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1.
J Sep Sci ; 45(1): 185-209, 2022 Jan.
Artigo em Inglês | MEDLINE | ID: mdl-34472701

RESUMO

Liquid-liquid extraction is a widely used technique of sample preparation in biomedical analysis. In spite of the high pre-concentration capacities of liquid-liquid extraction, it suffers from a number of limitations including time and effort consumption, large organic solvent utilization, and poor performance in highly polar analytes. Homogeneous liquid-liquid extraction is an alternative sample preparation technique that overcomes some drawbacks of conventional liquid-liquid extraction, and allows employing greener organic solvents in sample treatment. In homogeneous liquid-liquid extraction, a homogeneous phase is formed between the aqueous sample and the water-miscible extractant, followed by chemically or physically induced phase separation. To form the homogeneous phase, aqueous samples are mixed with water-miscible organic solvents, water-immiscible solvents/cosolvents, surfactants, or smart polymers. Then, phase separation is induced chemically (adding salt, sugar, or buffer) or physically (changing temperature or pH). This mode is rapid, sustainable, and cost-effective in comparison with other sample preparation techniques. Moreover, homogeneous liquid-liquid extraction is more suitable for the extraction of delicate macromolecules such as enzymes, hormones, and proteins and it is more compatible with liquid chromatography with tandem mass spectrometry, which is a vital technique in metabolomics and proteomics. In this review, the principle, types, applications, automation, and technical aspects of homogeneous liquid-liquid extraction are discussed.


Assuntos
Hormônios/isolamento & purificação , Extração Líquido-Líquido/métodos , Proteínas/isolamento & purificação , Animais , Cromatografia Líquida de Alta Pressão , Hormônios/química , Humanos , Extração Líquido-Líquido/instrumentação , Proteínas/química , Solventes/química , Espectrometria de Massas em Tandem
2.
J Sep Sci ; 43(15): 3146-3163, 2020 Aug.
Artigo em Inglês | MEDLINE | ID: mdl-32573988

RESUMO

The structural information and spatial distribution of molecules in biological tissues are closely related to the potential molecular mechanisms of disease origin, transfer, and classification. Ambient ionization mass spectrometry imaging is an effective tool that provides molecular images while describing in situ information of biomolecules in complex samples, in which ionization occurs at atmospheric pressure with the samples being analyzed in the native state. Ambient ionization mass spectrometry imaging can directly analyze tissue samples at a fairly high resolution to obtain molecules in situ information on the tissue surface to identify pathological features associated with a disease, resulting in the wide applications in pharmacy, food science, botanical research, and especially clinical research. Herein, novel ambient ionization techniques, such as techniques based on spray and solid-liquid extraction, techniques based on plasma desorption, techniques based on laser desorption ablation, and techniques based on acoustic desorption were introduced, and the data processing of ambient ionization mass spectrometry imaging was briefly reviewed. Besides, we also highlight recent applications of this imaging technology in clinical researches and discuss the challenges in this imaging technology and the perspectives on the future of the clinical research.


Assuntos
Pesquisa Biomédica , Doença , Projetos de Pesquisa , Pressão Atmosférica , Testes Diagnósticos de Rotina/instrumentação , Humanos , Extração Líquido-Líquido/instrumentação , Prognóstico , Extração em Fase Sólida/instrumentação , Espectrometria de Massas por Ionização e Dessorção a Laser Assistida por Matriz/instrumentação
3.
Int J Mol Sci ; 21(18)2020 Sep 18.
Artigo em Inglês | MEDLINE | ID: mdl-32962106

RESUMO

This study investigates the separation of two heavy metals, Cd(II) and Cu(II), from the mixed synthetic feed using a liquid-liquid extraction. The current study uses tri-octyl methylammonium chloride (Aliquat 336) as the extractant (with tributyl phosphate (TBP) as a phase modifier), diluted in toluene, in order to investigate the selective extraction of Cd(II) over Cu(II) ions. We investigate the use of ethylenediaminetetraacetic acid (EDTA) as a masking agent for Cu(II), when added in aqueous feed, for the selective extraction of Cd(II). Five factors that influence the selective extraction of Cd(II) over Cu(II) (the equilibrium pH (pHeq), Aliquat 336 concentration (Aliquat 336), TBP concentration (TBP), EDTA concentration (EDTA), and organic to aqueous ratio (O:A)) were analyzed. Results from a 25-1 fractional factorial design show that Aliquat 336 significantly influenced Cd(II) extraction, whereas EDTA was statistically significant for the antagonistic effect on the E% of Cu(II) in the same system. Moreover, results from optimization experiment showed that the optimum conditions are Aliquat 336 concentration of 99.64 mM and EDTA concentration of 48.86 mM-where 95.89% of Cd(II) was extracted with the least extracted Cu(II) of 0.59%. A second-order model was fitted for optimization of Cd(II) extraction with a R2 value of 0.998, and ANOVA results revealed that the model adequately fitted the data at a 5% significance level. Interaction between Aliquat 336 and Cd(II) has been proven via FTIR qualitative analysis, whereas the addition of TBP does not affect the extraction mechanism.


