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1.
Anal Chim Acta ; 1307: 342624, 2024 Jun 08.
Artigo em Inglês | MEDLINE | ID: mdl-38719414

RESUMO

BACKGROUND: Pesticides are used in agricultural production for prevent and control crop diseases and pests, but it is easy to cause excessive pesticides residues in agricultural products, polluting the environment and endangering human health. Due to their unmatched and sustainable capabilities, nanoextraction procedures are becoming every day more important in Analytical Chemistry. In particular, nanoconfined liquid phase extraction has shown extraction capabilities toward polar, medium polar, and/or nonpolar substances, which can be easily modulated depending on the nanoconfined solvent used. Furthermore, this "green" technique showed excellent characteristics in terms of recoveries, extraction time (≤1 min), reliability, and versatility. (97) RESULTS: In this work, the advantages of this technique have been coupled with those of filtration membrane extraction, making use of carbon nanofibers (CnFs) growth on carbon microspheres (CµS). This substrate has been deposited on a filter, which combined with gas chromatographic mass spectrometry (GC-MS) analysis successfully employed for the nanoextraction of 30 pesticides (18 organochlorine and 12 pyrethroids) in tea samples. Under the optimized extraction conditions, the linear range with standard solutions was from 1 to 1000 ng mL-1 (R2 ≥ 0.99), the limit of detections in tea samples were in the range 0.56-17.98 µg kg-1. The accuracy of the developed method was evaluated by measuring the extraction recovery of the spiked tea samples, and recoveries between 74.41 % and 115.46 %. (119) SIGNIFICANCE: Considering the versatility of nanoconfined liquid phase extraction and the functionality of the filtration membrane extraction procedure, this new extraction method can be considered a powerful candidate for automatized high-throughput analyses of real samples. (34).


Assuntos
Filtração , Hidrocarbonetos Clorados , Extração Líquido-Líquido , Praguicidas , Piretrinas , Chá , Chá/química , Piretrinas/análise , Piretrinas/isolamento & purificação , Hidrocarbonetos Clorados/análise , Hidrocarbonetos Clorados/isolamento & purificação , Extração Líquido-Líquido/métodos , Filtração/métodos , Praguicidas/análise , Praguicidas/isolamento & purificação , Cromatografia Gasosa-Espectrometria de Massas/métodos , Membranas Artificiais
2.
Anal Chim Acta ; 1295: 342288, 2024 Mar 22.
Artigo em Inglês | MEDLINE | ID: mdl-38355222

RESUMO

BACKGROUND: Vitamins are micronutrients that are required for normal growth and development of living organisms. However, due to their various chemical properties (e.g., acid-base behavior, the presence of numerous forms) and fluctuating concentration levels within complex matrices, simultaneous analysis of multi-class vitamins, including their active forms, is a challenging task. The growing nutrient shortage in foods is concerning for food consumers, manufacturers, and quality control organizations. Hence, a simple, fast, and greener approach that can simultaneously analyze multi-class vitamins is required to aid food testing and clinical laboratories in evaluating vitamin content more rapidly and accurately. RESULTS: A green and rapid analytical method based on online two-dimensional microscale carbon fiber/activated carbon fiber fractionation-mass spectrometry (2DµCFs-MS) was developed and validated for simultaneous determination of vitamins (water- and fat-soluble vitamins and some analogs) in food supplements and fortified energy drinks. Vitamins have been successfully separated into three different fractions using the minimum toxic solvent (only 0.7 mL of organic solvent) in a single run within 6 min. The limit of detection (LOD) ranges from 0.1 to 10.4 ng/mL, and the limit of quantification (LOQ) ranges from 0.39 to 34.5 ng/mL. The method also showed adequate repeatability and intermediate precision, with RSD<10 % and R2 > 0.99 for most vitamins. The analytical method was evaluated in terms of greenness, with an analytical greenness (AGREE) score of 0.68. SIGNIFICANCE: The 2DµCFs-MS system was developed to separate and detect multi-class vitamins simultaneously, which can be used as a beneficial tool to investigate vitamin content for food labeling and determining the vitamins in biological fluids and other complex samples. The developed method can tackle the challenge of simultaneous and fast routine analysis of multi-class vitamins.


