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1.
Sensors (Basel) ; 24(6)2024 Mar 20.
Artigo em Inglês | MEDLINE | ID: mdl-38544236

RESUMO

Caffeine is the most widely consumed stimulant and is the subject of significant ongoing research and discussions due to its impact on human health. The industry's need to comply with country-specific food and beverage regulations underscores the importance of monitoring caffeine levels in commercial products. In this study, we propose an alternative technique for caffeine analysis that relies on mid-infrared laser-based photothermal spectroscopy (PTS). PTS exploits the high-power output of the quantum cascade laser (QCL) sources to enhance the sensitivity of the mid-IR measurement. The laser-induced thermal gradient in the sample scales with the analytes' absorption coefficient and concentration, thus allowing for both qualitative and quantitative assessment. We evaluated the performance of our experimental PTS spectrometer, incorporating a tunable QCL and a Mach-Zehnder interferometer, for detecting caffeine in coffee, black tea, and an energy drink. We calibrated the setup with caffeine standards (0.1-2.5 mg mL-1) and we benchmarked the setup's capabilities against gas chromatography (GC) and Fourier-transform infrared (FTIR) spectroscopy. Quantitative results aligned with GC analysis, and limits of detection matched the research-grade FTIR spectrometer, indicating an excellent performance of our custom-made instrument. This method offers an alternative to established techniques, providing a platform for fast, sensitive, and non-destructive analysis without consumables as well as with high potential for miniaturization.


Assuntos
Bebidas , Cafeína , Humanos , Cafeína/análise , Espectrofotometria Infravermelho , Espectroscopia de Infravermelho com Transformada de Fourier/métodos , Bebidas/análise , Lasers Semicondutores
2.
Spectrochim Acta A Mol Biomol Spectrosc ; 313: 124124, 2024 May 15.
Artigo em Inglês | MEDLINE | ID: mdl-38460230

RESUMO

Derivative spectroscopy is used to separate the small absorption peaks superimposed on the main absorption band, which is widely adopted in modern spectral analysis to increase both the valid spectral information and the identification accuracy. In this study, a method based on attenuated total reflectance-Fourier transform infrared spectroscopy (ATR-FTIR) with first-order derivative (FD) processing combined with chemometrics is proposed for rapid qualitative and quantitative analysis of Panax ginseng polysaccharides (PGP), Panax notoginseng polysaccharides (PNP), and Panax quinquefolius polysaccharides (PQP). First, ATR-FTIR with FD processing was used to establish the discriminant model combined with principal component analysis (PCA), partial least squares discriminant analysis (PLS-DA) and linear discriminant analysis (LDA). After that, two-dimensional ATR-FTIR based on single-characteristic temperature as external interference (2D-sATR-FTIR) was established using ATR-FTIR with FD processing. Then, ATR-FTIR with FD processing was combined with PLS to establish and optimize the quantitative regression model. Finally, the established discriminant model and 2D-sATR-FTIR successfully distinguished PGP, PNP and PQP, and the optimal PLS regression model had a good prediction ability for the Panax polysaccharide extracts content. This strategy provides an efficient, economical and nondestructive method for the distinction and quantification of PGP, PNP and PQP in a short detection time.


Assuntos
Panax notoginseng , Espectroscopia de Infravermelho com Transformada de Fourier/métodos , Análise Discriminante , Análise dos Mínimos Quadrados , Polissacarídeos
3.
Int J Pharm ; 655: 123997, 2024 Apr 25.
Artigo em Inglês | MEDLINE | ID: mdl-38484861