Assuntos
Cádmio/análise , Cádmio/isolamento & purificação , Cobre/análise , Cobre/isolamento & purificação , Extração Líquido-Líquido/métodos , Ácido Edético/química , Concentração de Íons de Hidrogênio , Líquidos Iônicos/química , Extração Líquido-Líquido/instrumentação , Organofosfatos/química , Compostos de Amônio Quaternário/química , Análise de Regressão , Solventes/química , Espectroscopia de Infravermelho com Transformada de Fourier , Tolueno/química
4.
J Sep Sci ; 42(9): 1768-1776, 2019 May.
Artigo em Inglês | MEDLINE | ID: mdl-30809926

RESUMO

A homogeneous liquid-liquid extraction performed in narrow tube coupled to in-syringe-dispersive liquid-liquid microextraction based on deep eutectic solvent has been developed for the extraction of six herbicides from tea samples. In this method, sodium chloride as a separation agent is filled into the narrow tube and the tea sample is placed on top of the salt. Then a mixture of deionized water and deep eutectic solvent (water miscible) is passed through the tube. In this procedure, the deep eutectic solvent is realized as tiny droplets in contact with salt. By passing the droplets from the tea layer placed on the salt layer, the analytes are extracted into them. After collecting the solvent as separated layer, it is mixed with another deep eutectic solvent (choline chloride/butyric acid) and the mixture is dispersed into deionized water placed in a syringe. After adding acetonitrile to break up the cloudy state, the collected organic phase is injected into gas chromatography-mass spectrometry. Under optimal conditions, limits of detection and quantification in the ranges of 2.6-8.4 and 9.7-29 ng/kg, respectively, were obtained. The extraction recoveries and enrichment factors in the ranges of 70-89% and 350-445 were obtained, respectively.


Assuntos
Herbicidas/isolamento & purificação , Microextração em Fase Líquida/métodos , Extração Líquido-Líquido/métodos , Chá/química , Contaminação de Alimentos/análise , Cromatografia Gasosa-Espectrometria de Massas , Herbicidas/química , Microextração em Fase Líquida/instrumentação , Extração Líquido-Líquido/instrumentação , Seringas
5.
Molecules ; 24(2)2019 Jan 18.
Artigo em Inglês | MEDLINE | ID: mdl-30669256

RESUMO

The reliable and efficient production of radioisotopes for diagnosis and therapy is becoming an increasingly important capability, due to their demonstrated utility in Nuclear Medicine applications. Starting from the first processes involving the separation of 99mTc from irradiated materials, several methods and concepts have been developed to selectively extract the radioisotopes of interest. Even though the initial methods were based on liquid-liquid extraction (LLE) approaches, the perceived difficulty in automating such processes has slowly moved the focus towards resin separation methods, whose basic chemical principles are often similar to the LLE ones in terms of chelators and phases. However, the emerging field of flow chemistry allows LLE to be easily automated and operated in a continuous manner, resulting in an even improved efficiency and reliability. In this contribution, we will outline the fundamentals of LLE processes and their translation into flow-based apparatuses; in addition, we will provide examples of radioisotope separations that have been achieved using LLE methods. This article is intended to offer insights about the future potential of LLE to purify medically relevant radioisotopes.


Assuntos
Extração Líquido-Líquido , Radioisótopos/isolamento & purificação , Extração Líquido-Líquido/instrumentação , Extração Líquido-Líquido/métodos , Medicina Nuclear/instrumentação , Medicina Nuclear/métodos
6.
Molecules ; 24(7)2019 Apr 06.
Artigo em Inglês | MEDLINE | ID: mdl-30959894

RESUMO

The new prototype device is applied to the Solvent Front Position Extraction (SFPE) sample preparation procedure. The mobile phase is deposited onto the chromatographic plate adsorbent layer by the pipette, which is moved, according to programmed movement path, by a 3D printer mechanism. The application of the prototype device to SFPE procedure leads to the increased repeatability of the results and significant reduction of the analysis time in comparison to the classical procedure of chromatogram development. Additionally, the new equipment allows use procedures that are not possible to run using the classic chromatogram development. In this paper, the results of manual and semi-automatic sample preparation with SFPE are compared and the possible application of this prototype device is discussed.