Assuntos
Vitaminas , Água , Água/química , Vitaminas/análise , Vitaminas/química , Suplementos Nutricionais/análise , Nutrientes , Solventes/análise
3.
Anal Sci ; 39(7): 1151-1161, 2023 Jul.
Artigo em Inglês | MEDLINE | ID: mdl-36947336

RESUMO

This work first proposed a novel green and efficient method based on Quick, Easy, Cheap, Efficient, Rugged, and Safe pretreatment (QuEChERS) combined with switchable hydrophilic solvent homogeneous liquid-liquid microextraction (SHS-HLLME) for trace determination of triazole fungicides (TFs) in agricultural products such as vegetables and fruits by gas chromatography-mass spectrometry (GC-MS). N,N-Dimethyl benzylamine was used for the synthesis of SHS. Box-Behnken design was applied for the optimization of extraction conditions and a mathematical model was obtained. Ultimately, 0.50 mL SHS, 1.0 mL 10 mol L-1 sodium hydroxide, and 45 s ultrasonic time were determined as optimal conditions for the SHS-HLLME method. The limit of detection and limit of quantification determined using the optimal method (SHS-HLLME/GC-MS) were 0.13-0.27 ng mL-1 and 0.43-0.90 ng mL-1, respectively. In addition, the SHS-HLLME method under optimal conditions was combined with the traditional QuEChERS method to realize the advancement of the SHS-HLLME method from simple to complex matrix analysis, and the QuEChERS-SHS-HLLME method was successfully applied to the analysis of TFs in cucumbers, tomatoes, watermelon and grapes in agricultural products. Matrix-matched calibration standards were used to improve the accuracy of TFs in spiked cucumber samples to obtain recovery results close to 100%. It was shown that the new method is green and rapid, enabling fast and inexpensive sample pretreatment with up to 100-fold enrichment factor and low detection limit compared with the original QuEChERS method.


Assuntos
Fungicidas Industriais , Microextração em Fase Líquida , Resíduos de Praguicidas , Praguicidas , Cromatografia Gasosa-Espectrometria de Massas/métodos , Praguicidas/análise , Solventes/química , Fungicidas Industriais/análise , Microextração em Fase Líquida/métodos , Resíduos de Praguicidas/análise
4.
Anal Chem ; 94(33): 11500-11507, 2022 08 23.
Artigo em Inglês | MEDLINE | ID: mdl-35943850

RESUMO

The development of new technologies for the separation, selection, and isolation of microparticles such as rare target cells, circulating tumor cells, cancer stem cells, and immune cells has become increasingly important in the last few years. Microparticle separation technologies are usually applied to the analysis of disease-associated cells, but these procedures often face a cell separation problem that is often insufficient for single specific cell analyses. To overcome these limitations, a highly accurate size-based microparticle separation technique, herein called "rotating magnetic chromatography", is proposed in this work. Magnetic nanoparticles, placed in a microfluidic separation channel, are forced to move in well-defined trajectories by an external magnetic field, colliding with microparticles that are in this way separated on the basis of their dimensions with high accuracy and reproducibility. The method was optimized by using fluorescein isothiocyanate-modified polystyrene particles (chosen as a reference standard) and then applied to the analysis of cancer cells like Hep-3B and SK-Hep-1, allowing their fast and high-resolution chromatographic separation as a function of their dimensions. Due to its unmatched sub-micrometer cell separation capabilities, RMC can be considered a break-through technique that can unlock new perspectives in different scientific fields, that is, in medical oncology.


Assuntos
Cromatografia , Magnetismo , Separação Celular , Fenômenos Magnéticos , Poliestirenos/química , Reprodutibilidade dos Testes
5.
J Chromatogr A ; 1675: 463178, 2022 Jul 19.
Artigo em Inglês | MEDLINE | ID: mdl-35660318

RESUMO

A low matrix effect pretreatment method by Gas-liquid microextraction technique (GLME) combined with ultrasound assisted extraction (UAE-GLME) has been developed for fast analysis of 41 multi-class pesticides in different crop samples. Extraction and cleanup procedures were completed within 20 min, and the impact of matrix effects in potato, lentil, corn and soybean matrices were systematically evaluated. As high as 97.6% pesticides treated by UAE-GLME experienced low matrix effect, and up to 99% pesticides except parathion-methyl in lentil samples were categorized as medium matrix effect. Good trueness (recoveries of 61.3-115.8%) and precision (RSD≤20%) were demonstrated by the UAE-GLME method, with MLOQs ranged from 0.005 to 0.02 mg kg-1. This method detected 2-phenylphenol, pyrimethanil, triadimefon and tebuconazole in the range of 0.008-0.012 mg kg-1 in real food samples. The multiresidue analysis feature of GLME has been validated, which displays further potential for high-throughput determination of organic pollutants in foods with distinctive properties.


