution, dosage of RAM-MIPs, adsorption time and volume ratios of elution solvent were primarily optimized. In optimization conditions, RAM-MIPs-DSPE was combined with HPLC-UV to enrich fluoroquinolones in untreated milk and river water, achieving satisfactory linear correlation (R2 > 0.9988), good limits of detection (LOD, 1.02-3.15 µg L-1 for milk and 0.93-2.87 µg L-1 for river water) and better recoveries (80.7-103.5% and 85.1-105.9% with relative standard deviation (RSD) of not higher than 5.3% and 4.7% for milk and river water samples, respectively). The research results illustrate that it provides a simple and efficient method for the direct detection of FQs in complex samples.


Assuntos
Antibacterianos/análise , Fluoroquinolonas/análise , Estruturas Metalorgânicas/química , Leite/química , Nanoestruturas/química , Rios/química , Extração em Fase Sólida/métodos , Adsorção , Animais , Antibacterianos/isolamento & purificação , Cromatografia Líquida de Alta Pressão , Fluoroquinolonas/isolamento & purificação , Impressão Molecular , Polimerização
8.
J Chromatogr A ; 1627: 461395, 2020 Sep 13.
Artigo em Inglês | MEDLINE | ID: mdl-32823100

RESUMO

Nowadays, enantioseparation of racemic pharmaceuticals in preparations is a prime concern by drug authorities across the globe. In the present work, it was attempted to develop novel enantioselective extraction method for five clinically used drugs (atenolol, propranolol, metoprolol, racecadotril, and raceanisodamine in their tablets) as racemates. The enantioselective solid-liquid extraction of these racemic drugs was carried out successfully by the use of chiral ionic liquid (CIL) in combination with a metal organic framework (MOF) for the first time. The composite CIL@MOF was synthesized from tropine based chiral ionic liquids with L-proline anion ([CnTr][L-Pro], n=3-6) and HKUST-1 type MOF, which was comprehensively characterized before being used as sorbent for enantioselective dispersive solid-liquid extraction. Preliminary selection of appropriate CIL was carried out on thin layer chromatography (TLC); under the joint participation of copper ion in the developing reagent, [C3Tr][L-Pro] ionic liquid showed better resolution performance with ΔRf value of 0.35 between the enantiomers was obtained for racemic atenolol. Moreover, the effect of copper salt dosage, amount of CIL, soli-liquid ratio and extraction time were investigated. The optimal conditions were obtained after thorough investigations; i.e. sample solution: ethanol, elution solvent: methanol, solid-liquid ratio: 12.5 mg:50 mL, amount of copper salt: 8 mg L-1, amount of impregnated CIL: 30% and extraction time of 30 min. As a result, enantiomeric excess values are 90.4%, 95%, 92%, 81.6% and 83.2% for atenolol, propranolol, metoprolol, racecadotril and raceanisodamine, respectively. The developed enantioselective method was validated following ICH guidelines and it was proved to be simple, effective and enantioselective way for separation of racemic pharmaceuticals with similar behaviors.


Assuntos
Líquidos Iônicos/química , Estruturas Metalorgânicas/química , Preparações Farmacêuticas/isolamento & purificação , Extração em Fase Sólida/métodos , Antagonistas Adrenérgicos beta/análise , Antagonistas Adrenérgicos beta/isolamento & purificação , Atenolol/análise , Atenolol/isolamento & purificação , Cromatografia Líquida de Alta Pressão/métodos , Cobre/química , Metoprolol/análise , Metoprolol/isolamento & purificação , Preparações Farmacêuticas/análise , Propranolol/análise , Propranolol/isolamento & purificação , Solventes/química , Estereoisomerismo
9.
J Chromatogr A ; 1627: 461398, 2020 Sep 13.
Artigo em Inglês | MEDLINE | ID: mdl-32823103