RESUMO

The superior flexibility, efficient drug loading, high surface-to-volume ratio, ease of formulation, and cost-controlled production are considered exceptional advantages of nanofibers (NFs) as a smart delivery system. Deflazacort (DEF) is an anti-inflammatory and immunosuppressant agent. It is categorized as a poorly soluble class II drug. In this study, DEF-loaded polymeric nanofibrous using the electrospinning technique mats, Polyvinyl pyrrolidone (PVP) with or without Poloxamer 188 (PX) were used as mat-forming polymers. Microscopical imaging, drug content (%), and in vitro dissolution studies were conducted for all NFs formulae (F1-F7). All NFs improved the DEF dissolution compared to the unprocessed form, with the superiority of the PVP/PX hybrid. The optimized formula (F7) exhibited an average diameter of 655.46 ± 90.4 nm and % drug content of 84.33 ± 5.58. The dissolution parameters of DEF loaded in PVP/PX NFs (F7) reflected a release of 95.3 % ± 3.1 and 102.6 % ± 1.7 after 5 and 60 min, respectively. NFs (F7) was investigated for drug-polymer compatibility using Fourier-Transform Infrared Spectroscopy (FTIR), Powder X-ray diffraction analysis (PXRD), and Differential Scanning Calorimetry (DSC). In vivo anti-inflammatory study employing male Sprague-Dawley rats showed a significant reduction of rat paw edema for F7 (p < 0.05) compared with unprocessed DEF with a normal epidermal and dermal skin structure comparable to the healthy negative control. Immunohistochemical and morphometric data displayed similarities between the immune reaction of F7 and the negative healthy control. The finding of this work emphasized that DEF loaded in PVP/PX NFs could be considered a useful strategy for enhancing the therapeutic performance of DEF.


Assuntos
Nanofibras , Povidona , Pregnenodionas , Masculino , Ratos , Animais , Povidona/química , Polivinil , Poloxâmero , Nanofibras/química , Solubilidade , Ratos Sprague-Dawley , Polímeros/química , Espectroscopia de Infravermelho com Transformada de Fourier/métodos , Anti-Inflamatórios , Varredura Diferencial de Calorimetria
4.
Molecules ; 29(5)2024 Feb 20.
Artigo em Inglês | MEDLINE | ID: mdl-38474435

RESUMO

Cervical cancer was considered the fourth most common cancer worldwide in 2020. In order to reduce mortality, an early diagnosis of the tumor is required. Currently, this type of cancer occurs mostly in developing countries due to the lack of vaccination and screening against the Human Papillomavirus. Thus, there is an urgent clinical need for new methods aiming at a reliable screening and an early diagnosis of precancerous and cancerous cervical lesions. Vibrational spectroscopy has provided very good results regarding the diagnosis of various tumors, particularly using Fourier transform infrared microspectroscopy, which has proved to be a promising complement to the currently used histopathological methods of cancer diagnosis. This spectroscopic technique was applied to the analysis of cryopreserved human cervical tissue samples, both squamous cell carcinoma (SCC) and non-cancer samples. A dedicated Support Vector Machine classification model was constructed in order to categorize the samples into either normal or malignant and was subsequently validated by cross-validation, with an accuracy higher than 90%.


Assuntos
Carcinoma de Células Escamosas , Neoplasias do Colo do Útero , Feminino , Humanos , Carcinoma de Células Escamosas/patologia , Neoplasias do Colo do Útero/patologia , Espectroscopia de Infravermelho com Transformada de Fourier/métodos
5.
Langmuir ; 40(11): 5858-5868, 2024 Mar 19.
Artigo em Inglês | MEDLINE | ID: mdl-38445553

RESUMO

Throughout bioprocessing, transportation, and storage, therapeutic monoclonal antibodies (mAbs) experience stress conditions that may cause protein unfolding and/or chemical modifications. Such structural changes may lead to the formation of aggregates, which reduce mAb potency and may cause harmful immunogenic responses in patients. Therefore, aggregates need to be detected and removed or ideally prevented from forming. Air-liquid interfaces, which arise during various stages of bioprocessing, are one of the stress factors causing mAb aggregation. In this study, the behavior of an immunoglobulin G (IgG) at the air-liquid interface was investigated under flow using macro attenuated total reflection Fourier transform infrared (ATR-FTIR) spectroscopic imaging. This chemically specific imaging technique allows observation of adsorption of IgG to the air-liquid interface and detection of associated secondary structural changes. Chemical images revealed that IgG rapidly accumulated around an injected air bubble under flow at 45 °C; however, no such increase was observed at 25 °C. Analysis of the second derivative spectra of IgG at the air-liquid interface revealed changes in the protein secondary structure associated with increased intermolecular ß-sheet content, indicative of aggregated IgG. The addition of 0.01% w/v polysorbate 80 (PS80) reduced the amount of IgG at the air-liquid interface in a static setup at 30 °C; however, this protective effect was lost at 45 °C. These results suggest that the presence of air-liquid interfaces under flow may be detrimental to mAb stability at elevated temperatures and demonstrate the power of ATR-FTIR spectroscopic imaging for studying the structural integrity of mAbs under bioprocessing conditions.