Assuntos
Poluentes Ambientais , Resíduos de Praguicidas , Praguicidas , Produtos Agrícolas/química , Poluentes Ambientais/análise , Cromatografia Gasosa-Espectrometria de Massas/métodos , Resíduos de Praguicidas/análise , Praguicidas/análise , Extração em Fase Sólida/métodos
6.
Anal Methods ; 14(12): 1187-1193, 2022 03 24.
Artigo em Inglês | MEDLINE | ID: mdl-35230360

RESUMO

A new method was developed for the determination of three triazole fungicides in environmental water samples by gas chromatography-mass spectrometry (GC-MS) based on ultrasonic assisted switchable hydrophilic solvent homogeneous liquid-liquid microextraction. As a switchable hydrophilic solvent, N,N-dimethylcyclohexylamine (DMCHA) does not require a dispersant or centrifugation. Ultrasound assistance is helpful to speed up the extraction of target compounds and can reduce the pretreatment time. The entire pretreatment process of this method only takes 5 minutes. Using the Box-Behnken design as the means of optimization, optimal extraction conditions were obtained through a mathematical model. Good linearity was obtained in the range of 5-500 µg L-1, and the correlation coefficient of target compounds was greater than 0.999. The matrix spiked recoveries were between 81.3% and 111.1% and the detection limit was between 0.46 and 0.99 µg L-1. Intraday relative standard deviation (n = 3) was 13.0-13.9% at 100 µg L-1. Finally, it was concluded that the method is a rapid, efficient and simple method for the analysis of triazole fungicides in water.


Assuntos
Fungicidas Industriais , Microextração em Fase Líquida , Fungicidas Industriais/análise , Cromatografia Gasosa-Espectrometria de Massas , Microextração em Fase Líquida/métodos , Solventes/química , Triazóis/análise , Água/análise
7.
Environ Sci Pollut Res Int ; 29(5): 7079-7088, 2022 Jan.
Artigo em Inglês | MEDLINE | ID: mdl-34467484

RESUMO

Due to their wide distribution and availability, plant leaves can be considered interesting candidates as biomonitoring substrates for the evaluation of atmospheric pollution. In addition, some species can also retain historical information, for example, related to environmental pollution, due to their leaf class age. In this study, the content of polycyclic aromatic hydrocarbons (PAHs) in Abies holophylla and Pinus tabuliformis needle samples in the function of their class age has been investigated to obtain information regarding the degradation constant for each PAH under investigation (α values ranging from 0.173 to 1.870) and to evaluate the possibility to correlate the presence of PAHs in needles with some important pollution environmental factors. Considering air pollutant variables registered in Jilin Province, interesting correlations (at 95% confidence level) have been found between coal consumption per year and anthracene contents in needles, while fluorene, phenanthrene, and anthracene results correlated with coal consumption. Furthermore, it has been demonstrated that the total PAH concentration in needles, for both species, increased with their age (from 804 to 3604 ng g-1 dry weight), showing a general tendency to accumulate these substances through years. PAH degradation rates increased instead with molecular complexity. This study could be considered a first trial to obtain historical environmental information by pine needles biomonitoring.


Assuntos
Abies , Pinus , Hidrocarbonetos Policíclicos Aromáticos , China , Monitoramento Ambiental , Folhas de Planta/química , Hidrocarbonetos Policíclicos Aromáticos/análise
8.
Food Chem ; 367: 130774, 2022 Jan 15.
Artigo em Inglês | MEDLINE | ID: mdl-34390913

RESUMO

Gas-liquid microextraction technique (GLME) has been integrated with dispersive solid phase extraction to establish a one-step sample pretreatment approach for rapid analysis of multi-class pesticides in different plant-derived foods. A 50 µL of organic solvent plus 40 mg of PSA were required throughout the 5-minute pretreatment procedure. Good trueness (recoveries of 67.2 - 105.4%) and precision (RSD ≤ 18.9%) were demonstrated by the one-step GLME method, with MLOQs ranged from 0.001 to 0.011 mg kg-1. As high as 93.6% pesticides experienced low matrix effect through this method, and the overall matrix effects (ME%) were generally better or comparable to QuEChERS. This method successfully quantified 2-phenylphenol, quintozene, bifenthrin and permethrin in the range of 0.001 - 0.008 mg kg-1 in real food samples. The multiresidue analysis feature of GLME has been validated, which displays further potential for on-site determination of organic pollutants in order to safeguard food safety and human health.