RESUMO

A new mode of dispersive solid phase extraction based on in situ formation of adsorbent in aqueous phase has been introduced as an efficient method for the extraction of some pesticide residues in fruit juice samples. In this method, polycarbonate which is an inexpensive polymer is used as an adsorbent for the first time. The method is followed by dispersive liquid-liquid microextraction for more enrichment of the analytes. In the present study, a proper amount of the polymer is dissolved in N,N-dimethyl formamide and the obtained solution is injected into an aqueous phase containing the analytes. After injection, polycarbonate particles are formed and adsorbed the analytes. Then, the adsorbent is separated from the aqueous solution and eluted by acetone. The obtained acetone phase is mixed with 1,1,1-trichloroethane and the mixture is dispersed into deionized water and a cloudy solution is formed. Ultimately, after centrifugation, the obtained sedimented phase containing the extracted analytes is injected into gas chromatography-flame ionization detection. In the proposed method, the adsorbent synthesis step, which often is a time-consuming, expensive, and laborious step in most adsorbent-based sample preparation methods, has been removed. Moreover, there is no need for sonication or vortex agitation. Under the optimized experimental conditions, the relative standard deviation was equal or less than 7% for intra- (n = 6) and inter-day (n = 5) precisions at a concentration of 50 µg L-1 of each pesticide. The limits of detection and quantification were in the ranges of 0.34-1.2 and 1.1-4.0 µg L-1, respectively. In addition, extraction recoveries and enrichment factors varied in the ranges of 44-89% and 220-443, respectively.


Assuntos
Sucos de Frutas e Vegetais/análise , Cromatografia Gasosa-Espectrometria de Massas/métodos , Resíduos de Praguicidas/análise , Centrifugação , Limite de Detecção , Microextração em Fase Líquida/métodos , Resíduos de Praguicidas/isolamento & purificação , Extração em Fase Sólida , Solventes/química , Triazinas/análise , Triazinas/isolamento & purificação , Água/química
10.
J Chromatogr A ; 1627: 461399, 2020 Sep 13.
Artigo em Inglês | MEDLINE | ID: mdl-32823104

RESUMO

Citrinin is a toxic small organic molecule produced as a secondary metabolite by fungi types Penicillium, Monascus and Aspergillus and is known to contaminate various food commodities during postharvest stages of food production. During the last 10 years, most reported methods for citrinin analysis employed enzyme-linked immunosorbent assays or high-performance liquid chromatography. Over this same time period, liquid extraction, solid-phase extraction, dispersive liquid-liquid microextraction and QuEChERS were the most cited sample preparation and clean-up methods. In this review the advantages and disadvantages of the various sample preparation, separation and detection methods for citrinin analysis over the last decade are evaluated. Furthermore, current trends, emerging technologies and the future prospects of these methods are discussed.


Assuntos
Cromatografia Líquida de Alta Pressão/métodos , Citrinina/análise , Espectrometria de Massas em Tandem/métodos , Aspergillus/metabolismo , Citrinina/isolamento & purificação , Citrinina/urina , Ensaio de Imunoadsorção Enzimática , Contaminação de Alimentos/análise , Humanos , Microextração em Fase Líquida , Monascus/metabolismo , Extração em Fase Sólida
11.
J Chromatogr A ; 1628: 461440, 2020 Sep 27.
Artigo em Inglês | MEDLINE | ID: mdl-32822980

RESUMO

A selective and highly sensitive high performance liquid chromatography (HPLC) with fluorescence derivatization method was developed for determination of ethinyl estradiol (EE); one of endocrine-disrupting compounds (EDCs). The fluorescence derivatization procedure was based on Sonogashira coupling reaction using 4-(4, 5-diphenyl-1H-imidazole-2-yl) iodobenzene (DIB-I), a fluorescence labeling reagent, to derivatize EE in presence of copper and palladium ions. The formed fluorescent product was separated on Cosmosil 5C18 MS-II by an isocratic elution with a mobile phase composed of acetonitrile: 5.0 mM Tris-HNO3 buffer, pH 7.4 (60:40, v/v %). The detection wavelengths were set at 310 and 400 nm as excitation and emission wavelengths, respectively. Various parameters affecting derivatization reaction were optimized. Further, the proposed method was validated and a good linearity with low detection limit (S/N=3) 7.4 ng L-1 was obtained in water sample after a simple solid-phase disk extraction (C18 SPE disk) method. The proposed method was successfully applied for detection of EE in river water samples in order to monitor EE concentration and to distinguish its effect on the ecosystem and human health.