Assuntos
Anticorpos Monoclonais , Imunoglobulina G , Humanos , Anticorpos Monoclonais/química , Espectroscopia de Infravermelho com Transformada de Fourier/métodos , Estrutura Secundária de Proteína , Imunoglobulina G/química , Desdobramento de Proteína , Proteínas Mutadas de Ataxia Telangiectasia
6.
AAPS PharmSciTech ; 25(4): 67, 2024 Mar 22.
Artigo em Inglês | MEDLINE | ID: mdl-38519767

RESUMO

Despite being discovered over five decades ago, little is still known about ivermectin. Ivermectin has several physico-chemical properties that can result in it having poor bioavailability. In this study, polymorphic and co-crystal screening was used to see if such solid-state modifications can improve the oil solubility of ivermectin. Span® 60, a lipophilic non-ionic surfactant, was chosen as co-former. The rationale behind attempting to improve oil solubility was to use ivermectin in future topical and transdermal preparations to treat a range of skin conditions like scabies and head lice. Physical mixtures were also prepared in the same molar ratios as the co-crystal candidates, to serve as controls. Solid-state characterization was performed using X-ray powder diffraction (XRPD), Fourier-transform infrared spectroscopy (FTIR), differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA). The FTIR spectra of the co-crystal candidates showed the presence of Span® 60's alkyl chain peaks, which were absent in the spectra of the physical mixtures. Due to the absence of single-crystal X-ray data, co-crystal formation could not be confirmed, and therefore these co-crystal candidates were referred to as co-processed crystalline solids. Following characterization, the solid-state forms, physical mixtures and ivermectin raw material were dissolved in natural penetration enhancers, i.e., avocado oil (AVO) and evening primrose oil (EPO). The co-processed solids showed increased oil solubility by up to 169% compared to ivermectin raw material. The results suggest that co-processing of ivermectin with Span® 60 can be used to increase its oil solubility and can be useful in the development of oil-based drug formulations.


Assuntos
Ivermectina , Óleos , Solubilidade , Difração de Raios X , Composição de Medicamentos , Varredura Diferencial de Calorimetria , Espectroscopia de Infravermelho com Transformada de Fourier/métodos
7.
Spectrochim Acta A Mol Biomol Spectrosc ; 313: 124142, 2024 May 15.
Artigo em Inglês | MEDLINE | ID: mdl-38493515

RESUMO

In this work, we investigated the oxidative stress-related biochemical alterations in red blood cells (RBCs) and their membranes with the use of spectroscopic techniques. We aimed to show their great advantage for the in situ detection of lipid classes and secondary structures of proteins without the need for their extraction in the cellular environment. The exposition of the cells to peroxides, t-butyl hydroperoxide (tBOOH) or hydrogen peroxide (H2O2) led to different degradation processes encompassing the changes in the composition of membranes and structural modifications of hemoglobin (Hb). Our results indicated that tBOOH is generally a stronger oxidizing agent than H2O2 and this observation was congruent with the activity of superoxide and glutathione peroxidase. ATR-FTIR and Raman spectroscopies of membranes revealed that tBOOH caused primarily the partial loss and peroxidation of the lipids resulting in loss of the integrity of membranes. In turn, both peroxides induced several kinds of damage in the protein layer, including the partial decrease of their content and irreversible aggregation of spectrin, ankyrin, and membrane-bound globin. These changes were especially pronounced on the membrane surface where stress conditions induced the formation of ß-sheets and intramolecular aggregates, particularly for tBOOH. Interestingly, nano-FTIR spectroscopy revealed the lipid peroxidative damage on the membrane surface in both cases. As far as hemoglobin was concerned, tBOOH and H2O2 caused the increase of the oxyhemoglobin species and conformational alterations of its polypeptide chain into ß-sheets. Our findings confirm that applied spectroscopies effectively track the oxidative changes occurring in the structural components of red blood cells and the simplicity of conducting measurements and sample preparation can be readily applied to pharmacological and clinical studies.