Assuntos
Automação , Extração Líquido-Líquido , Solventes , Animais , Bovinos , Cromatografia Líquida , Desenho de Equipamento , Extração Líquido-Líquido/instrumentação , Extração Líquido-Líquido/métodos , Solventes/química , Espectrometria de Massas em Tandem
7.
Molecules ; 24(16)2019 Aug 18.
Artigo em Inglês | MEDLINE | ID: mdl-31426603

RESUMO

Zeaxanthin and lutein have a wide range of pharmacological applications. In this study, we conducted systematic experimental research to optimize antioxidant extraction based on detection, extraction, process amplification, and purification. An ultrasonic-assisted method was used to extract zeaxanthin and lutein with high efficiency from corn gluten meal. Firstly, the effects of solid-liquid ratio, extraction temperature, and ultrasonic extraction time on the extraction of zeaxanthin were investigated in single-factor experiments. The optimization extraction parameters of zeaxanthin and lutein with ethanol solvent were obtained using the response surface methodology (RSM) as follows: liquid-solid ratio of 7.9:1, extraction temperature of 56 °C, and extraction time of 45 min. The total content of zeaxanthin and lutein was 0.501%. The optimum extraction experimental parameters were verified by process amplification, and we confirmed that the parameters of the extraction process optimized using the RSM design are reliable and precise. Zeaxanthin and lutein from crude extract of corn gluten were separated and purified using silica gel column chromatography with the purity of zeaxanthin increasing from 0.28% to 31.5% (about 110 times) and lutein from 0.25% to 16.3% (about 65 times), which could be used for large-scale industrial production of carotenoids.


Assuntos
Antioxidantes/isolamento & purificação , Extração Líquido-Líquido/métodos , Luteína/isolamento & purificação , Sonicação/métodos , Zea mays/química , Zeaxantinas/isolamento & purificação , Etanol/química , Análise Fatorial , Humanos , Extração Líquido-Líquido/instrumentação , Reprodutibilidade dos Testes , Sementes/química , Solventes/química
8.
Molecules ; 24(8)2019 Apr 23.
Artigo em Inglês | MEDLINE | ID: mdl-31018583

RESUMO

Polysaccharides are a main active substance in Panax ginseng; however, microwave-assisted extraction used to prepare P. ginseng polysaccharides (MPPG) has rarely been reported, and knowledge of the bactericidal activity of P. ginseng polysaccharides remains low. Thus, this study was designed to investigate the extraction of P. ginseng polysaccharides by using two methods-hot water extraction and microwave-assisted extraction-and compare their chemical composition and structure. In addition, their antibacterial and antioxidant activities were also determined. The data implied that P. ginseng polysaccharides extracted by microwave-assisted extraction possessed a higher extraction yield than hot water extraction (WPPG) under optimized conditions, and the actual yields were 41.6% ± 0.09% and 28.5% ± 1.62%, respectively. Moreover, the preliminary characterization of polysaccharides was identified after purification. The WPPG with the molecular weight (Mw) of 2.07 × 105 Da was composed of Man, Rib, Rha, GalA, Glu, Gal, and Arab, and the typical characteristics of polysaccharides were determined by IR spectra. Compared with WPPG, MPPG had a higher Mw, uronic acid content, and Glu content. More importantly, the antioxidant activity of MPPG was higher than WPPG, which was probably ascribed to its highly Mw and abundant uronic acid content. Besides, both of them exhibited high bactericidal activity. These results demonstrate that microwave-assisted extraction is an effective method for obtaining P. ginseng polysaccharides, and MPPG could be applied as an antioxidant and antibacterial agent.


Assuntos
Antibacterianos/isolamento & purificação , Antioxidantes/isolamento & purificação , Extração Líquido-Líquido/métodos , Panax/química , Polissacarídeos/isolamento & purificação , Antibacterianos/química , Antibacterianos/farmacologia , Antioxidantes/química , Antioxidantes/farmacologia , Análise Fatorial , Ginsenosídeos/química , Ginsenosídeos/isolamento & purificação , Ginsenosídeos/farmacologia , Bactérias Gram-Negativas/efeitos dos fármacos , Bactérias Gram-Negativas/crescimento & desenvolvimento , Bactérias Gram-Positivas/efeitos dos fármacos , Bactérias Gram-Positivas/crescimento & desenvolvimento , Temperatura Alta , Extração Líquido-Líquido/instrumentação , Testes de Sensibilidade Microbiana , Micro-Ondas , Peso Molecular , Monossacarídeos/química , Monossacarídeos/isolamento & purificação , Monossacarídeos/farmacologia , Extratos Vegetais/química , Proteínas de Plantas/química , Proteínas de Plantas/isolamento & purificação , Proteínas de Plantas/farmacologia , Raízes de Plantas/química , Polissacarídeos/química , Polissacarídeos/farmacologia , Ácidos Urônicos/química , Ácidos Urônicos/isolamento & purificação , Ácidos Urônicos/farmacologia , Água/química
9.
Anal Bioanal Chem ; 410(20): 4967-4978, 2018 Aug.
Artigo em Inglês | MEDLINE | ID: mdl-29947895

