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1.
Pak J Pharm Sci ; 37(1(Special)): 245-255, 2024 Jan.
Article En | MEDLINE | ID: mdl-38747276

Aripiprazole (ARI), an antipsychotic having low solubility and stability. To overcome this, formation of binary and ternary using inclusion complexes of Methyl-ß-cyclodextrin (MßCD) /Hydroxy propyl beta cyclodextrin (HPßCD) and L-Arginine (ARG)/ Lysine (LYS) are analyzed by dissolution testing and phase stability study along with their complexation efficacy and solubility constants made by physical mixing. Inclusion complexes with ARG were better than LYS and prepared by solvent evaporation and lyophilization method as well. They are characterized by Attenuated Total Reflection Fourier Transform Infrared Spectroscopy (AT-FTIR), X-ray powder diffractometry (XRD), Differential Scanning Calorimetry (DSC), Scanning electron microscopy (SEM) and Thermal gravimetric analysis (TGA). The bond shifting in AT-FTIR confirmed the molecular interactions between host and guest molecules. The SEM images also confirmed a complete change of drug morphology in case of ternary inclusion complexes prepared by lyophilization method for both the polymers. ARI: MßCD: ARG when used in the specific molar ratio of 1:1:0.27 by prepared by lyophilization method has 18 times best solubility while ARI:HPßCD:ARG was 7 times best solubility than pure drug making MßCD a better choice than HPßCD. Change in the molar ratio will cause loss of stability or solubility. Solvent evaporation gave significant level of solubility but less stability.


2-Hydroxypropyl-beta-cyclodextrin , Arginine , Aripiprazole , Calorimetry, Differential Scanning , Lysine , Solubility , beta-Cyclodextrins , Aripiprazole/chemistry , Arginine/chemistry , beta-Cyclodextrins/chemistry , 2-Hydroxypropyl-beta-cyclodextrin/chemistry , Lysine/chemistry , Spectroscopy, Fourier Transform Infrared , X-Ray Diffraction , Freeze Drying , Antipsychotic Agents/chemistry , Drug Stability , Microscopy, Electron, Scanning , Drug Compounding , Chemistry, Pharmaceutical/methods
2.
Molecules ; 29(9)2024 Apr 23.
Article En | MEDLINE | ID: mdl-38731409

As a powerful imidazole antifungal drug, ketoconazole's low solubility (0.017 mg/mL), together with its odor and irritation, limited its clinical applications. The inclusion complex of ketoconazole with randomly methylated ß-cyclodextrin was prepared by using an aqueous solution method after cyclodextrin selection through phase solubility studies, complexation methods, and condition selection through single factor and orthogonal strategies. The complex was confirmed by FTIR (Fourier-transform infrared spectroscopy), DSC (differential scanning calorimetry), TGA (thermogravimetric analysis), SEM (scanning electron microscope images), and NMR (Nuclear magnetic resonance) studies. Through complexation, the water solubility of ketoconazole in the complex was increased 17,000 times compared with that of ketoconazole alone, which is the best result so far for the ketoconazole water solubility study. In in vitro pharmacokinetic studies, ketoconazole in the complex can be 100% released in 75 min, and in in vivo pharmacokinetic studies in dogs, through the complexation, the Cmax was increased from 7.56 µg/mL to 13.58 µg/mL, and the AUC0~72 was increased from 22.69 µgh/mL to 50.19 µgh/mL, indicating that this ketoconazole complex can be used as a more efficient potential new anti-fungal drug.


Antifungal Agents , Ketoconazole , Solubility , beta-Cyclodextrins , Ketoconazole/chemistry , Ketoconazole/pharmacokinetics , Ketoconazole/pharmacology , Ketoconazole/administration & dosage , beta-Cyclodextrins/chemistry , Animals , Antifungal Agents/pharmacology , Antifungal Agents/pharmacokinetics , Antifungal Agents/chemistry , Dogs , Calorimetry, Differential Scanning , Spectroscopy, Fourier Transform Infrared , Methylation
3.
BMC Oral Health ; 24(1): 551, 2024 May 11.
Article En | MEDLINE | ID: mdl-38734599