Assuntos
Resíduos de Praguicidas , Praguicidas , Humanos , Resíduos de Praguicidas/análise , Praguicidas/análise , Extração em Fase Sólida , Solventes
9.
Technol Cancer Res Treat ; 20: 15330338211062325, 2021.
Artigo em Inglês | MEDLINE | ID: mdl-34825851

RESUMO

Objective: Conventional chemotherapy remains the mainstay treatment for many breast cancer patients, but its effectiveness is limited by toxic side effects. Incorporating drugs such as docetaxel into nanoparticle medicines can reduce toxicity but further improvements are required. To facilitate more active tumor targeting, we prepared transferrin-docetaxel-loaded pegylated-albumin nanoparticles (Tf-PEG-DANPS). Methods: The growth inhibitory effects and the ability of unmodified DANPS or PEG-DANPS to induce apoptosis in 4T1 mouse mammary cancers were compared to Tf-PEG-DANPS treatment using 3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide (MTT) and flow cytometry. These experiments were extended in vivo to the intravenous treatment of 4T1 tumors where PEG-DANPS was compared to Tf-PEG-DANPS alone or Tf-PEG-DANPS combined with ultrasound (US + Tf-PEG-DANPS). Histological assessments using hematoxylin and eosin (HE) sections were performed to examine antitumor activity, metastasis to lung and liver, and body weight measurements taken as an indicator of toxicity. Results: MTT experiments show that, in the normal and low concentration interval, the inhibition ability of the Tf-PEG-DANPS is higher than that of other drug-giving groups, and the flow cytometry show that the proportion of induced apoptosis in each given group is 2.88%, 42.95%, 48.23%, and 57.89%, indicating that the Tf-PEG-DANPS group has more significant ability to induce apoptosis than other drug-giving groups. From the pathological HE staining and semiquantitative analysis, US+Tf-PEG-DANPS can effectively inhibit the growth of breast cancer transplanted tumors and suppress metastases, it also has smaller toxic side effects on mice. Conclusion: The antitumor effect of US+Tf-PEG-DANPS represents an effective combination that exhibits increased antitumor activity and metastasis reduction with an improved side-effect profile.


Assuntos
Nanopartículas , Transferrina/administração & dosagem , Terapia por Ultrassom , Ondas Ultrassônicas , Animais , Apoptose/efeitos dos fármacos , Apoptose/efeitos da radiação , Linhagem Celular Tumoral , Células Cultivadas , Modelos Animais de Doenças , Composição de Medicamentos , Neoplasias Hepáticas/diagnóstico , Neoplasias Hepáticas/secundário , Neoplasias Pulmonares/diagnóstico , Neoplasias Pulmonares/secundário , Camundongos , Nanopartículas/química , Nanopartículas/ultraestrutura , Nanomedicina Teranóstica , Terapia por Ultrassom/métodos
10.
Anal Chim Acta ; 1182: 338957, 2021 Oct 16.
Artigo em Inglês | MEDLINE | ID: mdl-34602203

RESUMO

A reciprocating magnetic-field-assisted on-line solid-phase extraction (RMF-SPE) method coupled with liquid chromatography-tandem mass spectrometry (LC-MS/MS) has been developed for continuous enrichment of trace chemicals in water samples. Under the assist of the reciprocating magnetic field, carboxyl-modified magnetic nanoparticles (CMNPs) were applied to prepare microcolumn with even dispersion by periodical motion, instead of traditional compaction as extraction sorbents. When water sample passed through the extraction region, dynamic sorbents generates an advantage of countless contacts between sorbents and targets without blocking for high efficient extraction. In this study, the on-line RMF-SPE method was established and evaluated by determination of tetracyclines (TCs) from water samples as analysis models, including oxytetracycline, tetracycline, demeclocycline, metacycline, chlortetracycline, and doxycycline. Experimental conditions have been investigated such as flow rate, reciprocating speed, elution time, and so on. The method showed high relative recovery (95.4-111.1%) and good repeatability with RSD from 2.9 to 11.8% for the 200 mL water sample. The linearity range, limits of detection (LODs), and limits of quantification (LOQs) were 0.5-200 µg L-1 (chlortetracycline) and 0.1-200 µg L-1 (other TCs), 12.0-74.1 ng L-1, and 40.1-247 ng L-1, respectively. More importantly, the high enrichment factors in a range of 204 (chlortetracycline) to 276 (demeclocycline) indicate that a small amount of dynamic sorbents (only 10 mg) give full play to extraction attributing to the reciprocating movement, especially for trace analysis and continuous extraction, which is significant for water samples from sea, river and domestic waste.