Assuntos
Cromatografia Líquida de Alta Pressão , Monitoramento Ambiental/métodos , Etinilestradiol/análise , Rios/química , Espectrometria de Fluorescência , Disruptores Endócrinos/análise , Fluorescência , Extração em Fase Sólida , Poluentes Químicos da Água/análise
12.
J Anal Toxicol ; 44(7): 708-717, 2020 Oct 12.
Artigo em Inglês | MEDLINE | ID: mdl-32808043

RESUMO

An analytical method for the detection of 40 benzodiazepines, (±)-zopiclone, zaleplon and zolpidem in blood and urine by solid-phase extraction liquid chromatography-tandem mass spectrometry was developed and validated. Twenty-nine of 43 analytes were quantified in 0.5 mL whole blood for investigating postmortem, drug-facilitated sexual assault (DFSA) and driving under the influence of drugs cases (DUID). The four different dynamic ranges of the seven-point, linear, 1/x weighted calibration curves with lower limits of quantification of 2, 5, 10 and 20 µg/L across the analytes encompassed the majority of our casework encountered in postmortem, DFSA and DUID samples. Reference materials were available for all analytes except α-hydroxyflualprazolam, a hydroxylated metabolite of flualprazolam. The fragmentation of α-hydroxyflualprazolam was predicted from the fragmentation pattern of α-hydroxyalprazolam, and the appropriate transitions were added to the method to enable monitoring for this analyte. Urine samples were hydrolyzed at 55°C for 30 min with a genetically modified ß-glucuronidase enzyme, which resulted in >95% efficiency measured by oxazepam glucuronide. Extensive sample preparation included combining osmotic lysing and protein precipitation with methanol/acetonitrile mixture followed by freezing and centrifugation resulted in exceptionally high signal-to-noise ratios. Bias and between-and within-day imprecision for quality controls (QCs) were all within ±15%, except for clonazolam and etizolam that were within ±20%. All 29 of the 43 analytes tested for QC performance met quantitative reporting criteria within the dynamic ranges of the calibration curves, and 14 analytes, present only in the calibrator solution, were qualitatively reported. Twenty-five analytes met all quantitative reporting criteria including dilution integrity. The ability to analyze quantitative blood and qualitative urine samples in the same batch is one of the most useful elements of this procedure. This sensitive, specific and robust analytical method was routinely employed in the analysis of >300 samples in our laboratory over the last 6 months.


Assuntos
Benzodiazepinas/metabolismo , Hipnóticos e Sedativos/metabolismo , Detecção do Abuso de Substâncias/métodos , Alprazolam/análogos & derivados , Compostos Azabicíclicos/sangue , Compostos Azabicíclicos/metabolismo , Compostos Azabicíclicos/urina , Benzodiazepinas/sangue , Benzodiazepinas/urina , Cromatografia Líquida/métodos , Diazepam/análogos & derivados , Toxicologia Forense , Humanos , Hipnóticos e Sedativos/análise , Hipnóticos e Sedativos/sangue , Hipnóticos e Sedativos/urina , Limite de Detecção , Piperazinas/sangue , Piperazinas/metabolismo , Piperazinas/urina , Medicamentos Indutores do Sono/sangue , Medicamentos Indutores do Sono/metabolismo , Medicamentos Indutores do Sono/urina , Extração em Fase Sólida/métodos , Espectrometria de Massas em Tandem/métodos , Zolpidem/sangue , Zolpidem/metabolismo , Zolpidem/urina
13.
J Chromatogr A ; 1627: 461382, 2020 Sep 13.
Artigo em Inglês | MEDLINE | ID: mdl-32823094

RESUMO

A method is described for the functionalization of magnetic carbon nanotubes to recognize aristolochic acid Ⅰ and Ⅱ. 3-Glycidyloxypropyltrimethoxysilane was used as a coupling agent to immobilize adenine on a solid support. The morphology and structure of adenine-coated magnetic carbon nanotubes was investigated using transmission electron microscopy (TEM), scanning electron microscopy (SEM), X-ray diffraction (XRD) and a vibrating sample magnetometer (VSM). The adsorption performance of the adenine-coated magnetic carbon nanotubes was evaluated via adsorption isotherms, the kinetics and selectivity tests. The adsorption capacity of the adenine-functionalized sorbent for aristolochic acid Ⅰ was determined to be 24.5 µg mg-1. By combining magnetic solid phase extraction with HPLC detection, a method was developed to enrich and detect aristolochic acids used in traditional Chinese medicine. A satisfactory recovery (92.7 - 97.5% for aristolochic acid Ⅰ and 92.6 - 99.4% for aristolochic acid Ⅱ) and an acceptable relative standard deviation (<4.0%) were obtained.