RESUMO

Benzodiazepines (BZD) and Z-hypnotics are frequently analyzed in forensic laboratories, and in 2012, the designer benzodiazepines (DBZD) emerged on the illegal drug scene. DBZD represent a particular challenge demanding new analytical methods. In this work, parallel artificial liquid membrane extraction (PALME) is used for sample preparation of DBZD, BZD, and Z-hypnotics in whole blood prior to UHPLC-MS/MS analysis. PALME of BZD, DBZD, and Z-hypnotics was performed from whole blood samples, and the analytes were extracted across a supported liquid membrane (SLM) and into an acceptor solution of dimethyl sulfoxide and 200 mM formic acid (75:25, v/v). The method was validated according to EMA guidelines. The method was linear throughout the calibration range (R2 > 0.99). Intra- and inter-day accuracy and precision, as well as matrix effects, were within the guideline limit of ± 15%. LOD and LLOQ ranged from 0.10 to 5.0 ng mL-1 and 3.2 to 160 ng mL-1, respectively. Extraction recoveries were reproducible and above 52%. The method was specific, and the analytes were stable in the PALME extracts for 4 and 10 days at 10 and - 20 °C. No carry-over was observed within the calibration range. PALME and UHPLC-MS/MS for the determination of DBZD, BZD, and Z-hypnotics in whole blood are a green and low-cost alternative that provides high sample throughput (96-well format), extensive sample clean-up, good sensitivity, and high reproducibility. The presented method is also the first method incorporating analysis of DBZD, BZD, and Z-hypnotics in whole blood in one efficient analysis. Graphical abstract.


Assuntos
Benzodiazepinas/sangue , Cromatografia Líquida de Alta Pressão/métodos , Drogas Desenhadas/análise , Hipnóticos e Sedativos/sangue , Membranas Artificiais , Espectrometria de Massas em Tandem/métodos , Benzodiazepinas/análise , Benzodiazepinas/isolamento & purificação , Cromatografia Líquida de Alta Pressão/economia , Drogas Desenhadas/isolamento & purificação , Desenho de Equipamento , Humanos , Hipnóticos e Sedativos/análise , Hipnóticos e Sedativos/isolamento & purificação , Limite de Detecção , Extração Líquido-Líquido/economia , Extração Líquido-Líquido/instrumentação , Espectrometria de Massas em Tandem/economia , Fatores de Tempo
10.
Anal Bioanal Chem ; 410(22): 5331-5351, 2018 Sep.
Artigo em Inglês | MEDLINE | ID: mdl-29951771

RESUMO

Monitoring of chemicals of toxicological concern in food is commonly needed for many purposes, which include (in part) food safety, regulatory enforcement, risk assessment, international food trade, label claims, environmental protection, industry needs, academic research, and consumer confidence. Chemicals of current concern include a variety of toxins, pesticides, veterinary drugs, growth promoters, environmental contaminants, toxic metals, allergens, endocrine disruptors, genetically modified organisms, melamine, acrylamide, furans, nitrosamines, food additives, packaging components, and miscellaneous other chemicals. In light of past crises, the potential harm from known or unknown chemicals not currently monitored are a source of additional concern by the food industry, regulators, scientists, and consumers. As global food trade has expanded and detection techniques have improved, chemical contaminant analysis of foods has also increased in importance and activity. This critical review article is aimed to highlight current trends in the literature, including neglected research needs, on the analysis of chemicals of toxicological concern in foods. Graphical abstract.


Assuntos
Técnicas de Química Analítica/métodos , Contaminação de Alimentos/análise , Análise de Perigos e Pontos Críticos de Controle/métodos , Animais , Técnicas Biossensoriais/instrumentação , Técnicas Biossensoriais/métodos , Técnicas de Química Analítica/instrumentação , Cromatografia/instrumentação , Cromatografia/métodos , Inocuidade dos Alimentos/métodos , Humanos , Extração Líquido-Líquido/instrumentação , Extração Líquido-Líquido/métodos , Espectrometria de Massas/instrumentação , Espectrometria de Massas/métodos , Extração em Fase Sólida/instrumentação , Extração em Fase Sólida/métodos , Estudos de Validação como Assunto
11.
Mar Drugs ; 16(12)2018 Dec 13.
Artigo em Inglês | MEDLINE | ID: mdl-30551573

RESUMO

The metabolism of seaweeds depends on environmental parameters, the availability of nutrients, and biotic/abiotic stresses; therefore, their chemical composition fluctuates throughout the year. This study investigated seasonal variations in the metabolome of the Baltic Sea brown alga Fucus vesiculosus and its potential relation to the bioactivity profile. By using a definitive screening design (DSD) combined with pressurised liquid extraction (PLE), an optimised protocol was developed to extract algal biomass monthly for a full calendar year. An untargeted metabolomics approach using ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MSn)-based molecular networking and manual dereplication was employed. The extracts were simultaneously screened for their in vitro antimicrobial, anticancer/apoptotic, and free radical scavenging activities. 44 compounds were putatively dereplicated in the metabolome. Many compounds were found to vary with the sampling month; phlorotannin total ion count (TIC) was highest in summer, whilst chlorophylls, lipids, and carotenoids peaked in winter and spring. The greatest radical scavenging and apoptotic activities against pancreas cancer cells observed in the summer months were attributed to high phlorotannin TIC. Methicillin-resistant Staphylococcus aureus (MRSA) inhibitory activity was produced year-round without a clear seasonal trend. This is the first study applying DSD-based optimised PLE extraction combined with a metabolome analysis of F. vesiculosus for the identification of seasonal variations in both metabolome and bioactivity.