Assuntos
Tetraciclinas , Água , Cromatografia Líquida , Campos Magnéticos , Extração em Fase Sólida , Espectrometria de Massas em Tandem
11.
Plant Sci ; 298: 110576, 2020 Sep.
Artigo em Inglês | MEDLINE | ID: mdl-32771138

RESUMO

A trapping-based gas liquid microextraction (GLME) method coupled with gas chromatography-mass spectrometry (GC-MS) was utilized to qualitatively and quantitatively characterize semiochemicals in plants. The main GLME extraction efficiency associated parameters (heating temperature and extraction time) were optimized. The results obtained from GLME process were compared with those of steam distillation and ultrasonic extraction, and the recovery, peak number and reproducibility were evaluated by using Thuja koraiensis Nakai as a representative plant. Furthermore, the quantitative performances of the GLME in terms of sample amount, recoveries of spiked standards and correlation were systematically evaluated using standard addition method, which gave a good quantitative ability for all the compounds with squares of correlation coefficient (r2) of higher than 0.99. Finally, the contents of α-pinene, camphene, linalool, α-terpinenol, ß-caryophyllene, α-caryophyllene, and totarol in Thuja koraiensis Nakai samples were quantified, and their concentrations (SD, n = 3) were; 0.65 (0.06), 0.62 (0.05), 4.12 (0.15), 0.99 (0.08), 1.11 (0.07), 0.63 (0.04), and 21.91 (0.25) µg g-1, respectively. It was demonstrated that GLME is a powerful sample preparation technique for quantitative and qualitative analysis of plant semiochemicals.


Assuntos
Cromatografia Gasosa-Espectrometria de Massas/métodos , Microextração em Fase Líquida/métodos , Feromônios/análise , Thuja/química , Cromatografia Gasosa-Espectrometria de Massas/instrumentação , Microextração em Fase Líquida/instrumentação , Feromônios/química
12.
J Pharm Biomed Anal ; 187: 113339, 2020 Aug 05.
Artigo em Inglês | MEDLINE | ID: mdl-32480199

RESUMO

In this work, a new an innovative micro liquid extraction technique named "gas purge micro solvent extraction" (GP-MSE) have been tested, hyphenated with gas chromatography-mass spectrometry (GC-MS), to evaluate its capability to extract volatile fractions from vegetal samples respect to classical steam distillation extraction procedure, by comparing essential oil fingerprints from three different Atractylodes species. GP-MSE showed higher extraction capabilities and sensitivities (in particular for semi-volatile components), obtaining more structured essential oil fingerprints with high reliabilities (relative standard deviation of the peak areas between 0.34% and 5.83%), requiring at the same time smaller sample amounts and reduced extraction times. Essential oil profile data were also submitted to principal component analysis and included cosine angle in order to highlight differences among the Atractylodes species under investigation. GP-MSE can be considered an alternative, simple, fast, sensitive and environmentally friendly extraction method, with high extraction efficiencies and reproducibility toward both volatile and semi-volatile compounds.


Assuntos
Atractylodes/química , Cromatografia Gasosa-Espectrometria de Massas/métodos , Óleos Voláteis/química , Gases , Microextração em Fase Líquida , Óleos Voláteis/análise , Óleos Voláteis/isolamento & purificação , Análise de Componente Principal , Reprodutibilidade dos Testes , Solventes/química , Fatores de Tempo
13.
Analyst ; 145(9): 3266-3273, 2020 May 07.
Artigo em Inglês | MEDLINE | ID: mdl-32236242

