Vitamin A is an important nutrient for multiple physiological functions. To elucidate the role of vitamin A in vivo, vitamin A-deficient diets have been often used in mice to establish a vitamin ...A-deficiency model. However, the information on the appropriate feeding periods and time course of changes in vitamin A content in organs after the start of vitamin A-deficient diet feeding is lacking. This study aimed to assess the retinoids levels in liver and white adipose tissue in mice fed a vitamin A-deficient diet for £8 weeks. High-performance liquid chromatography was used to measure the retinoids levels in liver and white adipose tissue every 2 weeks for £8 weeks. Vitamin A-deficient diet feeding significantly decreased retinol in the liver over 6 weeks, but retinyl palmitate, a main storage form of vitamin A, was not changed over 8 weeks. The plasma retinol level remained constant throughout the experiment. In white adipose tissue, retinyl palmitate gradually decreased over 8 weeks. These results indicate that vitamin A-deficient diet feeding longer than 6 weeks reduced retinol in liver and retinyl palmitate in white adipose tissue over 8 weeks, although it is not enough for the induction of a whole-body vitamin A deficiency.
Introduction
Sicklepod Cassia obtusifolia L. syn Senna obtusifolia (L.) H.S. Irwin & Barneby, Fabaceae sprouts are promising ingredients with health‐promoting benefits. Notwithstanding, the ...pharmacologically active compounds in sicklepod sprouts have not been studied or analysed in detail.
Objective
This study aimed to isolate and structurally identify phytochemicals showing α‐glucosidase inhibitory activity in sicklepod sprouts and simultaneously quantify the compounds in the sprouts to determine the optimal cultivation method and germination time to maximise active compounds.
Method
A simultaneous high‐performance liquid chromatography‐ultraviolet (HPLC‐UV) method with high sensitivity and accuracy was developed and used to analyse time‐dependent changes in anthraquinone content during sicklepod germination.
Results
Thirteen anthraquinones were isolated and identified, of which six—chrysoobtusin, emodin, 1‐O‐methyl‐2‐methoxychrysophanol, 7‐O‐methylobtusin, chrysophanol, and physcion—showed moderate α‐glucosidase inhibitory activity. The maximum content of anthraquinones in a sprout was observed on Day 5 under both light and dark conditions.
Conclusion
The findings of this study revealed that sicklepod sprouts which are promising functional food materials contain a variety of anthraquinones.
In this study, the functional characterization and simultaneous HPLC analysis of 13 anthraquinones in sicklepod (Cassia obtusifolia L.) sprouts. The phytochemical investigation revealed that sicklepod sprouts produced various free anthraquinones, which exhibited α‐glucosidase inhibitory activity. Interestingly, the anthraquinone content increased during sprouting. Hypothetically, because hydrolase in the seeds was activated during sprouting and anthraquinone glycosides were changed to free anthraquinones with α‐glucosidase inhibitory activity, the activity of the sprouts was stronger than that of the seeds.
•A new stationary phase (β-CD-DCIPI@SiO2) with chiral separation properties was constructed.•Chlorine substituents in β-CD-DCIPI@SiO2 provided the possibility for separation of chiral ...enantiomers.•Separation performance of β-CD-DCIPI@SiO2 in chiral compounds was explored by reversed-phase HPLC.
β-Cyclodextrin (β-CD) has a unique three-dimensional structure and chemical properties, and has a strong chiral separation ability. In this study, we linked 3,5-dichlorobenzene isocyanate to β-cyclodextrin and named this newly synthesized molecule β-CD-DCIPI. 3,5-Dimethylbenzene isocyanate was attached to β-cyclodextrin and named β-CD-DPIC. A modified polymerization-induced colloidal aggregation (PICA) method and self-made silica sol were used to synthesize mesoporous silica microspheres with a particle size of 2.38 μm-5.51 μm. A green non-toxic diazoresin (DR) is used as a coupling agent, which is connected to the surface of silica microspheres through electrostatic interaction. After ultraviolet light irradiation, ionic bonds are transformed into covalent bonds, and a new chiral stationary phase with chiral separation properties (β-CD-DCIPI@SiO2 and β-CD-DPIC@SiO2) is constructed. This article first characterizes the properties of mesoporous silica microspheres and β-CD-DCIPI@SiO2 and β-CD-DPIC@SiO2. Through reversed-phase high-performance liquid chromatography (RP-HPLC), the separation performance of two new chiral stationary phases in chiral compounds was explored and compared, and five chiral enantiomers were effectively separated.