BACKGROUND: Periodontal diseases may benefit more from topical treatments with nanoparticles rather than systemic treatments due to advantages such as higher stability and controlled release profile. This study investigated the preparation and characterization of thermosensitive gel formulations containing clindamycin-loaded niosomes and solid lipid nanoparticles (SLNs) loaded with fluconazole (FLZ), as well as their in vitro antibacterial and antifungal effects in the treatment of common microorganisms that cause periodontal diseases. METHODS: This study loaded niosomes and SLNs with clindamycin and FLZ, respectively, and assessed their loading efficiency, particle size, and zeta potential. The particles were characterized using a variety of methods such as differential scanning calorimetry (DSC), dynamic light scattering (DLS), and Transmission Electron Microscopy (TEM). Thermosensitive gels were formulated by combining these particles and their viscosity, gelation temperature, in-vitro release profile, as well as antibacterial and antifungal effects were evaluated. RESULTS: Both types of these nanoparticles were found to be spherical (TEM) with a mean particle size of 243.03 nm in niosomes and 171.97 nm in SLNs (DLS), and respective zeta potentials of -23.3 and -15. The loading rate was 98% in niosomes and 51% in SLNs. The release profiles of niosomal formulations were slower than those of the SLNs. Both formulations allowed the release of the drug by first-order kinetic. Additionally, the gel formulation presented a slower release of both drugs compared to niosomes and SLNs suspensions. CONCLUSION: Thermosensitive gels containing clindamycin-loaded niosomes and/or FLZ-SLNs were found to effectively fight the periodontitis-causing bacteria and fungi.


Clindamycin , Fluconazole , Gels , Liposomes , Nanoparticles , Particle Size , Periodontal Diseases , Clindamycin/administration & dosage , Clindamycin/therapeutic use , Nanoparticles/chemistry , Fluconazole/administration & dosage , Fluconazole/pharmacology , Periodontal Diseases/drug therapy , Antifungal Agents/administration & dosage , Antifungal Agents/pharmacology , Anti-Bacterial Agents/administration & dosage , Anti-Bacterial Agents/pharmacology , Microscopy, Electron, Transmission , Temperature , Calorimetry, Differential Scanning , Candida albicans/drug effects , Viscosity , Lipids/chemistry , Humans
4.
Food Res Int ; 187: 114310, 2024 Jul.
Article En | MEDLINE | ID: mdl-38763627

Rice bran was modified by steam explosion (SE) treatment to investigate the impact of different steam pressure (0.4, 0.8, 1.2, 1.6, and 2.0 MPa) with rice bran through 60 mesh and rice bran pulverization (60, 80, and 100 mesh) with the steam pressure of 1.2 MPa on the structure, thermal stability, physicochemical and functional characteristics of insoluble dietary fiber (IDF) extracted from rice bran. IDF with SE treatment from scanning electron microscopy images showed a porous honeycomb structure, and lamellar shape in IDF became obvious with the increase of steam pressure. The relative crystallinity and polymerization degree of crystalline regions in IDF from rice bran with SE treatment from X-ray diffraction analysis were decreased. Differential scanning calorimetry results showed that thermal stability of IDF with SE treatment increased with the increase of crushing degree. The results of FT-IR also suggested that some glycosidic and hydrogen bonds in IDF could be broken, and some cellulose and hemicellulose were degraded during SE process. The physicochemical and functional characteristics of IDF, including water-holding capacity, oil-holding, glucose adsorption capacity, α-amylase and pancreatic lipase inhibition capacity were decreased with the increase of steam pressure and crushing degree. The swelling and nitrite adsorption capacities of IDF were increased first and then decreased with the increase of steam pressure. The physicochemical and functional characteristics of IDF from rice bran were improved after SE treatment, which might provide references for the utilization of IDF from rice bran with SE treatment.


