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1.
Sci Rep ; 14(1): 10613, 2024 05 09.
Artigo em Inglês | MEDLINE | ID: mdl-38719831

RESUMO

Chlorogenic acid (CA) is an effective ingredient that can strengthen immunity during following the COVID-19 era. The current cost of CA is high owing to its complex purification process and low yield (approximately 2%). In this study, a one-step path orthogonal experiment was designed based on the results from Gauss calculation, which consisted of acidity, coordination, and hydrolysis in molecules. The optimized extraction conditions were 60 â„ƒ, 60 min, 1:20 liquid ratio, and 40% ethanol in a nitrogen atmosphere controlled using a device of our own design, which led to CA yields of up to 6.35% from potato leaves. The purified CA was analyzed using high-performance liquid chromatography, thin-layer chromatography, ultraviolet-visible spectroscopy, and molecular fluorescence. This accurate and reproducible method can not only be used to obtain high yields of CA but can also be used for the quality control of active plant products and their isomers.


Assuntos
Ácido Clorogênico , Folhas de Planta , Solanum tuberosum , Ácido Clorogênico/análise , Solanum tuberosum/química , Folhas de Planta/química , Cromatografia Líquida de Alta Pressão/métodos , Cromatografia em Camada Fina/métodos
2.
Folia Med (Plovdiv) ; 66(2): 255-263, 2024 Apr 30.
Artigo em Inglês | MEDLINE | ID: mdl-38690822

RESUMO

INTRODUCTION: In the period between 1997 and 2010, sibutramine-containing drugs were widely prescribed for obesity and over-weight management. Due to safety concerns, in 2010 all medicines containing sibutramine were urgently withdrawn from the USA and European pharmaceutical market. Although sibutramine is no longer available in pharmaceutical products, there have been numerous reports of mislabeled weight-loss dietary supplements containing sibutramine.


Assuntos
Depressores do Apetite , Ciclobutanos , Suplementos Nutricionais , Ciclobutanos/análise , Suplementos Nutricionais/análise , Cromatografia em Camada Fina/métodos , Depressores do Apetite/análise , Humanos
3.
Sci Rep ; 14(1): 10025, 2024 05 01.
Artigo em Inglês | MEDLINE | ID: mdl-38693137

RESUMO

The coronavirus-2 has led to a global pandemic of COVID-19 with an outbreak of severe acute respiratory syndrome leading to worldwide quarantine measures and a rise in death rates. The objective of this study is to propose a green, sensitive, and selective densitometric method to simultaneously quantify remdesivir (REM) in the presence of the co-administered drug linezolid (LNZ) and rivaroxaban (RIV) in spiked human plasma. TLC silica gel aluminum plates 60 F254 were used as the stationary phase, and the mobile phase was composed of dichloromethane (DCM): acetone (8.5:1.5, v/v) with densitometric detection at 254 nm. Well-resolved peaks have been observed with retardation factors (Rf) of 0.23, 0.53, and 0.72 for REM, LNZ, and RIV, respectively. A validation study was conducted according to ICH Q2 (R1) Guidelines. The method was rectilinear over the concentration ranges of 0.2-5.5 µg/band, 0.2-4.5 µg/band and 0.1-3.0 µg/band for REM, LNZ and RIV, respectively. The sensitivities of REM, LIN, and RIV were outstanding, with quantitation limits of 128.8, 50.5, and 55.8 ng/band, respectively. The approach has shown outstanding recoveries ranging from 98.3 to 101.2% when applied to pharmaceutical formulations and spiked human plasma. The method's greenness was assessed using Analytical Eco-scale, GAPI, and AGREE metrics.