Assuntos
Eritrócitos , Peróxido de Hidrogênio , Humanos , Peróxido de Hidrogênio/farmacologia , Peróxido de Hidrogênio/metabolismo , Eritrócitos/metabolismo , Hemoglobinas/metabolismo , Peróxidos/farmacologia , Espectroscopia de Infravermelho com Transformada de Fourier/métodos , Lipídeos , Estresse Oxidativo
8.
J Hazard Mater ; 469: 133874, 2024 May 05.
Artigo em Inglês | MEDLINE | ID: mdl-38430588

RESUMO

This study presents a possible application of Fourier transform infrared (FTIR) spectrometry and multivariate data analysis, principal component analysis (PCA), and partial least squares-discriminant analysis (PLS-DA) for classifying asbestos and their nonasbestiform analogues. The objectives of the study are: 1) to classify six regulated asbestos types and 2) to classify between asbestos types and their nonasbestiform analogues. The respirable fraction of six regulated asbestos types and their nonasbestiform analogues were prepared in potassium bromide pellets and collected on polyvinyl chloride membrane filters for FTIR measurement. Both PCA and PLS-DA classified asbestos types and their nonasbestiform analogues on the score plots showed a very distinct clustering of samples between the serpentine (chrysotile) and amphibole groups. The PLS-DA model provided ∼95% correct prediction with a single asbestos type in the sample, although it did not provide all correct predictions for all the challenge samples due to their inherent complexity and the limited sample number. Further studies are necessary for a better prediction level in real samples and standardization of sampling and analysis procedures.


Assuntos
Amianto , Espectroscopia de Infravermelho com Transformada de Fourier/métodos , Análise de Fourier , Análise Multivariada , Análise Discriminante , Asbestos Serpentinas , Análise dos Mínimos Quadrados
9.
Sensors (Basel) ; 24(4)2024 Feb 09.
Artigo em Inglês | MEDLINE | ID: mdl-38400318

RESUMO

By focusing our attention on nitrogen components in plants, which are important for cultivation management in data-driven agriculture, we developed a simple, rapid, non-chemical and simultaneous quantification method for proteinic and nitrate nitrogen in a leaf model based on near-infrared (NIR) spectroscopic information obtained using a compact Fourier Transform NIR (FT-NIR) spectrometer. The NIR spectra of wet leaf models impregnated with a protein-nitric acid mixed solution and a dry leaf model obtained by drying filter paper were acquired. For spectral acquisition, a compact MEMS (Micro Electro Mechanical Systems) FT-NIR spectrometer equipped with a diffuse reflectance probe accessory was used. Partial least square regression analysis was performed using the spectral information of the extracted absorption bands based on the determination coefficients between the spectral absorption intensities and the contents of the two-dimensional spectral analysis between NIR and mid-infrared spectral information. Proteinic nitrogen content in the dry leaf model was well predicted using the MEMS FT-NIR spectroscopic method. Additionally, nitrate nitrogen in the dry leaf model was also determined by the provided method, but the necessity of adding the data for a wider range of nitric acid concentrations was experimentally indicated for the prediction of nitrate nitrogen content in the wet leaf model. Consequently, these results experimentally suggest the possibility of the application of the compact MEMS FT-NIR for obtaining the bioinformation of crops at agricultural on-sites.


Assuntos
Nitratos , Nitrogênio , Ácido Nítrico , Espectroscopia de Luz Próxima ao Infravermelho/métodos , Análise dos Mínimos Quadrados , Proteínas , Folhas de Planta , Espectroscopia de Infravermelho com Transformada de Fourier/métodos
10.
Spectrochim Acta A Mol Biomol Spectrosc ; 311: 123998, 2024 Apr 15.
Artigo em Inglês | MEDLINE | ID: mdl-38340448

RESUMO

As2O3 has shown significant anti-gastric cancer effects, but the mechanism is still unclear. Thus, biomacromolecular changes induced by As2O3 were investigated by using human gastric cancer AGS cells as the model. Flow cytometry results confirmed that As2O3 induced AGS cells apoptosis. Fourier transform infrared (FTIR) microspectroscopy detected biomacromolecular changes during As2O3-induced AGS cells apoptosis sensitively: IR spectra showed significant changes in the lipids content and the proteins and DNA structure. Peak-area ratios indicated obvious changes in the lipids and DNA content and the proteins structure, while also showing a relatively good linear relationship between A1733/A969 and the apoptosis rate. PCA exhibited significant alteration in nucleic acids while curve fitting further revealed the changes in nucleic acids and proteins. On the whole, our study explored As2O3-induced gastric cancer cells apoptosis in depth on the basis of analyzing biomacromolecular changes, in addition, it also suggested FTIR microspectroscopy to be possibly useful in the research of apoptosis.


