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1.
Anal Methods ; 16(34): 5751-5776, 2024 Aug 29.
Artigo em Inglês | MEDLINE | ID: mdl-39143944

RESUMO

Malaria is a serious public health problem, being an endemic disease in 84 countries, mainly in Africa. This review explores the application of capillary electrophoresis (CE) techniques for analyzing antimalarial drugs, highlighting methods from 2000 to 2023 for the analysis of pharmaceutical formulations and human biological samples. The versatility, selectivity, high efficiency, cost-effectiveness, and high analytical frequency of CE techniques have become attractive choices for pharmaceutical analysis, focusing on quality control and impurity analysis applications. The evolution of achiral and chiral electromigration methods has been described based on the features of each mode of separation: capillary zone electrophoresis (CZE), micellar electrokinetic chromatography, microemulsion electrokinetic chromatography, and capillary electrochromatography. As expected, CZE is reported in most articles owing to its compatibility with drug properties and separation mode. However, it is necessary to perform other separation modes for a few drugs that are present in neutral form. After exhaustive research using different databases and statistical analyses, 27 articles using CE techniques for antimalarial drug analysis were found and are mentioned in this review.


Assuntos
Antimaláricos , Eletroforese Capilar , Antimaláricos/análise , Antimaláricos/química , Eletroforese Capilar/métodos , Humanos , Malária/tratamento farmacológico , Composição de Medicamentos/métodos
2.
Crit Rev Anal Chem ; : 1-13, 2023 Dec 26.
Artigo em Inglês | MEDLINE | ID: mdl-38147303

RESUMO

Lipid peroxidation occurs when substances, such as reactive oxygen species, attack lipids. Polyunsaturated fatty acids are the main targets. Several products are formed, including primary products such as lipid hydroperoxides and secondary products such as malondialdehyde (MDA), the most used lipid peroxidation biomarker. As MDA levels are elevated in several diseases, MDA is an essential indicator for assessing pathological states. The thiobarbituric acid reactive substances assay is the most widely used method for MDA determination. However, it lacks specificity. Capillary Electrophoresis (CE) is a separation technique that has been used to quantify MDA in biological samples. This technique has advantages such as the low amount of biological sample required, absence or low volume of organic solvent, short analysis time, separation of interferents, sample preparation step with only protein precipitation, and the possibility of direct detection of the MDA, without derivatization. To our knowledge, this review article is the first to show the CE background for analyzing MDA in biological samples. Therefore, given the potential of MDA in evaluating pathological states, this article demonstrates the potential of CE to become a reference method for MDA determination in clinical analysis laboratories, which will play a significant role in diagnosing and monitoring diseases.

3.
Anal Methods ; 15(20): 2512-2521, 2023 05 25.
Artigo em Inglês | MEDLINE | ID: mdl-37184618

RESUMO

Investigations of untargeted metabolomics are based on high-quality data acquisition usually from multiplatform systems that include high-resolution mass spectrometry equipment. The comprehensive set of results is used as data entry for bioinformatics and machine learning sciences to access reliable metabolic and biochemical information for clinical, forensic, environmental, and endless applications. In this context, design of experiments is a powerful tool for optimizing data acquisition procedures, using a multivariate approach, which enables the maximization of a high-quality amount of information with reduced number of tests. In this study, we applied a 33 Box-Behnken factorial design with central point triplicate for optimizing the ionization of an HPLC-ESI-QTOF method used for screening urine samples. Nozzle voltage (V), fragmentor voltage (V) and nebulizer pressure (psig) were the factors selected for variation. The response surface methodology was applied in the molecular features extracted at each level, resulting in a statistical model that helps evaluating the synergic interaction between these factors. Together with the qualitative analysis of the resulting total ion chromatograms, we came across a reproducible (6.14% RSD) and highly efficient method for untargeted metabolomics of human urine samples. The proposed method can be useful for applications in several urine-based metabolomics-driven studies, as the factorial design can be applied in the development of any analytical protocol considering different LC-MS setups.


Assuntos
Metaboloma , Metabolômica , Humanos , Metabolômica/métodos , Espectrometria de Massas/métodos , Cromatografia Líquida/métodos , Cromatografia Líquida de Alta Pressão/métodos
4.
Anal Methods ; 15(3): 311-321, 2023 01 19.
Artigo em Inglês | MEDLINE | ID: mdl-36562458

RESUMO

Shrimp is one of the most traded fishery products in the world. The shrimp-farming water ionic composition is fundamental to the growth and survival of these specimens. Therefore, this study is aimed to develop a method for the simultaneous separation of Cl-, SO42-, NO3-, NO2-, and HCO3- in this sample by capillary zone electrophoresis with UV indirect detection, without any prior sample treatment, besides dilution. The background electrolyte (BGE) was composed of CrO42- (60 mmol L-1), cetyltrimethylammonium bromide (CTAB, 2.5 mmol L-1), acetonitrile (0.875% (v/v)), and methanol (2.625% (v/v)). The mixture design optimized the BGE composition. Acetonitrile and methanol changed the degree of solvation of the anions, which decreased the radius, a phenomenon proven by calculating the radius of anions in all the conditions of the mixture design. The optimized and validated method allowed the simultaneous determination of the five above-mentioned anions in 10 min.