Assuntos
Monofosfato de Adenosina/análogos & derivados , Alanina/análogos & derivados , Antivirais , Tratamento Farmacológico da COVID-19 , COVID-19 , SARS-CoV-2 , Humanos , Antivirais/sangue , SARS-CoV-2/efeitos dos fármacos , COVID-19/sangue , Cromatografia em Camada Fina/métodos , Análise Custo-Benefício , Alanina/sangue , Linezolida/sangue
4.
Molecules ; 29(7)2024 Apr 08.
Artigo em Inglês | MEDLINE | ID: mdl-38611961

RESUMO

Lipophilicity is one of the most important properties of compounds required to estimate the absorption, distribution, and transport in biological systems, in addition to solubility, stability, and acid-base nature. It is crucial in predicting the ADME profile of bioactive compounds. The study assessed the usefulness of computational and chromatographic methods (thin-layer chromatography in a reversed-phase system, RP-TLC) for estimating the lipophilicity of 21 newly synthesized compounds belonging to diquinothiazines and quinonaphthiazines. In order to obtain reliable values of the relative lipophilicities of diquinothiazines and quinonaphthiazines, the partition coefficients obtained using different algorithms such as AlogPs, AClogP, AlogP, MLOGP, XLOGP2, XLOGP3, logP, and ClogP were compared with the chromatographic RM0 values of all the tested compounds measured by the experimental RP-TLC method (logPTLC). Additionally, logPTLC values were also correlated with other descriptors, as well as the predicted ADME and drug safety profiling parameters. The linear correlations of logPTLC values of the tested compounds with other calculated molecular descriptors such as molar refractivity, as well as ADME parameters (Caco-2 substrates, P-gp inhibitors, CYP2C19, and CYP3A4) generally show poor predictive power. Therefore, in silico ADME profiling can only be helpful at the initial step of designing these new candidates for drugs. The compliance of all discussed diquinothiazines and naphthoquinothiazines with the rules of Lipinski, Veber, and Egan suggests that the tested pentacyclic phenothiazine analogs have a chance to become therapeutic drugs, especially orally active drugs.


Assuntos
Algoritmos , Citocromo P-450 CYP3A , Humanos , Células CACO-2 , Cromatografia em Camada Fina , Projetos de Pesquisa
5.
Int J Mol Sci ; 25(7)2024 Apr 03.
Artigo em Inglês | MEDLINE | ID: mdl-38612781

RESUMO

Poplars provide medicinal raw plant materials used in pharmacy. Leaf buds are one of the herbal medicinal products collected from poplars, having anti-inflammatory and antiseptic properties, but there are no quality standards for their production and there is a need to determine their botanical sources. Therefore, the chemical compositions of the leaf buds from four species and varieties of poplars, Populus balsamifera, P. × berolinensis, P. × canadensis 'Marilandica', and P. wilsonii were investigated and compared using gas chromatography coupled with mass detection (GC-MS) and two-dimensional high-performance thin-layer chromatography (2D-HPTLC) in order to search for taxa characterized by a high content of biologically active compounds and with a diverse chemical composition that determines their therapeutic effects. The presence of 163 compounds belonging to the groups of flavonoids, phenolic acids derivatives, glycerides, and sesquiterpenes was revealed. Moreover, the conditions for the separation and identification of biologically active compounds occurring in analyzed leaf buds using 2D-HPTLC were optimized and used for metabolomic profiling of the studied poplars, enabling their fast and simple botanical identification. The total phenolic (TPC) and flavonoid (TFC) contents of examined extracts were determined and their antioxidant capacities were estimated by spectrophotometric DPPH, ABTS, and FRAP assays. Based on the analysis of phytochemicals and antioxidant activity, P. × berolinensis buds were selected as the raw plant material for medicinal purposes with the highest content of active compounds and the strongest antioxidant activity.


Assuntos
Antioxidantes , Populus , Cromatografia em Camada Fina , Cromatografia Gasosa , Flavonoides , Folhas de Planta
6.
Sichuan Da Xue Xue Bao Yi Xue Ban ; 55(2): 425-432, 2024 Mar 20.
Artigo em Chinês | MEDLINE | ID: mdl-38645843