Dietary Fiber , Oryza , Particle Size , Pressure , Steam , Oryza/chemistry , Dietary Fiber/analysis , Food Handling/methods , Solubility , X-Ray Diffraction , Hot Temperature , Spectroscopy, Fourier Transform Infrared , Microscopy, Electron, Scanning , Calorimetry, Differential Scanning
5.
Sci Rep ; 14(1): 10680, 2024 05 09.
Article En | MEDLINE | ID: mdl-38724608

Bosentan is a drug used to treat pulmonary hypertension via dual endothelial receptor antagonism. Bosentan has a restricted oral bioavailability, a problem that's mostly due to poor solubility and hepatic metabolism. It is extensively used for the elderly and children who require a friendly dosage form like orodispersible tablets. So, the goal of this research work was to hasten the dissolution rate of bosentan to produce an orodispersible tablet with immediate drug release. Bosentan was exposed to ethanol-assisted kneading with a rise of xylitol or menthol concentrations (1:1 and 1:2 molar ratio of bosentan with excipient). In addition to observing the dissolution behavior, the resulting dry products were investigated using Fourier transform infrared spectroscopy (FTIR), differential thermal analysis (DTA), and X-ray diffraction (XRD). The FTIR reflected possible hydrogen bonding with xylitol and menthol. DSC studies reflected a reduction in the enthalpy and Tm. These results with XRD data reflected partial co-amorphization in the case of xylitol and eutaxia in the case of menthol. These modifications were related to an accelerated dissolving rate. The developed systems were fabricated as orodispersible tablets which exhibited immediate release of bosentan. Thus, the current study offered simple co-processing for the preparation of orodispersible bosentan tablets.


Bosentan , Menthol , Solubility , Tablets , Xylitol , Bosentan/chemistry , Xylitol/chemistry , Menthol/chemistry , Administration, Oral , Spectroscopy, Fourier Transform Infrared , Drug Liberation , X-Ray Diffraction , Excipients/chemistry , Humans , Drug Compounding/methods , Calorimetry, Differential Scanning
6.
Protein Sci ; 33(6): e5010, 2024 Jun.
Article En | MEDLINE | ID: mdl-38723172

Recent studies have demonstrated that one can control the packing density, and in turn the filterability, of protein precipitates by changing the pH and buffer composition of the precipitating solution to increase the structure/order within the precipitate. The objective of this study was to examine the effect of sodium malonate, which is known to enhance protein crystallizability, on the morphology of immunoglobulin precipitates formed using a combination of ZnCl2 and polyethylene glycol. The addition of sodium malonate significantly stabilized the precipitate particles as shown by an increase in melting temperature, as determined by differential scanning calorimetry, and an increase in the enthalpy of interaction, as determined by isothermal titration calorimetry. The sodium malonate also increased the selectivity of the precipitation, significantly reducing the coprecipitation of DNA from a clarified cell culture fluid. The resulting precipitate had a greater packing density and improved filterability, enabling continuous tangential flow filtration with minimal membrane fouling relative to precipitates formed under otherwise identical conditions but in the absence of sodium malonate. These results provide important insights into strategies for controlling precipitate morphology to enhance the performance of precipitation-filtration processes for the purification of therapeutic proteins.


Malonates , Malonates/chemistry , Filtration , Chemical Precipitation , Immunoglobulins/chemistry , Polyethylene Glycols/chemistry , Chlorides/chemistry , Calorimetry, Differential Scanning , Malates/chemistry , Zinc Compounds
7.
Protein Sci ; 33(6): e5020, 2024 Jun.
Article En | MEDLINE | ID: mdl-38747397

Wheat germ agglutinin (WGA) demonstrates potential as an oral delivery agent owing to its selective binding to carbohydrates and its capacity to traverse biological membranes. In this study, we employed differential scanning calorimetry and molecular dynamics simulations to comprehensively characterize the thermal unfolding process of both the complete lectin and its four isolated domains. Furthermore, we present the nuclear magnetic resonance structures of three domains that were previously lacking experimental structures in their isolated forms. Our results provide a collective understanding of the energetic and structural factors governing the intricate unfolding mechanism of the complete agglutinin, shedding light on the specific role played by each domain in this process. The analysis revealed negligible interdomain cooperativity, highlighting instead significant coupling between dimer dissociation and the unfolding of the more labile domains. By comparing the dominant interactions, we rationalized the stability differences among the domains. Understanding the structural stability of WGA opens avenues for enhanced drug delivery strategies, underscoring its potential as a promising carrier throughout the gastrointestinal environment.