Assuntos
Fucus/metabolismo , Metaboloma , Extratos Vegetais/farmacologia , Estações do Ano , Alga Marinha/metabolismo , Células A549 , Antibacterianos/química , Antibacterianos/isolamento & purificação , Antibacterianos/metabolismo , Antibacterianos/farmacologia , Antineoplásicos Fitogênicos/química , Antineoplásicos Fitogênicos/isolamento & purificação , Antineoplásicos Fitogênicos/metabolismo , Antineoplásicos Fitogênicos/farmacologia , Produtos Biológicos/química , Produtos Biológicos/isolamento & purificação , Produtos Biológicos/metabolismo , Produtos Biológicos/farmacologia , Cromatografia Líquida de Alta Pressão/instrumentação , Cromatografia Líquida de Alta Pressão/métodos , Ensaios de Seleção de Medicamentos Antitumorais , Sequestradores de Radicais Livres/química , Sequestradores de Radicais Livres/isolamento & purificação , Sequestradores de Radicais Livres/metabolismo , Sequestradores de Radicais Livres/farmacologia , Fucus/química , Humanos , Extração Líquido-Líquido/instrumentação , Extração Líquido-Líquido/métodos , Metabolômica/instrumentação , Metabolômica/métodos , Staphylococcus aureus Resistente à Meticilina/efeitos dos fármacos , Testes de Sensibilidade Microbiana , Extratos Vegetais/química , Extratos Vegetais/isolamento & purificação , Pressão , Alga Marinha/química
12.
Natl Med J India ; 31(2): 67-69, 2018.
Artigo em Inglês | MEDLINE | ID: mdl-30829219

RESUMO

Background: Methamphetamine cannot be detected through conventional urine screening tests or other analytical methods in methamphetamine abusers who have not used the drug for some time. In some instances, detection of methamphetamine in fingernails can be a good alternative. We aimed to determine the sensitivity and specificity of the one-step methamphetamine test strip used in the detection of methamphetamine in urine in the detection of methamphetamine in fingernails. Methods: We took 72 fingernail samples, including 60 samples from methamphetamine abusers and 12 samples as controls from their relatives who had no history of methamphetamine use. The liquid-liquid extraction method was used on fingernail samples, and the resultant solution was tested with one-step methamphetamine test strip. We analysed participants' demographics including age, gender, duration of methamphetamine abuse and strip test results. Results: The mean (SD) age of the participants was 25 (4.33) years. The mean (SD) duration of methamphetamine abuse was 10 (4.5) months. Of the 72 participants, 61 (84.7%) had positive and 11 (15.3%) had negative strip test results. All 60 methamphetamine abusers had positive test results. A positive or negative history of methamphetamine abuse was taken as the gold standard. The sensitivity and specificity of the test was 100% and 91.6%, respectively. Conclusion: Performing liquid-liquid extraction on fingernails and using the strip test for detection of methamphetamine is a simple, inexpensive, rapid and accessible method, and its high sensitivity and specificity make it appropriate for screening. This method may be preferred over other urine and blood methamphetamine detection methods when the patient has not used the drug for a few days.


Assuntos
Transtornos Relacionados ao Uso de Anfetaminas/diagnóstico , Extração Líquido-Líquido/métodos , Metanfetamina/análise , Unhas/química , Detecção do Abuso de Substâncias/métodos , Adulto , Transtornos Relacionados ao Uso de Anfetaminas/etiologia , Estudos de Viabilidade , Feminino , Humanos , Extração Líquido-Líquido/instrumentação , Masculino , Metanfetamina/efeitos adversos , Sensibilidade e Especificidade , Detecção do Abuso de Substâncias/instrumentação , Fatores de Tempo , Adulto Jovem
13.
Molecules ; 23(6)2018 May 29.
Artigo em Inglês | MEDLINE | ID: mdl-29844266

RESUMO

As chemical drugs, separation and quantification of the specific enantiomer from the chiral compounds in herbal medicines are becoming more important. To clarify the chemical characterization of chiral glucosinolates-the antiviral active ingredients of Radix Isatidis, an optimized efficient method of HPLC-UV-CD was developed to simultaneously separate and quantify the four main chiral glucosinolates: progoitrin, epiprogoitrin, and R,S-goitrin. The first step was to determine progoitrin, epiprogoitrin, and R,S-goitrin using HPLC-UV, and then determine the R-goitrin and S-goitrin by coupling with CD detection. Subsequently, through the linear relations between anisotropy factor (g factor) and the percent optical purity of R-goitrin, the contents of R-goitrin and S-goitrin from the R,S-goitrin mixture were calculated separately. Furthermore, the chemical composition features of the four chiral glucosinolates in 37 samples from crude drugs, decoction pieces, and granules of R. Isatidis were conducted. The total content of the four glucosinolates was obviously higher in crude drugs, and the variance character of each glucosinolate contents was different. In summary, the accurate measurement method reported here allows for better control of the internal quality of R. Isatidis and its granules and provides a powerful approach for the analysis of other chiral components in traditional Chinese medicines.