RESUMO

Objective: To establish quality standards for Liuwei Nengxiao pills, to optimize the quality control method, and to provide references for the quality control of Liuwei Nengxiao pills. Methods: Chebula, dried ginger, and Tibetan liqueur root in Liuwei Nengxiao pills of different batch numbers were analyzed by thin layer chromatography (TLC). Then, the content of chrysophanol in the preparation was determined by high performance liquid chromatography (HPLC). Furthermore, a series of methodological validation, including the investigation of the linear relationship, precision, stability, and reproducibility and sample recovery test, were performed to verify the reliability of the results. Results: The TLC identification method was easy to perform and demonstrated high specificity, clear spots, and good separation effect. In addition, the negative controls showed no interference. The HPLC method showed high accuracy. The results of methodological validation showed that the peak area of chrysophanol had a good linear relationship (r2=1.0) in the range of 0.06-0.80 µg, presenting good precision (with the relative standard deviation being lower than 2.0%), good stability and reproducibility (with the relative standard deviation being lower than 1.0%), and an average recovery rate of 100.8%. Conclusion: TLC and HPLC are easy to perform, showing high accuracy and reproducibility. The quality standards established are scientific, reasonable, stable, and feasible, providing references for the quality control of Liuwei Nengxiao pills.


Assuntos
Antraquinonas , Medicamentos de Ervas Chinesas , Medicina Tradicional Tibetana , Controle de Qualidade , Medicamentos de Ervas Chinesas/normas , Medicamentos de Ervas Chinesas/química , Cromatografia Líquida de Alta Pressão/métodos , Medicina Tradicional Tibetana/normas , Cromatografia em Camada Fina/métodos , Reprodutibilidade dos Testes
7.
Anal Methods ; 16(16): 2449-2455, 2024 Apr 25.
Artigo em Inglês | MEDLINE | ID: mdl-38563199

RESUMO

Carotenoids are yellow, orange, and red pigments commonly found in plants. In leaves, these molecules are essential for photosynthesis, but they also play a major role in plant growth and development. Efficiently monitoring concentrations of specific carotenoids in plant tissues could help to explain plant responses to environmental stressors, infection and disease, fertilization, and other conditions. Previously, Raman methods have been used to demonstrate a correlation between plant fitness and the carotenoid content of leaves. Due to solvatochromatic effects and structural similarities within the carotenoid family, current Raman spectroscopy techniques struggle to assign signals to specific carotenoids with certainty, complicating the determination of amounts of individual carotenoids present in a sample. In this work, we use thin layer chromatography-Raman spectroscopy, or TLC-Raman, to identify and quantify carotenoids extracted from tomato leaves. These quick and accurate methods could be applied to study the relationship between pigment content and a number of factors affecting plant health.


Assuntos
Carotenoides , Folhas de Planta , Solanum lycopersicum , Análise Espectral Raman , Folhas de Planta/química , Análise Espectral Raman/métodos , Cromatografia em Camada Fina/métodos , Carotenoides/análise , Carotenoides/química , Solanum lycopersicum/química , Solanum lycopersicum/metabolismo , Pigmentos Biológicos/análise , Pigmentos Biológicos/química
8.
Int J Mol Sci ; 25(8)2024 Apr 13.
Artigo em Inglês | MEDLINE | ID: mdl-38673898

RESUMO

The absolute configuration and stability of two thianthrene chiral sulfoxides has been determined by means of X-ray single-crystal structure determinations. The analyses and configurations allow verification that the diastereomeric sulfoxides are stable in solution and are not interconverting, which has been suggested in some studies of sulfoxides. The two thianthrene sulfoxides have slightly different Rf values, which allowed their separation using flash chromatography on silica. The spots run back-to-back, which posed a challenge for their separation. The pure, separated compounds in solution remain as separate, single spots on a Thin Layer Chromatography (TLC) plate.