Assuntos
Antineoplásicos , Arsenicais , Neoplasias Gástricas , Humanos , Espectroscopia de Infravermelho com Transformada de Fourier/métodos , Análise de Fourier , Apoptose , DNA/química , Linhagem Celular Tumoral , Proteínas , Lipídeos/farmacologia , Óxidos/farmacologia , Antineoplásicos/farmacologia
11.
Naturwissenschaften ; 111(1): 9, 2024 Feb 11.
Artigo em Inglês | MEDLINE | ID: mdl-38342817

RESUMO

This article presents an attempt to discriminate between human male and female hair samples using a single strand of scalp hair. The methodology involves the non-destructive application of ATR-FTIR spectroscopy coupled with chemometric analysis. A total of 96 hair samples, evenly distributed between 48 male and 48 female volunteers from India, were collected. Spectral analysis revealed subtle differences between the two groups, and reliance on visual interpretation might introduce biasness. To avoid subjective biases, chemometric techniques such as principal component analysis (PCA) and partial least square-discriminant analysis (PLS-DA) were employed for enhanced data visualization and separation. PCA results revealed that the first 10 principal components accounted for 93% of the total variance, with three significant PCs. The PLS-DA model demonstrated a remarkable sensitivity and specificity in sex discrimination from hair samples, establishing its efficacy as a robust classification tool. Furthermore, the proposed model exhibited 100% accuracy in predicting unknown samples, underscoring its potential applicability in real-world scenarios. These outcomes affirm the viability of our approach for non-invasive classification of human male and female hair based on single-strand scalp hair analysis.


Assuntos
Quimiometria , Cabelo , Humanos , Masculino , Feminino , Espectroscopia de Infravermelho com Transformada de Fourier/métodos , Análise Discriminante , Cabelo/química , Análise de Componente Principal , Proteínas Mutadas de Ataxia Telangiectasia/análise
12.
Food Chem ; 442: 138604, 2024 Jun 01.
Artigo em Inglês | MEDLINE | ID: mdl-38306767

RESUMO

Katsuobushi, a smoked, dried skipjack tuna, is a traditional Japanese food additive with a unique flavor and taste. Gas chromatography mass spectrometry (GC-MS), fourier transform infrared (FTIR), and ultraviolet-visible-near infrared spectroscopy (UV-Vis-NIR) combined with chemometric methods were evaluated the quality of katsuobushi according to the number of smoking treatments. Using GC-MS, 46 metabolites were identified and five metabolites were selected as key compounds. All samples were classified according to their smoking number via principal component analysis (PCA), partial least squares-discriminate analysis (PLS-DA) and hierarchical cluster analysis (HCA) of the FTIR and NIR spectra. Partial least squares regression (PLSR) analysis revealed that the FTIR and NIR spectra were highly correlated with the metabolites by GC-MS. These results demonstrated the potential of using the FTIR and NIR spectroscopy combined with chemometrics to assess the quality of katsuobushi based on the smoking treatments, with NIR spectroscopy showed particularly promising.


Assuntos
Quimiometria , Espectroscopia de Luz Próxima ao Infravermelho , Espectroscopia de Luz Próxima ao Infravermelho/métodos , Espectroscopia de Infravermelho com Transformada de Fourier/métodos , Análise por Conglomerados , Fumar , Análise dos Mínimos Quadrados
13.
Spectrochim Acta A Mol Biomol Spectrosc ; 312: 124012, 2024 May 05.
Artigo em Inglês | MEDLINE | ID: mdl-38364451