Assuntos
Antivirais/isolamento & purificação , Medicamentos de Ervas Chinesas/química , Glucosinolatos/isolamento & purificação , Extração Líquido-Líquido/métodos , Oxazolidinonas/isolamento & purificação , Antivirais/química , Cromatografia Líquida de Alta Pressão , Dicroísmo Circular , Glucosinolatos/química , Humanos , Extração Líquido-Líquido/instrumentação , Medicina Tradicional Chinesa , Oxazolidinonas/química , Extratos Vegetais/química , Raízes de Plantas/química , Estereoisomerismo
14.
Wei Sheng Yan Jiu ; 47(3): 446-452, 2018 May.
Artigo em Chinês | MEDLINE | ID: mdl-30082015

RESUMO

OBJECTIVE: To establish a method to determinate 25 pesticides in liquid health food from Chinese herbal medicines by direct immersion solid phase micro extraction coupled with gas chromatography-mass spectrometry. METHODS: The sample was diluted with ultrapure water, adjusted p H with acetic acid, and then filtered by 0. 45µm filter. The target compounds were extracted and concentrated by the method of on-line immersion solid phase micro extraction( SPME) coupled with 65 µm PDMS/DVB extraction fiber. The sample was separated by GC-MS with TG-5 MS( 30 m × 0. 25 mm ×0. 25 µm) capillary column. RESULTS: The method showed a good linearity R2 above 0. 99 in the range of 20-200 µg/kg for 25 organic phosphorus pesticides analytes with average recovery rates of 77. 9%-97. 9%( n = 6) and the relative standard deviation( RSD)within 1. 72%-13. 57%. The limits of detection( LOD) were between 3-10 µg/kg. CONCLUSION: The method is simple, accurate, sensitive and very environmental friendly. It is suitable for the determination of 25 pesticides in liquid health food from Chinese herbal medicines.


Assuntos
Análise de Alimentos/métodos , Contaminação de Alimentos/análise , Praguicidas/isolamento & purificação , Benzenossulfonatos , Cromatografia Gasosa-Espectrometria de Massas , Humanos , Limite de Detecção , Extração Líquido-Líquido/instrumentação , Microextração em Fase Sólida/instrumentação
15.
Anal Chem ; 89(2): 1155-1162, 2017 01 17.
Artigo em Inglês | MEDLINE | ID: mdl-27958721

RESUMO

Circulating tumor cells (CTCs) have great potential to provide minimally invasive ways for the early detection of cancer metastasis and for the response monitoring of various cancer treatments. Despite the clinical importance and progress of CTC-based cancer diagnostics, most of the current methods of enriching CTCs are difficult to implement in general hospital settings due to complex and time-consuming protocols. Among existing technologies, size-based isolation methods provide antibody-independent, relatively simple, and high throughput protocols. However, the clogging issues and lower than desired recovery rates and purity are the key challenges. In this work, inspired by antifouling membranes with liquid-filled pores in nature, clog-free, highly sensitive (95.9 ± 3.1% recovery rate), selective (>2.5 log depletion of white blood cells), rapid (>3 mL/min), and label-free isolation of viable CTCs from whole blood without prior sample treatment is achieved using a stand-alone lab-on-a-disc system equipped with fluid-assisted separation technology (FAST). Numerical simulation and experiments show that this method provides uniform, clog-free, ultrafast cell enrichment with pressure drops much less than in conventional size-based filtration, at 1 kPa. We demonstrate the clinical utility of the point-of-care detection of CTCs with samples taken from 142 patients suffering from breast, stomach, or lung cancer.


Assuntos
Separação Celular/instrumentação , Técnicas Analíticas Microfluídicas/instrumentação , Neoplasias/patologia , Células Neoplásicas Circulantes/patologia , Linhagem Celular Tumoral , Separação Celular/economia , Separação Celular/métodos , Tamanho Celular , Desenho de Equipamento , Humanos , Extração Líquido-Líquido/economia , Extração Líquido-Líquido/instrumentação , Extração Líquido-Líquido/métodos , Técnicas Analíticas Microfluídicas/economia , Técnicas Analíticas Microfluídicas/métodos , Neoplasias/sangue , Fatores de Tempo
16.
J Sep Sci ; 40(1): 203-212, 2017 01.
Artigo em Inglês | MEDLINE | ID: mdl-27759332