Assuntos
Sulfóxidos , Estereoisomerismo , Sulfóxidos/química , Cristalografia por Raios X/métodos , Modelos Moleculares , Cromatografia em Camada Fina/métodos , Fenantrenos/química , Estrutura Molecular
9.
Molecules ; 29(8)2024 Apr 20.
Artigo em Inglês | MEDLINE | ID: mdl-38675702

RESUMO

The goal of this study was to apply the principles of analytical quality by design (AQbD) to the analytical method for determining the radiochemical purity (PQR) of the radiopharmaceutical sodium iodide 131I oral solution, utilizing thin-layer chromatography (TLC) with a radio-TLC scanner, which also enables the evaluation of product quality. For AQbD, the analytical target profile (ATP), critical quality attributes (CQA), risk management, and the method operable design region (MODR) were defined through response surface methodology to optimize the method using MINITAB® 19 software. This study encompassed the establishment of a control strategy and the validation of the method, including the assessment of selectivity, linearity, precision, robustness, detection limit, quantification limit, range, and the stability of the sample solution. Under the experimental conditions, the method parameters of the TLC scanner were experimentally demonstrated and optimized with an injection volume of 3 µL, a radioactive concentration of 10 mCi/mL, and a carrier volume of 40 µL. Statistical analysis confirmed the method's selectivity for the 131I iodide band Rf of 0.8, a radiochemical impurity IO3- Rf of 0.6, a linearity from 6.0 to 22.0 mCi/mL, and an intermediate precision with a global relative standard deviation (RSD) of 0.624%. The method also exhibited robustness, with a global RSD of 0.101%, a detection limit of 0.09 mCi/mL, and a quantification limit of 0.53 Ci/mL, meeting the prescribed range and displaying stability over time (at 0, 2, and 20 h) with a global RSD of 0.362%, resulting in consistent outcomes. The development of a method based on AQbD facilitated the creation of a design space and an operational space, with comprehensive knowledge of the method's characteristics and limitations. Additionally, throughout all operations, compliance with the acceptance criteria was verified. The method's validity was confirmed under the established conditions, making it suitable for use in the manufacturing process of sodium iodide 131I and application in nuclear medicine services.


Assuntos
Radioisótopos do Iodo , Compostos Radiofarmacêuticos , Iodeto de Sódio , Cromatografia em Camada Fina/métodos , Compostos Radiofarmacêuticos/química , Compostos Radiofarmacêuticos/análise , Radioisótopos do Iodo/análise , Iodeto de Sódio/química , Administração Oral , Reprodutibilidade dos Testes
10.
J Agric Food Chem ; 72(17): 10106-10116, 2024 May 01.
Artigo em Inglês | MEDLINE | ID: mdl-38629120

RESUMO

The authentication of ingredients in formulas is crucial yet challenging, particularly for constituents with comparable compositions but vastly divergent efficacy. Rehmanniae Radix and its derivatives are extensively utilized in food supplements, which contain analogous compositions but very distinct effects. Rehmanniae Radix, also a difficult-to-detect herbal ingredient, was chosen as a case to explore a novel HPTLC-QDa MS technique for the identification of herbal ingredients in commercial products. Through systematic condition optimization, including thin layer and mass spectrometry, a stable and reproducible HPTLC-QDa MS method was established, which can simultaneously detect oligosaccharides and iridoids. Rehmannia Radix and its processed products were then analyzed to screen five markers that could distinguish between raw and prepared Rehmannia Radix. An HPTLC-QDa-SIM method was further established for formula detection by using the five markers and validated using homemade prescriptions and negative controls. Finally, this method was applied to detect raw and prepared Rehmannia Radix in 12 commercial functional products and supplements.


Assuntos
Medicamentos de Ervas Chinesas , Rehmannia , Rehmannia/química , Cromatografia em Camada Fina/métodos , Medicamentos de Ervas Chinesas/química , Cromatografia Líquida de Alta Pressão/métodos , Raízes de Plantas/química , Suplementos Nutricionais/análise , Espectrometria de Massas/métodos , Oligossacarídeos/análise , Oligossacarídeos/química , Iridoides/análise , Iridoides/química
11.
Methods Mol Biol ; 2790: 427-438, 2024.
Artigo em Inglês | MEDLINE | ID: mdl-38649585

RESUMO

The biological role of lipids goes far beyond the formation of a structural membrane bilayer platform for membrane proteins and controlling fluxes across the membranes. For example, in photosynthetic thylakoid membranes, lipids occupy well-defined binding niches within protein complexes and determine the structural organization of membrane proteins and their function by controlling generic physicochemical membrane properties. In this chapter, two-dimensional thin-layer chromatography (2D TLC) and gas chromatography (GC) techniques are presented for quantitative analysis of lipid classes and fatty acids in thylakoid membranes. In addition, lipid extraction methods from isolated thylakoid membranes and leaves are described together with a procedure for the derivatization of fatty acids to fatty acid methyl esters (FAME) that is required for GC analysis.