RESUMO

This study developed a traceless clean-up method by combining solid phase extraction (SPE) with gas purge-microsyringe extraction (GP-MSE) to purify sample extracts for the determination of polycyclic aromatic hydrocarbons (PAHs) in plant leaves. SPE exhibited good purification performance for the removal of polar lipids, while the GP-MSE technique effectively eliminated less-volatile lipids hence realizing zero damage to the instrument, and significantly improved the peak tailings. After ultrasonic extraction, the combined two-step clean-up procedure successfully removed over 99% of lipids from nineteen types of tree leaves, and PAHs in tree leaves were determined by GC-MS. The relative standard deviations (RSDs) for intra-day (n = 3) and inter-day (n = 3) analyses of PAHs in spiked willow samples were in the range of 0.8%-12.1% and 4.7%-15.3%, respectively. The recoveries of PAHs from spiked willow extracts ranged from 74 to 90%, with an average of 86%. The method detection limit (MDL) of PAHs in tree leaves ranged from 0.1 to 4.9 ng g-1 dry weight. In conclusion, the clean-up method in this study realized the analysis of PAHs in plant leaves with high accuracy, sensitivity and reproducibility. Most importantly, the two-step purification method significantly minimizes damage to the GC-MS system particularly to the column and ion source, which is beneficial to ensure continuous analysis of a large number of samples with good performance.


Assuntos
Cromatografia Gasosa-Espectrometria de Massas/métodos , Folhas de Planta/química , Hidrocarbonetos Policíclicos Aromáticos/análise , Limite de Detecção , Lipídeos/isolamento & purificação , Pinus/química , Pinus/metabolismo , Folhas de Planta/metabolismo , Hidrocarbonetos Policíclicos Aromáticos/isolamento & purificação , Quercus/química , Quercus/metabolismo , Reprodutibilidade dos Testes , Extração em Fase Sólida/métodos , Sonicação
14.
J Chromatogr A ; 1606: 360245, 2019 Nov 22.
Artigo em Inglês | MEDLINE | ID: mdl-31122728

RESUMO

In this review, recent advances in the analysis of water-soluble vitamins (WSVs) have been reported considering the advantages and disadvantages of various extraction, separation and detection techniques, commonly used for their quantification. Acid hydrolysis, enzyme treatment, SPE based methods and some other extraction methods have been discussed. Particular attention has been devoted to the analytical techniques based on liquid chromatography and electrophoresis. Furthermore, suitability and selectivity of hydrophilic interaction liquid chromatography (HILIC) for WSVs has been discussed in detail. Problems related to these techniques and their possible solutions have also been considered. Special focus has been given to the applications of liquid chromatography (since 2014-2019) for the simultaneous analysis of WSVs and their homologous in complex food samples.


Assuntos
Técnicas de Química Analítica/métodos , Técnicas de Química Analítica/tendências , Vitaminas/análise , Água/química , Eletroforese Capilar , Interações Hidrofóbicas e Hidrofílicas , Solubilidade , Vitaminas/química
15.
Analyst ; 143(19): 4575-4584, 2018 Sep 24.
Artigo em Inglês | MEDLINE | ID: mdl-30113043

RESUMO

In order to extract trace organic compounds (TrOCs) from large volumes of water (over 10 L), an ultrasound-assisted liquid-liquid spray extraction (UA-LLSE) technique is proposed. The UA-LLSE integrates liquid-liquid extraction, spray atomisation and ultrasonication in a single step. Under an acoustic field, a water sample is continuously spray injected into an extracting organic solvent to generate numerous water microdroplets in the organic phase. As a result, the extraction time and efficiency are significantly improved through increasing the interactive surface area, collision probability and mass transfer between two liquid phases. Other major parameters affecting the extraction efficiency such as nozzle type, spray angle, flow rate, nozzle position, ultrasonication energy, and extraction cycle were optimised. This newly developed technique has been applied to determine the trace organic compounds in real-world environmental matrices, and the results were compared with the results of the conventional liquid-liquid extraction method. For the analysis of high-volume water samples, UA-LLSE is a simple, inexpensive, time-saving (20 min for 10 L of water sample) and environmentally friendly method (reduction in solvent usage), with high extraction efficiency (over 90% average recoveries) and excellent precision (lower than 7% relative standard deviation, RSD). Most importantly, it is an ideal on-site pre-treatment technique for the in situ extraction of trace organic compounds in high-volume water matrices.