Molecular Dynamics Simulation , Protein Stability , Wheat Germ Agglutinins , Wheat Germ Agglutinins/chemistry , Wheat Germ Agglutinins/metabolism , Nuclear Magnetic Resonance, Biomolecular , Protein Domains , Calorimetry, Differential Scanning
8.
Food Res Int ; 183: 114212, 2024 May.
Article En | MEDLINE | ID: mdl-38760140

This study evaluated the effect of ultrasound treatment combined or not with heat treatment applied to lentil protein isolate (LPI) aiming to enhance its ability to stabilize high internal phase emulsions (HIPE). LPI dispersion (2%, w/w) was ultrasound-treated at 60% (UA) and 70% (UB) amplitude for 7 min; these samples were subjected to and then heat treatments at 70 °C (UAT70 and UBT70, respectively) or 80 °C (UAT80 and UBT80, respectively) for 20 min. HIPEs were produced with 25% untreated and treated LPI dispersions and 75% soybean oil using a rotor-stator (15,500 rpm/1 min). The LPI dispersions were evaluated for particle size, solubility, differential scanning calorimetry, electrophoresis, secondary structure estimation (circular dichroism and FT-IR), intrinsic fluorescence, surface hydrophobicity, and free sulfhydryl groups content. The HIPEs were evaluated for droplet size, morphology, rheology, centrifugal stability, and the Turbiscan test. Ultrasound treatment decreased LPI dispersions' particle size (∼80%) and increased solubility (∼90%). Intrinsic fluorescence and surface hydrophobicity confirmed LPI modification due to the exposure to hydrophobic patches. The combination of ultrasound and heat treatments resulted in a reduction in the free sulfhydryl group content of LPI. HIPEs produced with ultrasound-heat-treated LPI had a lower droplet size distribution mode, greater oil retention values in the HIPE structure (> 98%), lower Turbiscan stability index (< 2), and a firmer and more homogeneous appearance compared to HIPE produced with untreated LPI, indicating higher stability for the HIPEs stabilized by treated LPI. Therefore, combining ultrasound and heat treatments could be an effective method for the functional modification of lentil proteins, allowing their application as HIPE emulsifiers.


Emulsions , Hot Temperature , Lens Plant , Particle Size , Plant Proteins , Lens Plant/chemistry , Emulsions/chemistry , Plant Proteins/chemistry , Solubility , Hydrophobic and Hydrophilic Interactions , Food Handling/methods , Calorimetry, Differential Scanning , Spectroscopy, Fourier Transform Infrared , Circular Dichroism , Rheology , Ultrasonics/methods , Sonication/methods
9.
Commun Biol ; 7(1): 588, 2024 May 16.
Article En | MEDLINE | ID: mdl-38755264

Although a low temperature limit for life has not been established, it is thought that there exists a physical limit imposed by the onset of intracellular vitrification, typically occurring at ~-20 °C for unicellular organisms. Here, we show, through differential scanning calorimetry, that molar concentrations of magnesium perchlorate can depress the intracellular vitrification point of Bacillus subtilis cells to temperatures much lower than those previously reported. At 2.5 M Mg(ClO4)2, the peak vitrification temperature was lowered to -83 °C. Our results show that inorganic eutectic salts can in principle maintain liquid water in cells at much lower temperatures than those previously claimed as a lower limit to life, raising the prospects of active biochemical processes in low temperature natural settings. Our results may have implications for the habitability of Mars, where perchlorate salts are pervasive and potentially other terrestrial and extraterrestrial, cryosphere environments.