Assuntos
Ácidos Graxos , Fotossíntese , Tilacoides , Tilacoides/metabolismo , Cromatografia em Camada Fina/métodos , Cromatografia Gasosa/métodos , Ácidos Graxos/metabolismo , Ácidos Graxos/química , Lipídeos de Membrana/metabolismo , Lipídeos de Membrana/química , Folhas de Planta/metabolismo , Folhas de Planta/química , Lipídeos/química , Lipídeos/isolamento & purificação , Lipídeos/análise
12.
Artigo em Inglês | MEDLINE | ID: mdl-38557311

RESUMO

Aleurites moluccanus (candlenut) and Bertholletia excelsa (Brazil nut) are marketed as dietary supplements for weight loss. These dietary supplements have been found to sometimes be adulterated with toxic nuts/seeds from Cascabela thevetia, commonly known as yellow oleander or lucky nut. This study emphasizes the key identification parameters to differentiate the genuine and adulterated nuts. Samples were obtained from authenticated sources of the nuts and from commercial sources of dietary supplements. This study examined 38 samples, including voucher and commercial samples. All eight commercial candlenut dietary supplement samples were adulterated. Additionally, two samples sold as Brazil nuts were also found to be adulterated. Other nuts were screened for the presence of Cardiac Glycosides, but none were found to be positive. The presence of yellow oleander was confirmed in all commercial dietary supplement samples marketed as candlenut as well as in commercial samples of Brazil nut. This study provides simple key identification characters using micro-morphology and histochemical localization of cardiac glycosides in the commercial nuts, HPTLC fingerprints, and LC-DAD-Q-ToF analytical parameters to detect and identify adulteration in commercial products.


Assuntos
Bertholletia , Suplementos Nutricionais , Suplementos Nutricionais/análise , Bertholletia/química , Contaminação de Alimentos/análise , Cromatografia em Camada Fina , Nozes/química , Cromatografia Líquida de Alta Pressão , Redução de Peso , Microscopia
13.
Chem Biodivers ; 21(5): e202301880, 2024 May.
Artigo em Inglês | MEDLINE | ID: mdl-38494456

RESUMO

This paper reports on some physicochemical and phytochemical characteristics (i. e. pH, electrical conductivity, colour, moisture content, total phenolic content, sugar profile) and in vitro antioxidant activity of honeys harvested from five legume species, red clover (Trifolium pratense), balansa clover (T. michelianum), Persian clover (T. resupinatum), purple clover (T. purpureum) and sanfoin, also known as holy clover (Onobrychis viciifolia), that were grown in enclosed shade houses to ensure that the honeys' characteristics are reflective of a truly monofloral honey. Glucose and fructose, determined via High-Performance Thin-Layer Chromatography (HPTLC) analysis, were found as the main sugars in all investigated honeys with the ratio of fructose to glucose ranging from 1 : 1.2 to 1 : 1.6. The honeys' pH values ranged from 3.9 to 4.6 which met Codes Alimentarius (CA) requirements. The moisture content was found to be between 17.6 and 22.2 % which in some cases was slightly higher than CA requirements (≤20 %). The honeys' colour values, prior and after filtration, were between 825.5-1149.5 mAU and 532.4-824.8 mAU respectively, illustrating golden yellow to deep yellow hues. The total phenolic content (TPC) of the honeys was determined using a modified Folin-Ciocalteu assay. Their antioxidant activity was captured by the Ferric Reducing-Antioxidant Power (FRAP) assay as well as HPTLC analysis coupled with 2,2-diphenyl-1-picrylhydrazyl (DPPH) derivatisation. The highest total phenolic content was found in red clover honey (45.4 mg GAE/100 g) whereas purple clover honey showed the highest level of activity in the FRAP assay (7.3 mmol Fe2+/kg). HPTLC-DPPH analysis of the honeys' organic extracts demonstrated the presence of various bioactive compounds that contribute to their overall antioxidant activity. This study developed a methodology for producing monofloral clover honeys in a space limited, enclosed production system, which allowed to collate important baseline data for these honeys that can serve as the foundation for their potential future development into commercial honeys, including honeys that can be used for medicinal purposes.