16.
Sci Total Environ ; 645: 220-228, 2018 Dec 15.
Artigo em Inglês | MEDLINE | ID: mdl-30029105

RESUMO

To date, information is scarce on the accumulation and potential risks of persistent chlorinated and fluorinated contaminants in birds. In this study, organohalogen contaminants (OHCs), such as polychlorinated biphenyls (PCBs), organochlorine pesticides (OCPs), and perfluoroalkyl substances (PFASs), were measured in the liver tissues of 10 bird species (n = 69) from Korea. Among the OHCs, PFASs showed the highest concentration, ranging from 5.40 to 11,300 (median: 294) ng/g wet weight. The median concentrations of OCPs and PCBs in all the bird samples were 147 and 81.9 ng/g lipid weight, respectively. The maximum concentration of perfluorooctane sulfonate (PFOS) observed in our bird samples was highest reported so far. Concentrations of OHCs in predatory birds were significantly greater than those measured in non-predatory birds, indicating the importance of diet and trophic position for bioaccumulation of these contaminants. In addition, different accumulation patterns of OHCs were found between predatory and non-predatory birds. Significant correlations were found between organochlorine concentrations and stable nitrogen isotope ratio (δ15N) measurements, whereas no correlation was found between PFASs and δ15N. Although the concentrations of PCBs and DDTs in birds were lower than the threshold levels, 25% and 49% of birds exceeded the toxicity reference value and predicted no effect concentration for PFOS, respectively, implying potential health risks to Korean birds.


Assuntos
Monitoramento Ambiental , Poluentes Ambientais/metabolismo , Hidrocarbonetos Clorados/metabolismo , Animais , Aves , Praguicidas , Bifenilos Policlorados , República da Coreia
17.
Se Pu ; 36(2): 173-178, 2018 Feb 08.
Artigo em Chinês | MEDLINE | ID: mdl-29582604

RESUMO

In order to develop a fast investigation method for phthalate esters (PAEs) from vegetable oils, a gas-liquid micro-extraction (GLME) technique that combined with GC-MS was established. A vegetable oil sample (0.1 g) was directly added into the GLME device. The integrated process of extraction, clean-up, and concentration of PAEs was completed within 5 min. Internal standard method was applied to ensure the accuracy of the results. Soybean oil, blend oil, olive oil, and sesame oil were spiked with 200 µg/kg of a mixed 15 PAEs standard, and the ranges of the recoveries and RSDs were between 60.0% to 112.3% and 0.9% to 28.4%, respectively. Compared with some traditional sample pretreatment methods such as liquid-liquid extraction, liquid-liquid micro-extraction, gel permeation chromatography, this method is simple and fast, with high accuracy, good repeatability and low matrix effect. This study verified the suitability of the GLME method for field detection of food products in food safety sector and exhibits great significance for the completion of food safety system in China.


Assuntos
Ésteres/isolamento & purificação , Ácidos Ftálicos/isolamento & purificação , Óleos de Plantas/análise , Cromatografia em Gel , Cromatografia Gasosa-Espectrometria de Massas , Extração Líquido-Líquido
18.
Environ Pollut ; 219: 191-200, 2016 Dec.
Artigo em Inglês | MEDLINE | ID: mdl-27814535

RESUMO

Few studies have been conducted on the alternatives to legacy flame retardants in avian species worldwide. In this study, polybrominated diphenyl ethers (PBDEs) and alternative flame retardants such as novel brominated flame retardants (NBFRs) and dechlorane plus (DP) were determined in livers of 10 species of birds from Korea to elucidate species-specific accumulation, biological factors that affect accumulation, and bioaccumulation potentials of these contaminants. Among the emerging alternative flame retardants, the highest occurrence was found for bis(2-ethylhexyl)-3,4,5,6-tetrabromo-phthalate (BEHTBP), syn-DP, anti-DP, and decabromodiphenyl ethane (DBDPE). PBDE concentrations (median: 17.1 ng/g lipid wt) measured in our study were within the ranges reported in previous studies, while the concentrations of BEHTBP, BTBPE and DP were greater than those reported earlier. Residential predatory birds showed significantly greater concentrations of PBDEs and NBFRs than migratory predators and passerine birds. The concentrations of PBDEs, BEHTBP, and DP in residential predatory birds were significantly correlated with increasing stable nitrogen isotope ratio (δ15N), which indicated biomagnification potentials of these contaminants. Our results suggest that the concentrations and accumulation patterns of PBDEs, NBFRs, and DP depend on the feeding habits and migration patterns of avian species. This is the first report on the accumulation of emerging alternatives to PBDEs in birds from Korea.