RESUMO

In pesticide residue analysis, relatively low-sensitivity traditional detectors, such as UV, diode array, electron-capture, flame photometric, and nitrogen-phosphorus detectors, have been used following classical sample preparation (liquid-liquid extraction and open glass column cleanup); however, the extraction method is laborious, time-consuming, and requires large volumes of toxic organic solvents. A quick, easy, cheap, effective, rugged, and safe method was introduced in 2003 and coupled with selective and sensitive mass detectors to overcome the aforementioned drawbacks. Compared to traditional detectors, mass spectrometers are still far more expensive and not available in most modestly equipped laboratories, owing to maintenance and cost-related issues. Even available, traditional detectors are still being used for analysis of residues in agricultural commodities. It is widely known that the quick, easy, cheap, effective, rugged, and safe method is incompatible with conventional detectors owing to matrix complexity and low sensitivity. Therefore, modifications using column/cartridge-based solid-phase extraction instead of dispersive solid-phase extraction for cleanup have been applied in most cases to compensate and enable the adaptation of the extraction method to conventional detectors. In gas chromatography, the matrix enhancement effect of some analytes has been observed, which lowers the limit of detection and, therefore, enables gas chromatography to be compatible with the quick, easy, cheap, effective, rugged, and safe extraction method. For liquid chromatography with a UV detector, a combination of column/cartridge-based solid-phase extraction and dispersive solid-phase extraction was found to reduce the matrix interference and increase the sensitivity. A suitable double-layer column/cartridge-based solid-phase extraction might be the perfect solution, instead of a time-consuming combination of column/cartridge-based solid-phase extraction and dispersive solid-phase extraction. Therefore, replacing dispersive solid-phase extraction with column/cartridge-based solid-phase extraction in the cleanup step can make the quick, easy, cheap, effective, rugged, and safe extraction method compatible with traditional detectors for more sensitive, effective, and green analysis.


Assuntos
Técnicas de Química Analítica/economia , Técnicas de Química Analítica/instrumentação , Resíduos de Praguicidas/análise , Cromatografia Gasosa/economia , Cromatografia Gasosa/instrumentação , Cromatografia Líquida/economia , Cromatografia Líquida/instrumentação , Produtos Agrícolas/química , Extração Líquido-Líquido/economia , Extração Líquido-Líquido/instrumentação , Extração em Fase Sólida/economia , Extração em Fase Sólida/instrumentação
17.
Molecules ; 22(12)2017 Dec 05.
Artigo em Inglês | MEDLINE | ID: mdl-29206179

RESUMO

The purpose of this study was to determine the possibility of using chokeberry powder as a supplement in apple juice to increase the nutritional value of the final product with the aim of developing a new functional food product. Also, to determine the influence of ultrasound assisted extraction on the bioactive compounds content, nutritional composition and antioxidant potential of apple juice with added chokeberry powder. The juice samples with added chokeberry powder had higher antioxidant capacity, irrespective of the extraction technique used. Apple juice samples with added chokeberry powder treated with high intensity ultrasound had significantly higher content of all analyzed bioactive compounds. The application of high intensity ultrasound significantly reduced the extraction time of the plant material. A positive correlation between vitamin C content, total phenols, flavonoids and anthocyanins content and antioxidant capacity was determined in juice samples with added chokeberry powder treated with high intensity ultrasound.


Assuntos
Antioxidantes/isolamento & purificação , Ácido Ascórbico/isolamento & purificação , Sucos de Frutas e Vegetais/análise , Extração Líquido-Líquido/métodos , Malus/química , Photinia/química , Antocianinas/química , Antocianinas/isolamento & purificação , Antioxidantes/química , Ácido Ascórbico/química , Flavonoides/química , Flavonoides/isolamento & purificação , Frutas/química , Extração Líquido-Líquido/instrumentação , Fenóis/química , Fenóis/isolamento & purificação , Extratos Vegetais/química , Polifenóis/química , Polifenóis/isolamento & purificação , Pós , Sonicação/instrumentação , Sonicação/métodos
18.
Molecules ; 22(6)2017 Jun 09.
Artigo em Inglês | MEDLINE | ID: mdl-28598407

RESUMO

In this study, the ultrasound-assisted extraction of polysaccharides (PSA) from Pinelliae Rhizoma Praeparatum Cum Alumine (PRPCA) was optimized by response surface methodology (RSM). The structural characteristics of PSA were analyzed by UV-vis spectroscopy, infrared spectroscopy, scanning electron microscopy, high performance gel permeation chromatography and high performance liquid chromatography, respectively. In addition, antioxidant and antimicrobial activities of PSA were studied by different in vitro assays. Results indicated that the optimal extraction conditions were as follows: the ratio of water to raw of 30 mL/g, extraction time of 46.50 min, ultrasonic temperature of 72.00 °C, and ultrasonic power of 230 W. Under these conditions, the obtained PSA yield (13.21 ± 0.37%) was closely agreed with the predicted yield by the model. The average molecular weights of the PSA were estimated to be 5.34 × 10³ and 6.27 × 105 Da. Monosaccharide composition analysis indicated that PSA consisted of mannose, galactose uronic acid, glucose, galactose, arabinose with a molar ratio of 1.83:0.55:75.75:1.94:0.45. Furthermore, PSA exhibited moderate antioxidant and antibacterial activities in vitro. Collectively, this study provides a promising strategy to obtain bioactive polysaccharides from processed products of herbal medicines.