Assuntos
Adenina/química , Ácidos Aristolóquicos/isolamento & purificação , Fenômenos Magnéticos , Nanotubos de Carbono/química , Adsorção , Medicamentos de Ervas Chinesas/química , Compostos Férricos/síntese química , Compostos Férricos/química , Concentração de Íons de Hidrogênio , Cinética , Nanocompostos/química , Nanotubos de Carbono/ultraestrutura , Concentração Osmolar , Reprodutibilidade dos Testes , Dióxido de Silício/síntese química , Dióxido de Silício/química , Extração em Fase Sólida , Temperatura , Difração de Raios X
14.
J Chromatogr A ; 1627: 461387, 2020 Sep 13.
Artigo em Inglês | MEDLINE | ID: mdl-32823095

RESUMO

A simple and efficient magnetic solid-phase extraction (MSPE) method was established with magnetic covalent organic framework (COF) as adsorbent to enrich organophosphorus pesticides from fatty milk samples, followed by the sensitive determination via LC-MS/MS. The key parameters influencing the MSPE efficiency were comprehensively investigated to afford an optimized procedure. All the target analytes could be captured directly by magnetic COF from milk without protein precipitation, making the pretreatment rapid and convenient. Systematic method validation demonstrated its satisfactory linearity, recoveries (80.0-105 %), and precision (RSDs <12.3 %). The method limits of quantification were 0.2-0.5 µg L-1. A comparison experiment to the reported solid-phase extraction fully verified the present MSPE more rapid, accurate, and environment-friendly. Furthermore, FT-IR and XPS analysis were performed to reveal the adsorption mechanisms of magnetic COF to organophosphorus pesticides, which could offer guidance on the rational design of COF adsorbent for various target analytes.


Assuntos
Fenômenos Magnéticos , Estruturas Metalorgânicas/química , Leite/química , Compostos Organofosforados/análise , Praguicidas/análise , Extração em Fase Sólida/métodos , Acetonitrilos/análise , Adsorção , Animais , Limite de Detecção , Espectroscopia Fotoeletrônica , Padrões de Referência , Reprodutibilidade dos Testes , Solventes/química , Espectroscopia de Infravermelho com Transformada de Fourier
15.
J Chromatogr A ; 1627: 461390, 2020 Sep 13.
Artigo em Inglês | MEDLINE | ID: mdl-32823096

RESUMO

A dispersive solid phase extraction method was combined with deep eutectic solvent-based solidification of floating organic drop-dispersive liquid-liquid microextraction and used for the extraction/preconcentration of some organophosphorus pesticides residues from edible oil samples. The extracted analytes were quantified with gas chromatography-nitrogen phosphorous detector. In this procedure, the sample lipids are saponified with a sodium hydroxide solution and then the analytes are adsorbed onto a primary secondary amine sorbent. After that the analytes are desorbed with acetone as an elution/dispersive solvent and mixed with choline chloride: 3,3-dimethyl butyric acid deep eutectic solvent and the mixture is rapidly dispersed into deionized water. Then, the obtained cloudy solution is centrifuged and placed into an ice bath. The extraction solvent is solidified on the top of the solution. Finally, it is removed and dissolved in acetonitrile, and 1 µL of the solution is injected into the separation system. Validation of the method showed that limits of detection and quantification were in the ranges of 0.06-0.24 and 0.20-0.56 ng mL-1, respectively. Enrichment factors and extraction recoveries of the analytes ranged from 170-192 and 68-77%, respectively. The method had an acceptable precision with relative standard deviations less than ≤9.2% for intra- (n=6) and inter-day (n=6) precisions at four concentrations (3, 10, 50, and 250 ng mL-1, each analyte). Finally the method was used for determination of the analytes in five edible oil samples.