RESUMO

Polyhydroxyalkanoate (PHA) is a family of naturally-occurring biopolymers synthesized by more than 300 microorganisms in the environment. These biopolymers have been investigated as a source material to substitute fossil fuel-based polymers; hence the synthesis of biopolymers and their characterization is a critical step in optimizing the process. Because of this, the biological production of PHA using PHA-producing microorganisms is currently the dominating process; however, the use of microbial mixed culture (MMC), such as wastewater sludge, is gaining attention. Different than pure cultures, MMC has higher culturing condition tolerance since the complex species composition and is easily obtained from wastewater treatment plants, which shortens the culturing time, lowers the cost, and promotes the application. The main constraint in MMC-based PHA is the extraction and quantification of PHA from the more complex matrix. In this paper, Fourier-transform infrared (FTIR) spectroscopy is evaluated to be used as a quantification method of PHA in MMC systems. Firstly, commercially available analytical standards, which consist of PHA/PHB, and two different solvents (chloroform and dichloromethane), were used and tested by this method, with KBr card and liquid cell methods, and the results are validated by gas chromatography mass spectrometry (GC/MS). The method was then tested using 12 samples from wastewater treatment plants. The PHA content in biomass varied from 3.42 w/w% to 1.22 w/w% following extraction with chloroform as solvent as determined by this method. In the four different combination standards, the best one is consisted of PHB and chloroform, and FTIR-liquid cell showed higher promise for PHA quantification in complex matrices.


Assuntos
Poli-Hidroxialcanoatos , Águas Residuárias , Esgotos/química , Poli-Hidroxialcanoatos/análise , Espectroscopia de Infravermelho com Transformada de Fourier/métodos , Clorofórmio , Reatores Biológicos , Biopolímeros
14.
Analyst ; 149(6): 1799-1806, 2024 Mar 11.
Artigo em Inglês | MEDLINE | ID: mdl-38385553

RESUMO

Pancreatic cancer, particularly Pancreatic ductal adenocarcinoma, remains a highly lethal form of cancer with limited early diagnosis and treatment options. Infrared (IR) spectroscopy, combined with machine learning, has demonstrated great potential in detecting various cancers. This study explores the translation of a diagnostic model from Fourier Transform Infrared to Quantum Cascade Laser (QCL) microscopy for pancreatic cancer classification. Furthermore, QCL microscopy offers faster measurements with selected frequencies, improving clinical feasibility. Thus, the goals of the study include establishing a QCL-based model for pancreatic cancer classification and creating a fast surgical margin detection model using reduced spectral information. The research involves preprocessing QCL data, training Random Forest (RF) classifiers, and optimizing the selection of spectral features for the models. Results demonstrate successful translation of the diagnostic model to QCL microscopy, achieving high predictive power (AUC = 98%) in detecting cancerous tissues. Moreover, a model for rapid surgical margin recognition, based on only a few spectral frequencies, is developed with promising differentiation between benign and cancerous regions. The findings highlight the potential of QCL microscopy for efficient pancreatic cancer diagnosis and surgical margin detection within clinical timeframes of minutes per surgical resection tissue.


Assuntos
Margens de Excisão , Neoplasias Pancreáticas , Humanos , Espectroscopia de Infravermelho com Transformada de Fourier/métodos , Microscopia/métodos , Neoplasias Pancreáticas/diagnóstico por imagem , Biópsia
15.
Food Chem ; 444: 138631, 2024 Jun 30.
Artigo em Inglês | MEDLINE | ID: mdl-38325079

RESUMO

Naringenin (NGE), a typical flavanone abundant in citrus fruits, exhibits remarkable antioxidant activities. However, its low solubility in oil restricts its widespread use in inhibiting lipid oxidation. In this study, we present a novel and effective approach to address this limitation by developing a naringenin-phospholipid complex (NGE-PC COM). Comprehensive analytical techniques including Fourier transform infrared (FTIR), differential scanning calorimetry (DSC), and X-ray diffraction (XRD) were employed to confirm the formation of the NGE-PC COM and elucidate the interaction mechanism between NGE and phospholipids molecules. Notably, the oil-solubility of NGE was significantly enhanced by approximately 2700-fold when formulated as a phospholipid complex in soybean oil. The improved oil-solubility of NGE-PC COM enabled effective inhibition of oil thermal oxidation under high temperature conditions. Generally, this investigation proposed a novel and promising strategy for employing flavanones with strong antioxidant activities to enhance the thermal oxidative stability of edible oil during heating processes.