The biological small‐angle X‐ray scattering (BioSAXS) beamline (BL19U2) at the Shanghai Synchrotron Radiation Facility, China, is dedicated exclusively to small‐angle scattering experiments for ...biological macromolecules in solution. With recent advances in data‐analysis algorithms and X‐ray detectors, SAXS becomes an ideal complementary technique to other structural and biophysical methods, but it can also be applied alone to obtain important structural information. Owing to the increasing interest in solution scattering studies from the biological community, the workload on BL19U2 has steadily risen. A major upgrade of BL19U2 was performed to improve the beamline data quality, to enrich the possible sample environments and to provide a user‐friendly interface. These upgrades involved the major components of BL19U2, including the optical system (slits, beamstop), the electronics, the control and acquisition software, and the sample environments, which resulted in improvements to the collected angular range in BL19U2. These upgrades have significantly broadened the scope of macromolecule size (from kilodaltons to gigadaltons) analysed at the beamline. The dedicated BL19U2 BioSAXS beamline now offers fully automated data‐collection and remote‐control possibilities. These developments have paved the way for high‐throughput studies that generate significant quantities of structure information over a short period of time.
The upgraded biological small‐angle X‐ray scattering (SAXS) station at the Shanghai Synchrotron Radiation Facility is equipped with an in‐vacuum automated sample loading system, an inline Agilent high‐performance liquid chromatography system and a Wyatt light scattering device. The versatile sample environments and easy‐to‐access remote‐control platform make the high‐brightness beamline BL19U2 ideally suitable for performing SAXS experiments on biological macromolecules in solution.
Hypertriglyceridemia has emerged as an independent risk factor for cardiovascular events, despite low-density lipoprotein-cholesterol (LDL-C) well-controlled with statins. We pooled data from the ...first 12 weeks of six randomized double-blind placebo-controlled studies of pemafibrate in Japan and investigated its efficacy and safety with and without statins, particularly focusing on patients with renal dysfunction. Subjects were 1253 patients (677 in the "with-statin" group and 576 in the "without-statin" group). At Week 12 (last observation carried forward), triglyceride (TG) was significantly reduced at all pemafibrate doses (0.1, 0.2, and 0.4 mg/day), both with and without statin, compared to placebo (
< 0.001 vs. placebo for all groups). In the "with-statin" group, the estimated percent change from baseline was -2.0% for placebo and -45.1%, -48.5%, and -50.0%, respectively, for the pemafibrate groups. Findings for both groups showed significant decreases in TG-rich lipoproteins and atherogenic lipid parameters compared to placebo. The incidence of adverse events was similar between the pemafibrate and placebo groups and was also similar for patients with and without renal dysfunction in the "with-statin" group. Pemafibrate lowered TG and improved atherogenic dyslipidemia without a significant increase in adverse events in comparison to the placebo, even among "with-statin" patients who had renal dysfunction.
•A simple, green and sensitive method for 17 phenolic compounds determination was proposed.•This method was based on SULLE pretreatment and HPLC-ECD quantification technique.•The SULLE method ...provided high extraction efficiency and consumed very little solvent and time.•The HPLC-ECD technique provided excellent sensitivity and selectivity.•The method was successfully applied for analysis of honey with different floral origin.
In this work, a simple sugaring-out assisted liquid-liquid extraction (SULLE) method coupled with high performance liquid chromatography-electrochemical detection (HPLC-ECD) has been developed for rapid and sensitive determination of 17 phenolic compounds in honey. To achieve the maximum extraction efficiency of target analytes, several parameters, such as pH, ionic strength, extraction times and the volume of extracting solvent were optimized. Chromatographic separation was performed on a C18 column with a gradient methanol/aqueous formic acid elution, and the ECD was set at 1.0 V in oxidative mode. Under the optimal conditions, good linearity was obtained for 17 phenolic compounds with the coefficients of determination (R2) higher than 0.9986 in the range of 0.05–20 μg mL–1. The limits of detection (LODs, S/N = 3) for the 17 phenolic compounds were in the range of 0.20–1.26 μg kg–1 by ECD, 9–83 times lower than those obtained with UV detection. Satisfactory recoveries between 79.8% and 105.7% were obtained for spiked honey samples with relative standard deviations (RSD) less than 5.1%. Compared with conventional LLE method, the proposed SULLE method provided higher extraction efficiency and had advantages of rapidity, ease of operation, much less consumption of organic solvents and samples. The proposed HPLC-ECD method featuring excellent sensitivity and selectivity has been applied to the quantification of phenolic compounds in honey samples of different floral origin.