Assuntos
Antibacterianos/isolamento & purificação , Antioxidantes/isolamento & purificação , Extração Líquido-Líquido/métodos , Pinellia/química , Polissacarídeos/isolamento & purificação , Sonicação/métodos , Antibacterianos/química , Antibacterianos/farmacologia , Antioxidantes/química , Antioxidantes/farmacologia , Benzotiazóis/antagonistas & inibidores , Benzotiazóis/química , Compostos de Bifenilo/antagonistas & inibidores , Compostos de Bifenilo/química , Candida albicans/efeitos dos fármacos , Candida albicans/crescimento & desenvolvimento , Escherichia coli/efeitos dos fármacos , Escherichia coli/crescimento & desenvolvimento , Análise Fatorial , Extração Líquido-Líquido/instrumentação , Testes de Sensibilidade Microbiana , Monossacarídeos/química , Picratos/antagonistas & inibidores , Picratos/química , Polissacarídeos/química , Polissacarídeos/farmacologia , Staphylococcus aureus/efeitos dos fármacos , Staphylococcus aureus/crescimento & desenvolvimento , Ácidos Sulfônicos/antagonistas & inibidores , Ácidos Sulfônicos/química , Superóxidos/antagonistas & inibidores , Superóxidos/química , Temperatura , Ácidos Urônicos/química
19.
Water Sci Technol ; 76(9-10): 2313-2320, 2017 Nov.
Artigo em Inglês | MEDLINE | ID: mdl-29144289

RESUMO

A new circular microchannel device has been proposed for the removal of chromium(III) from aqueous waste solution by using kerosene as a diluent and (2-ethylhexyl) 2-ethylhexyl phosphonate as an extractant. The proposed device has several advantages such as a flexible and easily adaptable design, easy maintenance, and cheap setup without the requirement of microfabrication. To study the extraction efficiency and advantages of the circular microchannel device in the removal of chromium(III), the effects of various operating conditions such as the inner diameter of the channel, the total flow velocity, the phase ratio, the initial pH of aqueous waste solution, the reaction temperature and the initial concentration of extractant on the extraction efficiency are investigated and the optimal process conditions are obtained. The results show that chromium(III) in aqueous waste solution can be effectively removed with (2-ethylhexyl) 2-ethylhexyl phosphonate in the circular microchannel. Under optimized conditions, an extraction efficiency of chromium(III) of more than 99% can be attained and the aqueous waste solution can be discharged directly, which can meet the Chinese national emission standards.


Assuntos
Cromo/isolamento & purificação , Extração Líquido-Líquido/métodos , Poluentes Químicos da Água/isolamento & purificação , Purificação da Água/métodos , Cromo/análise , Concentração de Íons de Hidrogênio , Querosene/análise , Extração Líquido-Líquido/instrumentação , Água , Poluentes Químicos da Água/análise , Purificação da Água/instrumentação
20.
J Environ Sci Health B ; 52(1): 1-9, 2017 Jan 02.
Artigo em Inglês | MEDLINE | ID: mdl-27629156

RESUMO

A simultaneous method for quantifying eight metabolites of organophosphate pesticides and pyrethroid pesticides in urine samples has been established. The analytes were extracted using liquid-liquid extraction coupled with WCX solid phase extraction (SPE) cartridges. Eight metabolites were chemically derivatized before analysis using gas chromatography-tandem mass spectrometry (GC-MS-MS). The separation was performed on a HP-5MS capillary column (30 m × 0.25 mm × 0.25 µm) with temperature programming. The detection was performed under electro-spray ionization (ESI) in multiple reaction monitoring (MRM) mode. An internal standard method was used. The extraction solvent, types of SPE cartridges and eluents were optimized by comparing the sample recoveries under different conditions. The results showed that the calibration curves of the five organophosphorus pesticides metabolites were linear in the range of 0.2-200 µg/L (r2 ≥ 0.992) and that of the three pyrethroid pesticides metabolites were linear in the range of 0.025-250 µg/L (r2 ≥ 0.991). The limits of detection (LODs, S/N ≥ 3) and the limits of quantification (LOQs, S/N ≥ 10) of the eight metabolites were 0.008-0.833 µg/L and 0.25-2.5 µg/L, respectively. The recoveries of the eight metabolites ranged from 54.08% to 82.49%. This efficient, stable, and cost-effective method is adequate to handle the large number of samples required for surveying the exposure level of organophosphorus and pyrethroid pesticides in the general population.


Assuntos
Cromatografia Gasosa-Espectrometria de Massas/métodos , Organofosfatos/urina , Praguicidas/urina , Espectrometria de Massas em Tandem/métodos , Calibragem , Exposição Ambiental/análise , Humanos , Limite de Detecção , Extração Líquido-Líquido/instrumentação , Extração Líquido-Líquido/métodos , Compostos Organofosforados , Piretrinas/urina , Reprodutibilidade dos Testes , Extração em Fase Sólida/instrumentação , Extração em Fase Sólida/métodos
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