Assuntos
Microextração em Fase Líquida/métodos , Compostos Organofosforados/análise , Praguicidas/análise , Óleos Vegetais/química , Extração em Fase Sólida/métodos , Solventes/química , Acetonitrilos/química , Reprodutibilidade dos Testes , Hidróxido de Sódio/química , Soluções , Sonicação , Fatores de Tempo
16.
Ecotoxicol Environ Saf ; 204: 111042, 2020 Nov.
Artigo em Inglês | MEDLINE | ID: mdl-32738626

RESUMO

Paralytic shellfish poisoning (PSP) toxins have received considerable attention in recent years because of their adverse effects on marine breeding industries and human health. In this study, a reliable method for the analysis of extracellular PSP toxins in the culture medium of marine toxic dinoflagellates was developed for the first time using graphitized carbon black-solid-phase extraction and hydrophilic interaction liquid chromatography-high-resolution mass spectrometry. The limit of quantification of typical PSP toxins in algal culture medium ranged from 0.072 µg/L to 0.151 µg/L under optimal conditions. Satisfactory absolute recoveries (87.5%-102.4%), precision (relative standard deviation ≤ 7.6%), and linearity (R2 ≥ 0.9998) were also achieved. In addition, the proposed method was applied to screen and determine the extracellular PSP toxins of two typical toxigenic dinoflagellates, Alexandrium minutum and Alexandrium tamarense. The total concentrations of the extracellular PSP toxins in A. minutum and A. tamarense over the whole growth period were within 2.0-735.5 and 2.0-19.2 µg/L, respectively. The concentrations of extracellular PSP toxins varied remarkably in the different growth stages of A. minutum and A. tamarense, and the contents of some extracellular PSP toxins were substantially higher than those of intracellular PSP toxins. Therefore, the extracellular PSP toxins released by toxigenic red tide algae cannot be ignored, and their environmental fate, bioavailability, and potential harm to aquatic environment need to be investigated in future studies.


Assuntos
Cromatografia Líquida/métodos , Meios de Cultura/química , Dinoflagelados/metabolismo , Toxinas Marinhas/análise , Espectrometria de Massas/métodos , Extração em Fase Sólida/métodos , Interações Hidrofóbicas e Hidrofílicas , Intoxicação por Frutos do Mar , Fuligem/química
17.
J Chromatogr A ; 1626: 461328, 2020 Aug 30.
Artigo em Inglês | MEDLINE | ID: mdl-32797818

RESUMO

Ferric oxide/carbon (Fe2O3@C) was fabricated via direct carbonization of metal-organic framework of iron (MOF-235) under argon atmosphere. The magnetic Fe2O3 nanoparticles are evenly embedded in porous carbon matrix, while original morphology of MOF-235 was well-maintained. The synthesized Fe2O3@C was used as magnetic sorbent for extracting five benzoylurea insecticides (BUs). The materials exhibited excellent extraction performance, which benefited not only from the strong π-π interaction and hydrophobic interaction (π-conjugated system), but also to the abundant adsorption sites and flexible transport channel (the interconnected 3D porous structure). A three-factor-three-level Box-Behnken design (BBD) was selected to optimize three greatly influential parameters: amount of adsorbent (A), desorption time (B) and volume of desorption solvent (C) by response surface methodology. The established method coupled to HPLC-UV detection showed wide linearity with the range of 0.2-450 µg•L-1, relatively low limits of detection (0.05-0.10 µg•L-1) with the relative standard deviation (RSD) (n = 7) lower t than 5.47%. Moreover, the proposed method was successfully applied to analyze BUs in tea samples and investigate the removal effect of different washing on BUs residues from tea leaf. These results indicated that the synthesized Fe2O3@C is a promising adsorbent material for magnetic solid phase extraction of BUs at trace concentrations from tea samples.


Assuntos
Inseticidas/análise , Nanopartículas de Magnetita/química , Estruturas Metalorgânicas/química , Chá/química , Ureia/análise , Adsorção , Carbono/química , Cromatografia Líquida de Alta Pressão/métodos , Cromatografia Líquida de Alta Pressão/normas , Compostos Férricos/química , Inseticidas/isolamento & purificação , Inseticidas/normas , Limite de Detecção , Porosidade , Padrões de Referência , Extração em Fase Sólida , Espectrofotometria Ultravioleta , Chá/metabolismo , Ureia/análogos & derivados , Ureia/isolamento & purificação , Ureia/normas
18.
J Chromatogr A ; 1626: 461346, 2020 Aug 30.
Artigo em Inglês | MEDLINE | ID: mdl-32797826

RESUMO

A molecularly imprinted polymer was synthesized and characterized to be used as solid-phase extraction sorbent for simultaneous chlorpyrifos and diazinon and their oxon derivatives. Several imprinted polymers were prepared and evaluated in a retention study of these analytes compared with a non-printed polymer. Several parameters affecting the extraction of imprinted polymer such as washing solvent, composition and volume of the eluting solvent and sample volume, were also investigated. Under the optimum conditions, the developed method provided satisfactory limits of detection ranging between 0.07 µg L-1 to 0.12 µg L-1 and the material showed an excellent reusability (> 50 reuses). The method was applied to the extraction and preconcentration of these analytes in water samples. The average recoveries ranged from 79 ± 6 to 104 ± 3 %.