Assuntos
Dióxido de Nitrogênio , Água , Metanol , Eletrólitos , Ânions/análise , Agricultura
5.
Eur J Med Chem ; 165: 18-30, 2019 Mar 01.
Artigo em Inglês | MEDLINE | ID: mdl-30654237

RESUMO

A series of1,2,4- and 1,3,4-oxadiazole derivatives were synthesized and evaluated for their anticancer activity. Halogenated 1,2,4-oxadiazoles were obtained from benzonitrile and coupled either lipophilic amines or with aminoalcohols. Lipophilic 1,3,4-oxadiazole derivatives were obtained through the Mannich reactions between 5-(aryl)-1,3,4-oxadiazole-2-thiol and alkylated or acylated amines. The in vitro cytotoxic effects were evaluated against 4T1- mammary carcinoma and CT26 - colon cancer cells. The best results were obtained for the 1,3,4-oxadiazole coupled to alkylated piperazine with 10-14 carbon chain moiety, with IC50 values ranging from 1.6 to 3.55µΜ for the 4T1 cell line, and from 1.6 to 3.9 µM for the CT26.WT cell line, and selectivity index up to 19. The most potent compounds were investigated with AnnexinV and PI staining as indicative of apoptosis induction.


Assuntos
Antineoplásicos/química , Oxidiazóis/farmacologia , Antineoplásicos/síntese química , Antineoplásicos/farmacologia , Apoptose/efeitos dos fármacos , Linhagem Celular Tumoral , Humanos , Interações Hidrofóbicas e Hidrofílicas , Oxidiazóis/síntese química , Oxidiazóis/química , Relação Estrutura-Atividade
6.
J AOAC Int ; 98(6): 1591-7, 2015.
Artigo em Inglês | MEDLINE | ID: mdl-26651572

RESUMO

A rapid method has been proposed for determination of the main conjugated linoleic acid precursors such as linoleic (C18:2 n-6) and linolenic (C18:3 n-3) acids in forages by capillary zone electrophoresis (CZE) with direct UV detection at 200 nm. Among the fatty acids found in forages, C18:2 n-6 and C18:3 n-3 have received particular attention due to their roles as precursors for the synthesis of conjugated linoleic acid, a class of health-enhancing compounds that is predominantly found in dairy products. The electrolyte background consisted of 12.0 mmol/L tetraborate buffer (pH 9.2) added to 12.0 mmol/L Brij 35®, 17% acetonitrile, and 33% methanol. Under the optimized conditions, the baseline separation of C18:2 n-6 and C18:3 n-3 was achieved within 4 min. The CZE-UV method was compared to GC with a flame ionization detector, which is the American Oil Chemists' Society (AOCS 996.06) official method for fatty acid analysis. The methods did not show any evidence of significant differences within 95% confidence interval (P>0.05). The CZE-UV method was successfully applied to the analysis of 80 genotypes of Brachiaria ruzizienses clones submitted to a genetic improvement program in agricultural research.


Assuntos
Brachiaria/química , Cromatografia Gasosa/métodos , Eletroforese Capilar/métodos , Ácidos Linoleicos Conjugados/análise , Brachiaria/genética , Ionização de Chama , Genótipo , Íons/química , Limite de Detecção , Espectrofotometria Ultravioleta , Fatores de Tempo
7.
J Dairy Sci ; 98(12): 8333-47, 2015 Dec.
Artigo em Inglês | MEDLINE | ID: mdl-26409966

RESUMO

Protein systems (PS) are routinely used by companies from Brazil and around the globe to improve the texture, yield, and palatability of processed foods. Understanding the synergistic behavior among the different protein structures of these systems during thermal treatment under the influence of pH can help to better define optimum conditions for products and processes. The interpretation of the reactions and interactions that occur simultaneously among the protein constituents of these systems as dispersions during thermal processing is still a major challenge. Here, using a rapid viscosity analyzer, we observed the rheological changes in the startup viscosities of 5 PS obtained by combining varying proportions of milk protein concentrate and whey protein concentrate under different conditions of pH (5.0, 6.5, and 7.0) and heat processing (85°C/15min and 95°C/5min). The solutions were standardized to 25% of total solids and 17% of protein. Ten analytical parameters were used to characterize each of the startup-viscosity ramps for 35 experiments conducted in a 2×3 × 5 mixed planning matrix, using principal component analysis to interpret behavioral similarities. The study showed the clear influence of pH 5.5 in the elevation of the initial temperature of the PS startup viscosity by at least 5°C, as well as the effect of different milk protein concentrate:whey protein concentrate ratios above 15:85 at pH 7.0 on the viscographic profile curves. These results suggested that the primary agent driving the changes was the synergism among the reactions and interactions of casein with whey proteins during processing. This study reinforces the importance of the rapid viscosity analyzer as an analytical tool for the simulation of industrial processes involving PS, and the use of the startup viscosity ramp as a means of interpreting the interactions of system components with respect to changes related to the treatment temperature.


Assuntos
Análise de Alimentos , Proteínas do Leite/química , Caseínas/química , Fenômenos Químicos , Temperatura Alta , Concentração de Íons de Hidrogênio , Reologia , Viscosidade , Proteínas do Soro do Leite/química
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