Assuntos
Flavanonas , Fosfolipídeos , Fosfolipídeos/química , Óleo de Soja , Antioxidantes , Calefação , Flavanonas/química , Solubilidade , Estresse Oxidativo , Varredura Diferencial de Calorimetria , Espectroscopia de Infravermelho com Transformada de Fourier/métodos , Difração de Raios X
16.
J Pharm Biomed Anal ; 241: 115991, 2024 Apr 15.
Artigo em Inglês | MEDLINE | ID: mdl-38301577

RESUMO

In this study there were utilized a combination of Fourier transform infrared spectroscopy in attenuated total reflection mode (ATR-FTIR) and partial least squares (PLS) regression method to develop quantitative models for determining the concentration of ademetionine in commercial tablets. The established and validated models were specifically designed for a commercial product containing ademetionine 1,4-butandiesulfonate. The coefficient of determination for the developed model was 0.999. Relative standard deviation (RSD) does not exceed 1.6% for repeatability and intermediate accuracy, which meets the international ICH and AOAC requirements for the method performance. The validation results effectively confirmed that this method is suitable and meets the current requirements for analytical methods in drug quality control. Consequently, this approach can be used for routine ademetionine analysis in pharmaceutical products and has the potential to be applied to other active pharmaceutical ingredients (APIs) in drug quality control.


Assuntos
S-Adenosilmetionina , Espectroscopia de Infravermelho com Transformada de Fourier/métodos , Análise dos Mínimos Quadrados , Comprimidos , Controle de Qualidade
17.
Anal Methods ; 16(8): 1272-1280, 2024 Feb 22.
Artigo em Inglês | MEDLINE | ID: mdl-38323628

RESUMO

The determination of the time of an injury has been a major problem in forensic science due to the lack of objective, reliable and portable methods. In this study, a subcutaneous hemorrhage model in rats was established over six days, and attenuated total reflection-Fourier transform infrared (ATR-FTIR) spectroscopy coupled with chemometrics was used to determine the time since injury. Initial principal component analysis (PCA) showed variance among hematoma sites. Subsequently, spectral data were acquired to establish a dependable partial least square (PLS) regression model with predictive abilities. The root mean square error of cross-validation (RMSECV) and the root mean square error of prediction (RMSEP) values produced by a genetic algorithm (GA) were 0.64 d (R2 = 0.88) and 0.57 d (R2 = 0.90), respectively. Few variables were involved in the model, and significantly better results were obtained in comparison to the conventional full-spectrum PLS model. In combination with the results of variable importance in projection (VIP) scores, all components, including proteins, nucleic acids and phospholipids, provided inferences regarding the samples at different time points; additionally, amide I and II bands represented the secondary structure of proteins and provided the largest contribution. Based on our preliminary study, the combination of swift and nondamaging ATR-FTIR spectroscopy with chemometrics could prove to be an advantageous approach for gauging the age of an injury in the forensic field.


Assuntos
Fosfolipídeos , Proteínas , Animais , Ratos , Espectroscopia de Infravermelho com Transformada de Fourier/métodos , Análise dos Mínimos Quadrados , Análise de Componente Principal
18.
Eur J Pharm Biopharm ; 196: 114202, 2024 Mar.
Artigo em Inglês | MEDLINE | ID: mdl-38309539

RESUMO

The crystal structure of a new Progesterone (PROG) co-crystal with para-aminobenzoic acid (PABA) showing enhanced solution properties is reported. PROG-PABA co-crystal was first identified though an in silico coformer screening process using the CSD Co-crystal deign function, then confirmed through a solution evaporation crystallisation experiment. The resulting co-crystal was characterized using single crystal X-ray diffraction, differential scanning calorimetry and Fourier-transform infrared spectroscopy. Liquid assisted grinding was selected as a suitable scale up method compared to spray drying and antisolvent methods due to minimal starting material phases in the final product. Following scale up, aqueous solubility, stability and dissolution measurements were carried out. PROG-PABA showed increased distinct aqueous solubility and dissolution compared to PROG starting material and was shown to be stable at 75 % relative humidity for 3 months. Tablets containing co-crystal were produced then compared to the Utrogestan® soft gel capsule formulation through a dissolution experiment. PROG-PABA tablets showed a substantial increase in dissolution over the course of the experiment with over 30× the amount of PROG dissolved at the 3-hour time point. This co-crystal shows positive implications for developing an improved oral PROG formulation.