Assuntos
Cromatografia Líquida de Alta Pressão/métodos , Impressão Molecular , Praguicidas/análise , Clorpirifos/análise , Clorpirifos/isolamento & purificação , Diazinon/análise , Diazinon/isolamento & purificação , Água Doce/análise , Limite de Detecção , Praguicidas/isolamento & purificação , Polímeros/química , Extração em Fase Sólida , Espectrofotometria Ultravioleta
19.
J Chromatogr A ; 1626: 461348, 2020 Aug 30.
Artigo em Inglês | MEDLINE | ID: mdl-32797828

RESUMO

Solid-phase extraction (SPE) is a widely-used and very well-established sample preparation technique for liquid samples. An area of on-going focus for innovation in this field concerns the development of new and improved SPE sorbents that can enhance the sensitivity and/or the selectivity of SPE processes. In this context, mixed-mode ion-exchange sorbents have been developed and commercialised, thereby allowing enhanced capacity and selectivity to be offered by one single material. The ion-selectivity of these materials is such that either anion-exchange or cation-exchange is possible, however one limitation to their use is that more than one sorbent type is required to capture both anions and cations. In this paper, we disclose the design, synthesis and exploitation of a novel SPE sorbent based on microporous polymer microspheres with amphoteric character. We show that it is possible to switch the ion-exchange retention mechanism of the sorbent simply by changing the pH of the loading solution; anion-exchange dominates at low pH, cation-exchange dominates at high pH, and both mechanisms can contribute to retention when the polymer-bound amphoteric species, which are based on the α-amino acid sarcosine (N-methylglycine), are in a zwitterionic state. This is an interesting and useful feature, since it allows distinctly different groups of analytes (acids and bases) to be fractionated using one single amphoteric sorbent with dual-functionality. The sarcosine-based sorbent was applied to the SPE of acidic, basic and amphoteric analytes from ultrapure water, river water and effluent wastewater samples. Under optimised conditions (loading 100 mL of sample at pH 6, washing with 1 mL of MeOH and eluting with an acidic or basic additive in MeOH) the recoveries for most of the compounds were from 57% to 87% for river water and from 61% to 88% for effluent wastewater. We anticipate that these results will lay the basis for the development of a new family of multifunctional sorbents, where two or more separation mechanisms can be embedded within one single, bespoke material optimised for application to challenging chemical separations to give significant selectivity advantages over essentially all other state-of-the-art SPE sorbents.


Assuntos
Ácidos/química , Microesferas , Polímeros/química , Extração em Fase Sólida/métodos , Adsorção , Cátions , Concentração de Íons de Hidrogênio , Troca Iônica , Porosidade , Rios/química , Solventes/química , Águas Residuárias/química , Poluentes Químicos da Água/análise
20.
J Chromatogr A ; 1626: 461384, 2020 Aug 30.
Artigo em Inglês | MEDLINE | ID: mdl-32797857

RESUMO

More and more various chemical media are being applied in enantioseparation; among them, ionic liquids (ILs) have attracted the long-term attention in this decade as green designable solvents. This paper provides comprehensive overview for the applications of ILs in chiral extraction, gas chromatography, liquid chromatography, capillary electrophoresis and other techniques for enantioseparation. Additionally, the important resolution mechanisms based on ILs have also been summarized and discussed. This review focuses on the latest development of enantioseparation methods by using ILs in various modes, leading to meaningful and valuable information to related fields and thus promotes further research and application of reported methods.


Assuntos
Cromatografia Gasosa/métodos , Cromatografia Líquida de Alta Pressão/métodos , Eletroforese Capilar/métodos , Líquidos Iônicos/química , Ligantes , Extração Líquido-Líquido , Extração em Fase Sólida , Estereoisomerismo
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