Bacillus subtilis , Perchlorates , Bacillus subtilis/metabolism , Bacillus subtilis/drug effects , Bacillus subtilis/physiology , Perchlorates/chemistry , Cold Temperature , Vitrification , Calorimetry, Differential Scanning
10.
Carbohydr Polym ; 335: 122070, 2024 Jul 01.
Article En | MEDLINE | ID: mdl-38616092

Starches are hydrolyzed into monosaccharides by mucosal α-glucosidases in the human small intestine. However, there are few studies assessing the direct digestion of starch by these enzymes. The objective of this study was to investigate the changes in the structure and enzyme binding of starches during in vitro hydrolysis by mammalian mucosal enzymes. Waxy maize (WMS), normal maize (NMS), high-amylose maize (HAMS), waxy potato (WPS), and normal potato (NPS) starches were examined. The order of the digestion rate was different compared with other studies using a mixture of pancreatic α-amylase and amyloglucosidase. NPS was digested more than other starches. WPS was more digestible than WMS. Hydrolyzed starch from NPS, NMS, WPS, WMS, and HAMS after 24 h was 66.4, 64.2, 61.7, 58.7, and 46.2 %, respectively. Notably, a significant change in the morphology, reduced crystallinity, and a decrease in the melting enthalpy of the three starches (NPS, NMS, and WPS) after 24 h of hydrolysis were confirmed by microscopy, X-ray diffraction, and differential scanning calorimetry, respectively. The bound enzyme fraction of NPS, NMS, and WPS increased as hydrolysis progressed. In contrast, HAMS was most resistant to hydrolysis by mucosal α-glucosidases in terms of digestibility, changes in morphology, crystallinity, and thermal properties.


Starch , alpha-Glucosidases , Humans , Animals , Hydrolysis , Amylose , Calorimetry, Differential Scanning , Waxes , Zea mays , Mammals
11.
Biochem Biophys Res Commun ; 709: 149806, 2024 May 21.
Article En | MEDLINE | ID: mdl-38579619

Differential Scanning Calorimetry (DSC) is a central technique in investigating drug - membrane interactions, a critical component of pharmaceutical research. DSC measures the heat difference between a sample of interest and a reference as a function of temperature or time, contributing essential knowledge on the thermally induced phase changes in lipid membranes and how these changes are affected by incorporating pharmacological substances. The manuscript discusses the use of phospholipid bilayers, which can form structures like unilamellar and multilamellar vesicles, providing a simplified yet representative membrane model to investigate the complex dynamics of how drugs interact with and penetrate cellular barriers. The manuscript consolidates data from various studies, providing a comprehensive understanding of the mechanisms underlying drug - membrane interactions, the determinants that influence these interactions, and the crucial role of DSC in elucidating these components. It further explores the interactions of specific classes of drugs with phospholipid membranes, including non-steroidal anti-inflammatory drugs, anticancer agents, natural products with antioxidant properties, and Alzheimer's disease therapeutics. The manuscript underscores the critical importance of DSC in this field and the need for continued research to improve our understanding of these interactions, acting as a valuable resource for researchers.


Antineoplastic Agents , Lipid Bilayers , Calorimetry, Differential Scanning , Lipid Bilayers/chemistry , Phospholipids/chemistry , Membranes, Artificial , Liposomes/chemistry
12.
Environ Sci Pollut Res Int ; 31(21): 31001-31014, 2024 May.
Article En | MEDLINE | ID: mdl-38616225

This research addresses the growing need for fast and cost-efficient methods for microplastic (MP) analysis. We present a thermo-analytical method that enables the identification and quantification of different polymer types in sediment and sand composite samples based on their phase transition behavior. Differential scanning calorimetry (DSC) was performed, and the results were evaluated by using different regression models. The melting and crystallization enthalpies or the change in heat capacity at the glass transition point were measured as regression analysis data. Ten milligrams of sea sand was spiked with 0.05 to 1.5 mg of microplastic particles (size: 100 to 200 µm) of the semi-crystalline polymers LD-PE, HD-PE, PP, PA6, and PET, and the amorphous polymers PS and PVC. The results showed that a two-factorial regression enabled the unambiguous identification and robust quantification of different polymer types. The limits of quantification were 0.13 to 0.33 mg and 0.40 to 1.84 mg per measurement for semi-crystalline and amorphous polymers, respectively. Moreover, DSC is robust with regard to natural organic matrices and allows the fast and non-destructive analysis of microplastic within the analytical limits. Hence, DSC could expand the range of analytical methods for microplastics and compete with perturbation-prone chemical analyses such as thermal extraction-desorption gas chromatography-mass spectrometry or spectroscopic methods. Further work should focus on potential changes in phase transition behavior in more complex matrices and the application of DSC for MP analysis in environmental samples.