Assuntos
Ácido 4-Aminobenzoico , Progesterona , Progesterona/química , Cristalografia por Raios X , Solubilidade , Cristalização/métodos , Varredura Diferencial de Calorimetria , Difração de Raios X , Espectroscopia de Infravermelho com Transformada de Fourier/métodos
19.
Sensors (Basel) ; 24(3)2024 Jan 31.
Artigo em Inglês | MEDLINE | ID: mdl-38339641

RESUMO

Edible insects have been recognised as an alternative food or feed ingredient due to their protein value for both humans and domestic animals. The objective of this study was to evaluate the ability of both near- (NIR) and mid-infrared (MIR) spectroscopy to identify and quantify the level of adulteration of cricket powder added into two plant proteins: chickpea and flaxseed meal flour. Cricket flour (CKF) was added to either commercial chickpea (CPF) or flaxseed meal flour (FxMF) at different ratios of 95:5% w/w, 90:10% w/w, 85:15% w/w, 80:20% w/w, 75:25% w/w, 70:30% w/w, 65:35% w/w, 60:40% w/w, or 50:50% w/w. The mixture samples were analysed using an attenuated total reflectance (ATR) MIR instrument and a Fourier transform (FT) NIR instrument. The partial least squares (PLS) cross-validation statistics based on the MIR spectra showed that the coefficient of determination (R2CV) and the standard error in cross-validation (SECV) were 0.94 and 6.68%, 0.91 and 8.04%, and 0.92 and 4.33% for the ALL, CPF vs. CKF, and FxMF vs. CKF mixtures, respectively. The results based on NIR showed that the cross-validation statistics R2CV and SECV were 0.95 and 3.16%, 0.98 and 1.74%, and 0.94 and 3.27% using all the samples analyzed together (ALL), the CPF vs. CKF mixture, and the FxMF vs. CKF mixture, respectively. The results of this study showed the effect of the matrix (type of flour) on the PLS-DA data in both the classification results and the PLS loadings used by the models. The different combination of flours (mixtures) showed differences in the absorbance values at specific wavenumbers in the NIR range that can be used to classify the presence of CKF. Research in this field is valuable in advancing the application of vibrational spectroscopy as routine tools in food analysis and quality control.


Assuntos
Críquete , Farinha , Animais , Humanos , Farinha/análise , Pós , Análise Espectral/métodos , Análise de Alimentos , Análise dos Mínimos Quadrados , Espectroscopia de Infravermelho com Transformada de Fourier/métodos
20.
PLoS One ; 19(2): e0297467, 2024.
Artigo em Inglês | MEDLINE | ID: mdl-38394326

RESUMO

Glipizide, a poor water-soluble drug belongs to BCS class II. The proposed work aimed to enhance the solubility of glipizide by preparing solid dispersions, using polyvinyl pyrrolidone (PVP) and polyethylene glycol (PEG). Solvent evaporation method was used for the preparation of glipizide solid dispersions. Solid dispersions were prepared in four different drug-to-polymer ratios i.e. 1:1, 1:2, 1:3 and 1:4. Mainly effect of three polymers (PVP K30, PVP K90 and PEG 6000) was evaluated on the solubility and dissolution of glipizide. The in-vitro dissolution of all prepared formulations was performed under pH 6.8 at 37°C using USP type II apparatus. In-vitro dissolution results revealed that the formulations having high concentrations of the polymer showed enhanced solubility. Enhancements in the solubility and rate of dissolution of the drug were noted in solid dispersion formulations compared to the physical blends and pure drug. Solid dispersions containing polyvinyl pyrrolidone exhibited a more favorable pattern of drug release compared to the corresponding solid dispersions with PEG. An increase in the maximum solubility of the drug within the solid dispersion systems was observed in all instances. Two solid dispersion formulations were optimized and formulated into immediate-release tablets, which passed all the pharmacopoeial and non-pharmacopoeial tests. Fourier transformed Infrared (FTIR) spectroscopy X-ray diffraction (XRD) and Differential scanning calorimetry (DSC) were used to indicate drug: polymer interactions in solid state. Analysis of the solid dispersion samples through characterization tests indicated the compatibility between the drug and the polymer.


Assuntos
Glipizida , Polivinil , Solubilidade , Polímeros/química , Polietilenoglicóis/química , Espectroscopia de Infravermelho com Transformada de Fourier/métodos , Povidona/química , Difração de Raios X , Varredura Diferencial de Calorimetria
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