Amitriptyline hydrochloride is an antidepressant drug with sedative effects used to treat the symptoms of anxiety, agitation with depression and schizophrenia with depression. A reversed‐phase ...high‐performance liquid chromatography method was developed to separate and quantitatively determine the assay and four organic impurities of amitriptyline in tablet dosage form and bulk drugs using a C18 column in an isocratic elution mode with mobile phase consisting of a mixture of pH 7.5 phosphate buffer and methanol. The pH conditions used in the chromatographic separation are discussed. The stability‐indicating characteristics of the proposed method were proved using stress testing 5 m HCl at 80°C/1 h, 5 m NaOH at 80°C/1 h, H2O (v/w) at 80°C/1 h, 6% H2O2 (v/v) at 25°C/1 h, dry heat at 105°C/24 h and UV–vis light/4 days and validated for specificity, detection limit, quantitation limit, linearity, precision, accuracy and robustness. For amitriptyline and its four known organic impurities, the quantitation limits, linearity and recoveries were in the ranges 0.25–3.0 μg/ml (r2 > 0.999) and 87.9–107.6%, respectively. The mass (m/z) spectral data of amitriptyline hydrochloride and its impurity are discussed. The proposed LC method is also suitable for impurity profiling and assay determination of amitriptyline in bulk drugs and pharmaceutical formulations.
•A novel magnetic composite (Fe3O4@APTES-GO/ZIF-8) was synthesized using a facile modification strategy.•Fe3O4@APTES-GO/ZIF-8 showed a large surface area and high magnetic response.•Good recoveries ...and a wider linear range with low LODs were achieved.•The method was applied for determination of fungicide residues in water and foods.
In this work, zeolite imidazolate framework-8 (ZIF-8) functionalized magnetic graphene oxide (Fe3O4@APTES-GO/ZIF-8) was successfully synthesized and used as a novel adsorbent in magnetic solid-phase extraction (MSPE) for the determination of four triazole fungicides in water, honey and fruit juices. The main parameters such as extraction time, amount of adsorbent, the pH value of the sample, ionic strength, and desorption solvent which could affect the experiment results were optimization. Under the optimum condition, the obtained linearity of this method ranged from 1 to 1000 µg L−1 for all analytes, with correlation coefficients (R2) ≥ 0.9914. Limit of detections (LODs) and limit of qualifications (LOQs) of four triazole fungicides were ranged from 0.014 to 0.109 µg L−1 and from 0.047 to 0.365 µg L−1, respectively. Based on comparison with outcomes from other studies, Fe3O4@APTES-GO/ZIF-8-MSPE could provide high performance and achieve satisfied results for the analysis of trace triazole fungicides in complicated matrices.
Botanical origin of a bee pollen sample is frequently determined by palynological analysis which also enables classification of the bee pollen samples as monofloral and polyfloral. Nevertheless, ...palynological analysis does not give an insight on its chemical composition and thus its potential therapeutic activities. In this study, the relationship between the botanical origins, chemical compositions and biological activities of bee pollen samples were comparatively investigated. Firstly, bee pollen samples (PO1-11) were examined by palynological method and 5 of them were grouped as monofloral, and the rest was grouped as polyfloral bee pollen. Then, HPTLC analysis was performed for fingerprinting of the phenolic compounds and caffeic acid, isoquercitrin, galangin and chrysin were found the common phenolic components in the bee pollen samples, and these were assigned as “key markers”. Then, a newly developed and validated HPLC method was applied to quantify these key markers in the samples. Furthermore, their total phenolic and total flavonoid contents were comparatively studied. Bioactivity of bee pollen samples were assessed by in-vitro antioxidant and antimicrobial activity tests. A polyfloral bee pollen sample (PO2) was found to exert the highest antioxidant activity. Besides, PO2 and PO9 (polyfloral) showed the highest antimicrobial activity.
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•Floral origins of different bee pollens were assessed by palynological analysis.•HPTLC fingerprints were used to characterize mono/polyfloral bee pollens.•Marker compounds were quantified by a validated HPLC method.•A polyfloral bee pollen showed the highest antioxidant and antimicrobial activity.
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