Assuntos
Antioxidantes , Mel , Compostos Fitoquímicos , Antioxidantes/química , Antioxidantes/farmacologia , Antioxidantes/análise , Mel/análise , Compostos Fitoquímicos/química , Compostos Fitoquímicos/farmacologia , Compostos Fitoquímicos/análise , Compostos Fitoquímicos/isolamento & purificação , Fenóis/análise , Fenóis/química , Concentração de Íons de Hidrogênio , Trifolium/química , Picratos/antagonistas & inibidores , Compostos de Bifenilo/antagonistas & inibidores , Cromatografia em Camada Fina
14.
Food Chem ; 448: 139025, 2024 Aug 01.
Artigo em Inglês | MEDLINE | ID: mdl-38522293

RESUMO

Monitoring of the accidental presence of gluten (Glu), resulting from cross-contamination, is imperative in different industries, in particular food industry. The objective of this study was the development of an analytical platform utilizing thin-layer chromatography (TLC) with colorimetric read-out for making binary (yes/no) decisions on surfaces and/or point of these industries. The composition of the extractive phase was optimized with commercial products used in cleaning processing lines. Subsequently, an exploration of TLC separation and detection was undertaken. CN-modified nanosilica plates and 30:70 acetonitrile:water were used to achieve a selective signal for Glu residues. The study of the detection performance showed that both spectroscopic measurement and image analysis were resulted in satisfactory results for quantitate analysis (RSD = 5 %, LOD = 0.12 mg). The practical application of the proposed methodology on surfaces of the food processing lines. This work demonstrated the operational feasibility in detecting gluten cross-contaminations within the food processing industry.


Assuntos
Colorimetria , Contaminação de Alimentos , Glutens , Contaminação de Alimentos/análise , Glutens/análise , Glutens/química , Colorimetria/métodos , Cromatografia em Camada Fina/métodos , Indústria Alimentícia
15.
J Pharm Biomed Anal ; 243: 116109, 2024 Jun 15.
Artigo em Inglês | MEDLINE | ID: mdl-38518458

RESUMO

An innovative ecofriendly high-performance thin layer chromatographic (HPTLC) method with spectrophotometric detection for simultaneous determination of Tramadol (TMD), Tapentadol (TAP), and Venlafaxine (VEN) in seized dosage forms was presented. Our method was conducted to achieve separation following the optimal conditions: pre-coated silica gel plates using a green mobile phase (heptane: acetone: ammonia, 7:3:0.5 v/v), with absorbance scanning at 272 nm. The validation of the method was done following International Conference on Harmonization (ICH) guidelines, demonstrates linearity, accuracy, precision, selectivity, robustness, and system suitability. Separation was achieved with a detection limit of 0.34, 0.16, and 0.084 (ug/band) for TMD, TAP, and VEN, respectively, the method successfully analyzes seized samples. Trueness is confirmed through a high degree of similarity between HPTLC and gas chromatography results. The study's ecofriendly approach, simplicity, and selectivity position it as a promising method for efficient, on-site monitoring of seized samples.


Assuntos
Tramadol , Tapentadol , Cloridrato de Venlafaxina , Cromatografia em Camada Fina/métodos , Preparações Farmacêuticas , Reprodutibilidade dos Testes
16.
Methods Mol Biol ; 2761: 149-157, 2024.
Artigo em Inglês | MEDLINE | ID: mdl-38427236

RESUMO

Chromatographic separation and purification of an individual lipid to homogeneity have long been introduced. Using this concept, a more precise method has been developed to identify and characterize the sphingolipid composition(s) using a small amount (30 mg) of biological sample. Sphingolipids (lipids containing sphingosine or dihydrosphingosine) are well-known regulators of the central nervous system development and play a critical role in neurodegenerative diseases. Introducing a silicic acid column chromatography, sphingolipid components have been separated to individual fractions such as ceramide, glucosyl/galactosylceramide, other neutral and acidic glycosphingolipids, including (dihydro)sphingosine and psychosine; as well as phospholipids from which individual components are quantified employing a single or combination of other advanced chromatography procedures such as thin-layer chromatography, gas chromatography-mass spectrometry, and high-performance liquid chromatography-mass spectrometry.