Assuntos
Aves/metabolismo , Poluentes Ambientais/análise , Poluentes Ambientais/metabolismo , Retardadores de Chama/análise , Retardadores de Chama/metabolismo , Fígado/metabolismo , Animais , Bromobenzenos/análise , Bromobenzenos/metabolismo , Dieta/veterinária , Ecossistema , Monitoramento Ambiental , Poluição Ambiental/análise , Hidrocarbonetos Clorados/análise , Hidrocarbonetos Clorados/metabolismo , Fígado/química , Ácidos Ftálicos/análise , Ácidos Ftálicos/metabolismo , Compostos Policíclicos/análise , Compostos Policíclicos/metabolismo , República da Coreia , Especificidade da Espécie
19.
Chemosphere ; 153: 426-35, 2016 Jun.
Artigo em Inglês | MEDLINE | ID: mdl-27031806

RESUMO

Legacy and new persistent organic pollutants (POPs) and polycyclic aromatic hydrocarbons (PAHs) were measured in sediments near a wastewater treatment plant (WWTP) outfall in a semi-enclosed bay, to investigate the current contamination and temporal changes in these contaminants associated with regulation activities in Korea. The concentrations of most of the POPs showed clear decreasing trends with an increase in the distance from the WWTP outfall, indicating that the WWTP discharges greatly contributed to the sediment contamination by POPs. Highly significant correlations were found for most of the POPs, indicating a common source for sediment contamination. Significant declines were found in the concentrations of polychlorinated dibenzo-p-dioxins and dibenzofurans (PCDD/Fs), dioxin-like polychlorinated biphenyls (DL-PCBs), polybrominated diphenyl ethers (PBDEs), and PAHs in the sediments collected between 2005 and 2013. This result suggested that legislative actions (regulation of the PCDD/Fs in flue gas, total pollution load management, and whole effluent toxicity for WWTP discharges) and change of fuels, were likely to be effective at reducing the POP and PAH levels in sediments during the past several years. The different compositional profiles of the PCDD/Fs and PAHs between 2005 and 2013 implied changes in and/or additional sources of these contaminants. Despite a decline in the PCDD/Fs over time, the present levels of PCDD/Fs in the sediment exceeded some of the sediment quality guidelines suggested by the National Oceanic and Atmospheric Administration.


Assuntos
Recuperação e Remediação Ambiental/legislação & jurisprudência , Sedimentos Geológicos/análise , Eliminação de Resíduos Líquidos , Poluição Química da Água/prevenção & controle , Monitoramento Ambiental , República da Coreia , Águas Residuárias/análise
20.
Zhong Xi Yi Jie He Xue Bao ; 1(2): 125-7, 2003 Jul.
Artigo em Chinês | MEDLINE | ID: mdl-15339585

RESUMO

OBJECTIVE: To study the effect of Boschniakia rossica extract on free radicals in the brain of D-galactose induced senile rats. METHODS: Sixty Wistar rats were randomly divided into normal group, model group (48 mg.kg(-1).d(-1) D-galactose, SC), Boschniakia rossica group (100, 150, 200 mg/kg ig and 48 mg.kg(-1).d(-1) D-galactose, SC). After 40 days, the activities of SOD, MAO and the content of MDA were measured with colorimetric method, and the histological changes were synchronously observed by electronic microscope. RESULTS: Boschniakia rossica extract significantly increased the SOD activity, decreased the MDA content, and inhibited the MAO activity in the brain tissue. It was observed under microscope that Boschniakia rossica extract could retrieve the degeneration of mitochondrion. CONCLUSION: Boschniakia rossica extract can clear the free radicals for D-galactose induced senile rats.


Assuntos
Envelhecimento/efeitos dos fármacos , Encéfalo/efeitos dos fármacos , Medicamentos de Ervas Chinesas/farmacologia , Radicais Livres/metabolismo , Orobanchaceae , Envelhecimento/metabolismo , Animais , Encéfalo/metabolismo , Feminino , Galactose/farmacologia , Masculino , Monoaminoxidase/efeitos dos fármacos , Monoaminoxidase/metabolismo , Extratos Vegetais/farmacologia , Ratos , Ratos Wistar , Superóxido Dismutase/efeitos dos fármacos , Superóxido Dismutase/metabolismo
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