Calorimetry, Differential Scanning , Geologic Sediments , Microplastics , Microplastics/analysis , Geologic Sediments/chemistry , Regression Analysis , Environmental Monitoring/methods
13.
Anal Biochem ; 691: 115533, 2024 Aug.
Article En | MEDLINE | ID: mdl-38642818

For irreversible denaturation transitions such as those exhibited by monoclonal antibodies, differential scanning calorimetry provides the denaturation temperature, Tm, the rate of denaturation at Tm, and the activation energy at Tm. These three quantities are essential but not sufficient for an accurate extrapolation of the rate of denaturation to temperatures of 25 °C and below. We have observed that the activation energy is not constant but temperature dependent due to the existence of an activation heat capacity, Cp,a. It is shown in this paper that a model that incorporates Cp,a is able to account for previous observations like, for example, that increasing the Tm does not always improve the stability at low temperatures; that some antibodies exhibit lower stabilities at 5 °C than at 25 °C; or that low temperature stabilities do not follow the rank order derived from Tm values. Most importantly, the activation heat capacity model is able to reproduce time dependent stabilities measured by size exclusion chromatography at low temperatures.


Antibodies, Monoclonal , Calorimetry, Differential Scanning , Protein Denaturation , Antibodies, Monoclonal/chemistry , Cold Temperature , Temperature , Protein Stability , Thermodynamics
14.
Mol Pharm ; 21(5): 2315-2326, 2024 May 06.
Article En | MEDLINE | ID: mdl-38644570

The main purpose of our studies is to demonstrate that commercially available mesoporous silica (MS) can be used to control the physical state of aripiprazole (ARP). The investigations performed utilizing differential scanning calorimetry and broadband dielectric spectroscopy reveal that silica can play different roles depending on its concentration in the system with amorphous ARP. At low MS content, it activates recrystallization of the active pharmaceutical ingredient and supports forming the III polymorphic form of ARP. At intermediate MS content (between ca. 27 and 65 wt %), MS works as a recrystallization inhibitor of ARP. At these concentrations, the formation of III polymorphic form is no longer favorable; therefore, it is possible to use this additive to obtain ARP in either IV or X polymorphic form. At the same time, employing MS in concentrations >65 wt % amorphous form of ARP with high physical stability can be obtained. Finally, regardless of the polymorphic form it crystallizes into, each composite is characterized by the same temperature dependence of relaxation times in the supercooled and glassy states.


Aripiprazole , Calorimetry, Differential Scanning , Crystallization , Silicon Dioxide , Aripiprazole/chemistry , Silicon Dioxide/chemistry , Porosity , Dielectric Spectroscopy , X-Ray Diffraction
15.
Int J Biol Macromol ; 267(Pt 2): 131285, 2024 May.
Article En | MEDLINE | ID: mdl-38583841

Thermal stability and iron saturation of lactoferrin (LF) are of great significance not only for the evaluation of the biological activities of LF but also for the optimization of the isolation and drying process parameters. Differential scanning calorimetry (DSC) is a well-established and efficient method for thermal stability and iron saturation detection in LF. However, multiple DSC measurements are typically performed sequentially, thus time-consuming and low throughput. Herein, we introduced the differential scanning fluorimetry (DSF) approach to overcome such limitations. The DSF can monitor LF thermal unfolding with a commonly available real-time PCR instrument and a fluorescent dye (SYPRO orange or Glomelt), and the measured melting temperature of LF is consistent with that determined by DSC. On the basis of that, a new quantification method was established for determination of iron saturation levels using the linear correlation of the degree of ion saturation of LF with DSF measurements. Such DSF method is simple, inexpensive, rapid (<15 min), and high throughput (>96 samples per experiment), and provides a valuable alternative tool for thermal stability detection of LF and other whey proteins.