Assuntos
Esfingolipídeos , Esfingosina , Esfingolipídeos/química , Esfingosina/análise , Ceramidas/análise , Cromatografia em Camada Fina/métodos , Sistema Nervoso Central/química
17.
Food Chem ; 447: 138936, 2024 Jul 30.
Artigo em Inglês | MEDLINE | ID: mdl-38461717

RESUMO

Rhodamine B is a synthetic dye known to enhance the visual appearance of chili powder. Due to its toxicity and carcinogenicity, chromatographic methods have been developed to monitor its presence in adulterated chili powder, but their assays are laborious, time consuming and expensive for screening purposes. The present studies propose an alternative for screening Rhodamine B in chili powder samples. The method combines thin layer chromatography (TLC) to solid surface room-temperature fluorescence spectroscopy. The scrape-dissolution procedure common to the instrumental analysis of TLC procedures was replaced with a fiber optic probe coupled to a commercial spectrofluorometer. The determination of Rhodamine B on the chromatographic plate is based on its retardation factor and maximum excitation and emission wavelengths. The limit of detection (1.9 ng.mL-1) and the limit of quantitation (5.2 ng.mL-1) are well below the usual contamination of Rhodamine B in adulterated foods.


Assuntos
Pós , Rodaminas/análise , Cromatografia em Camada Fina
18.
Toxicon ; 239: 107634, 2024 Feb 23.
Artigo em Inglês | MEDLINE | ID: mdl-38307130

RESUMO

Plumbago scandens L. (Plumbaginaceae) occurs in all regions of Brazil. It has been described as toxic to cattle and goats. Caustic lesions in the upper digestive tract characterize poisoning. P. scandens contains a naphthoquinone named plumbagin, which presents high cytotoxic activity. Plumbago auriculata Lam., a widely used ornamental plant, is considered potentially toxic, but there is limited data about its toxicity. This work aimed to validate analytical methodologies for determining the levels of plumbagin in samples of leaves, stems, and rumen content to be used as an auxiliary chemical marker in the laboratory diagnosis of intoxication. One methodology used thin layer chromatography (TLC), and another used high-performance liquid chromatography (HPLC). The presence of palisade grass (Urochloa brizantha (Hochst. ex A.Rich.) R.D.Webster), Guinea grass (Megathyrsus maximus (Jacq.) B.K.Simon & S.W.L.Jacobs), corn silage, and rumen content did not interfere with plumbagin in the two methodologies. The TLC methodology generates qualitative results but is simple to implement and has a low cost. The HPLC methodology showed a limit of detection (LOD) of 0.01 µg/mL and a limit of quantification (LOQ) of 0.05 µg/mL. Leaf and stem samples of P. scandens evaluated showed high levels of plumbagin (0.261 ± 0.087 % and 0.327 ± 0.055 %, respectively). In contrast, leaves of P. auriculata did not show detectable levels of the toxin, and some stem samples showed low levels (up to 0.000114 %). Thus, these methodologies can be used to confirm or rule out the consumption of P. scandens in rumen content from animals suspected of poisoning.