Fluorometry , Iron , Lactoferrin , Protein Stability , Lactoferrin/chemistry , Lactoferrin/analysis , Iron/chemistry , Fluorometry/methods , Calorimetry, Differential Scanning/methods , Temperature , High-Throughput Screening Assays/methods
16.
Biosci Biotechnol Biochem ; 88(6): 601-607, 2024 May 22.
Article En | MEDLINE | ID: mdl-38569654

Lipoic acid trisulfide, a sulfane sulfur-containing trisulfide of α-lipoic acid, holds promise in pharmaceuticals, yet knowledge gaps persist regarding its synthesis, properties, and stability. Here, we synthesized the lipoic acid trisulfide with a purity exceeding 99% from α-lipoic acid on a gram scale and obtained novel ß-cyclodextrin clathrates (84%-95% yield). Differential scanning calorimetry confirmed the inclusion of lipoic acid trisulfide in ß-cyclodextrins. The resulting ß-cyclodextrin clathrates exhibited significant improvements in water solubility and thermal stability. This pioneering study demonstrated a novel approach to the practical preparation of trisulfide and its ß-cyclodextrin clathrates as active ingredients, paving the way for clinical development.


Solubility , Thioctic Acid , beta-Cyclodextrins , Thioctic Acid/chemistry , beta-Cyclodextrins/chemistry , Sulfides/chemistry , Calorimetry, Differential Scanning , Drug Stability , Water/chemistry
17.
Int J Biol Macromol ; 268(Pt 1): 131550, 2024 May.
Article En | MEDLINE | ID: mdl-38631591

The influence of oat lipids on the structural, thermal, rheological, and in vitro digestibility properties of oat starch under heat processing conditions was investigated. X-ray diffraction, fourier infrared spectroscopy, and differential scanning calorimetry revealed the formation of a V-shaped crystal structure between starch and lipid, resulting in enhanced orderliness and enthalpy. Oat lipids decreased the final viscosity and gel strength of oat starch while weakening the trend towards gel network formation. Additionally, oat lipids exhibited enhanced resistance to starch hydrolase, leading to elevated contents of slowly digestible starch and resistant starch. Consequently, this leads to an augmentation in the rate constants for the rapid digestion fraction (k1) and the slow digestion fraction (k2). When the lipid content reached 7.50 %, a significant increase of 42.20 % was observed in the maximum digestibility of slow digestion fraction (C∞2), while a notable decrease of 44.06 % was noted in the maximum digestibility of rapid digestion fraction (C∞1). The correlation analysis revealed that lipid content, final viscosity, and enthalpy exerted significant influences on in vitro starch digestion. These results demonstrate the substantial impact of lipid content on oat starch structure, subsequently affecting its thermal, rheological, and digestive properties.


Avena , Digestion , Lipids , Rheology , Starch , Starch/chemistry , Starch/metabolism , Avena/chemistry , Viscosity , Lipids/chemistry , X-Ray Diffraction , Calorimetry, Differential Scanning , Temperature
18.
Int J Biol Macromol ; 268(Pt 1): 131576, 2024 May.
Article En | MEDLINE | ID: mdl-38636764

This work aimed to characterize and compare the physicochemical properties of four pulse starches: bean, chickpea, lentil, and pea. Chemical proximate analysis, elemental composition, morphological grain characterization, crystalline structure, thermal analysis, FTIR analysis, and pasting properties were conducted. The proximate analysis shows that these starches have low fat, mineral, and protein content but high amylose values ranging from 29 to 36 % determined by colorimetry. Despite the high amylose content, the starches did not exhibit the typical behavior of an amylose-rich starch, with high peak viscosity and low breakdown and setback. It was found that this behavior was likely due to the large granule size of the ellipsoidal, spherical, and kidney-shaped granules and the high content of some minerals such as Na, Mg, K, Fe, Mn, P, and Si. The study also found that all pulse starches simultaneously contain monoclinic and hexagonal crystals, making them C-type starches. The findings were verified through the Rietveld analyses of X-ray diffraction patterns and differential scanning calorimetry, in which bimodal endothermic peaks evidenced both types of crystals being gelatinized.


Amylose , Rheology , Starch , Starch/chemistry , Amylose/chemistry , Amylose/analysis , Chemical Phenomena , Viscosity , X-Ray Diffraction , Lens Plant/chemistry , Crops, Agricultural/chemistry , Cicer/chemistry , Calorimetry, Differential Scanning
19.
J Chromatogr A ; 1722: 464907, 2024 May 10.
Article En | MEDLINE | ID: mdl-38615560

Developing a reliable and effective quality evaluation system for traditional Chinese medicine (TCM) is both challenging and crucial for its advancement. This study employs fingerprinting techniques to establish precise and comprehensive quality control for TCM, taking Xuezhikang capsules as an example and aiming to facilitate the internationalization of TCM. The "double wavelength absorption coefficient ratio fingerprint" and "Reliability theory" are developed to determine the fingerprint peak purity and fingerprint reliability respectively. Subsequently, the dual-wavelength fusion fingerprint was obtained to avoid the limitations of a single wavelength. In addition, an electrochemical fingerprint (ECFP) was obtained to assess the similarity of electroactive components in the sample, and the Differential Scanning Calorimetry quantized fingerprint (DSC QFP) was introduced for thermal analysis. Fingerprint-efficacy correlations between PL-EC* and dual-wavelength fusion fingerprint (DWFFP) provided valuable insights that there are 76.6 % of the fingerprint compounds exhibited electroactivity. Finally, samples were classified into grades 1∼3 by combining DWFFP, ECFP and DSC QFP through the mean method, meeting the evaluation standard (SL-M > 0.9, PL-M between 80 % and 120 %). This study provides valuable information for ensuring the quality of TCM products, which represents a significant step forward in enhancing the reliability and authenticity of TCM products.


Calorimetry, Differential Scanning , Drugs, Chinese Herbal , Electrochemical Techniques , Medicine, Chinese Traditional , Quality Control , Drugs, Chinese Herbal/chemistry , Drugs, Chinese Herbal/analysis , Electrochemical Techniques/methods , Reproducibility of Results , Chromatography, High Pressure Liquid/methods
20.
Langmuir ; 40(15): 7883-7895, 2024 Apr 16.
Article En | MEDLINE | ID: mdl-38587263

N-Acylated amino acids and neurotransmitters in mammals exert significant biological effects on the nervous system, immune responses, and vasculature. N-Acyl derivatives of γ-aminobutyric acid (N-acyl GABA), which belong to both classes mentioned above, are prominent among them. In this work, a homologous series of N-acyl GABAs bearing saturated N-acyl chains (C8-C18) have been synthesized and characterized with respect to self-assembly, thermotropic phase behavior, and supramolecular organization. Differential scanning calorimetric studies revealed that the transition enthalpies and entropies of N-acyl GABAs are linearly dependent on the acyl chain length. The crystal structure of N-tridecanoyl GABA showed that the molecules are packed in bilayers with the acyl chains aligned parallel to the bilayer normal and that the carboxyl groups from opposite layers associate to form dimeric structures involving strong O-H···O hydrogen bonds. In addition, N-H···O and C-H···O hydrogen bonds between amide moieties of adjacent molecules within each layer stabilize the molecular packing. Powder X-ray diffraction studies showed odd-even alternation in the d spacings, suggesting that the odd chain and even chain compounds pack differently. Equimolar mixtures of N-palmitoyl GABA and dipalmitoylphosphatidylcholine (DPPC) were found to form stable unilamellar vesicles with diameters of ∼300-340 nm, which could encapsulate doxorubicin, an anticancer drug, with higher efficiency and better release characteristics than DPPC liposomes at physiologically relevant pH. These liposomes exhibit faster release of doxorubicin at acidic pH (<7.0), indicating their potential utility as drug carriers in cancer chemotherapy.


1,2-Dipalmitoylphosphatidylcholine , Liposomes , Animals , 1,2-Dipalmitoylphosphatidylcholine/chemistry , Thermodynamics , Doxorubicin , gamma-Aminobutyric Acid , Calorimetry, Differential Scanning , Lipid Bilayers/chemistry , Mammals
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