Assuntos
Naftoquinonas , Plumbaginaceae , Animais , Bovinos , Cromatografia Líquida de Alta Pressão/métodos , Cromatografia em Camada Fina , Plumbaginaceae/química , Raízes de Plantas/química
19.
Molecules ; 29(3)2024 Feb 05.
Artigo em Inglês | MEDLINE | ID: mdl-38338474

RESUMO

Biological activities of six under-utilized medicinal leafy vegetable plants indigenous to Africa, i.e., Basella alba, Crassocephalum rubens, Gnetum africanum, Launaea taraxacifolia, Solanecio biafrae, and Solanum macrocarpon, were investigated via two independent techniques. The total phenolic content (TPC) was determined, and six microtiter plate assays were applied after extraction and fractionation. Three were antioxidant in vitro assays, i.e., ferric reducing antioxidant power (FRAP), cupric reduction antioxidant capacity (CUPRAC), and 2,2-diphenyl-1-picrylhydrazyl (DPPH) scavenging, and the others were enzyme (acetylcholinesterase, butyrylcholinesterase, and tyrosinase) inhibition assays. The highest TPC and antioxidant activity from all the methods were obtained from polar and medium polar fractions of C. rubens, S. biafrae, and S. macrocarpon. The highest acetyl- and butyrylcholinesterase inhibition was exhibited by polar fractions of S. biafrae, C. rubens, and L. taraxacifolia, the latter comparable to galantamine. The highest tyrosinase inhibition was observed in the n-butanol fraction of C. rubens and ethyl acetate fraction of S. biafrae. In vitro assay results of the different extracts and fractions were mostly in agreement with the bioactivity profiling via high-performance thin-layer chromatography-multi-imaging-effect-directed analysis, exploiting nine different planar assays. Several separated compounds of the plant extracts showed antioxidant, α-glucosidase, α-amylase, acetyl- and butyrylcholinesterase-inhibiting, Gram-positive/-negative antimicrobial, cytotoxic, and genotoxic activities. A prominent apolar bioactive compound zone was tentatively assigned to fatty acids, in particular linolenic acid, via electrospray ionization high-resolution mass spectrometry. The detected antioxidant, antimicrobial, antidiabetic, anticholinesterase, cytotoxic, and genotoxic potentials of these vegetable plants, in particular C. rubens, S. biafrae, and S. macrocarpon, may validate some of their ethnomedicinal uses.


Assuntos
Anti-Infecciosos , Plantas Medicinais , Antioxidantes/química , Butirilcolinesterase , Verduras , Cromatografia em Camada Fina , Acetilcolinesterase , Monofenol Mono-Oxigenase , Plantas Medicinais/química , Extratos Vegetais/farmacologia , Extratos Vegetais/química , Anti-Infecciosos/análise
20.
Biomed Chromatogr ; 38(4): e5831, 2024 Apr.
Artigo em Inglês | MEDLINE | ID: mdl-38291628

RESUMO

Mycotoxins are toxic mycological products that when consumed, absorbed or inhaled cause sickness or even the death of humans. Therefore, the present study aimed to evaluate the contamination levels of mycotoxins (aflatoxins, AFB1 , AFB2 , AFG1 , AFG2 , and ochratoxin A, OTA) in selected medicinal herbs and shrubs using thin-layer chromatography (TLC) and high-performance liquid chromatography (HPLC). A total of 15 samples of medicinal herbs and shrubs were selected. Among them, four samples were aflatoxin contaminated while two samples were ochratoxin A contaminated. The highest level of aflatoxin was detected in Justicia adhathoda (4,704.94 ppb) through HPLC (153.4 ppb) and through TLC, while the lowest level of aflatoxin was detected in Pegnum harmala (205.1 ppb) through HPLC. Similarly, the highest level of OTA was detected in Dodonia viscosa (0.53 ppb) through HPLC (0.5 ppb) and through TLC, while the lowest level was detected in J. adhathoda (O.11 ppb) through HPLC (0.4 ppb) and through TLC. The OTA concentration was very low, being negligible and below permissible limits. The present study concludes that there is a potential risk for the consumption of herbal decoctions. Therefore, regular monitoring and proper management of mycotoxins, including aflatoxins and OTA, in herbal medicines are needed to ensure the safety of herbal drugs to protect consumers.


Assuntos
Aflatoxinas , Micotoxinas , Plantas Medicinais , Humanos , Micotoxinas/análise , Aflatoxinas/análise , Cromatografia em Camada Fina , Cromatografia Líquida de Alta Pressão/métodos , Contaminação de Alimentos/análise
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