Biomedical Chromatography最新文献

Back tuina massage and oral administration of astragalus are two methods used in traditional Chinese medicine (TCM) to improve immune function. The aim of this study is to analyze the effects of tuina and orally administered astragalus on immunosuppressed rabbits using proteomics technology. Additionally, we investigate the potential mechanism of action of astragalus components on immunosuppression using an integration of network pharmacology and molecular docking technology. The findings suggested that cyclophosphamide-induced immunosuppression is primarily mediated through signaling pathways that include complement and coagulation cascades and chemical carcinogenesis. Immunosuppression is modulated by tuina and the oral administration of astragalus through various proteins and signaling pathways. A network pharmacology analysis indicated that quercetin, trichothecene isoflavones, and kaempferol in astragalus exhibited immunomodulatory effects. Molecular docking validation demonstrated that 15 major targets showed strong binding affinities to their respective interacting active ingredients. This trial provides references for future studies on the immune-boosting properties of tuina and oral astragalus.

Methylophiopogonanone A (MOA) is one of the homoisoflavonoids isolated from Ophiopogon japonicus, which has been demonstrated to have extensive pharmacological activities. The aim of this study was to develop and validate a liquid chromatography–tandem mass spectrometry method for the measurement of MOA in rat plasma. Methylophiopogonanone B (MOB) was used as internal standard. After precipitation with acetonitrile, the samples were separated using a Waters ACQUITY HSS T₃ column with 0.1% formic acid solution and acetonitrile as mobile phase. Mass detection was monitored using multiple reactions monitoring mode with precursor-to-product ion transition of m/z 343.2 > 135.1 for MOA and m/z 329.2 > 121.1 for internal standard. The assay showed good linearity over the concentration range of 1–1000 ng/mL, with correlation coefficient > 0.997. The lower limit of quantification (LLOQ) was 1 ng/mL. Acetonitrile-mediated precipitation showed high extraction efficiency (> 80%). The accuracy and precision were within the acceptable limits. MOA was demonstrated to be stable in rat plasma under the tested storage conditions. After validation, the proposed method was applied to the pharmacokinetic study of MOA in rat plasma, and the data revealed that MOA showed rapid absorption and elimination from rat plasma. The oral bioavailability of MOA in rat was 24.5%.

The present study discusses the development of a simple, rapid, and specific HPLC method for the estimation of sodium benzoate in chlorzoxazone tablet dosage formulations. The current developed HPLC method was validated as per the current ICH guidelines. The chromatographic separation was achieved using a 0.02-M phosphate buffer adjusted to pH 3.0 with orthophosphoric acid as the buffer. Mobile phase A consisted of 100% buffer, and mobile phase B was a mixture of acetonitrile and buffer in a ratio of 80:20 (v/v). The column temperature was maintained at 30°C, the sample cooler at 25°C, and the flowrate at 0.8 mL min⁻¹. The injection volume was 10 μL. The UV detection was performed at 230 nm for Sodium benzoate. The validated HPLC method was highly specific, with linearity ranging between 1.2 and 7.5 μg/mL for sodium benzoate, and the correlation coefficient was found to be > 0.999. The method showed high accuracy, exceeding 97%. The results demonstrate the successful applicability of the current method for the estimation of sodium benzoate in marketed formulations, which can be extended to assess other formulation systems. The developed method was validated as per international ICH guidelines with respect to specificity, linearity, precision, accuracy, and robustness. The method was applied to the analysis of stability samples.

The four most used antimicrobial preservatives in biopharmaceutical parenteral formulations are phenol, meta-cresol, chlorobutanol, and benzyl alcohol. Preservatives are included in various combinations in biopharmaceuticals highlighting the importance of an analytical method to quantify the four preservatives simultaneously. A headspace GC–MS method was developed to quantify phenol, chlorobutanol, meta-cresol, and benzyl alcohol. The method was validated according to USP <1225>. System suitability <USP 621> was conducted daily for retention time (%RSD < 2.0%), peak area (%RSD < 5.0%), USP tailing factor (< 2.0 and %RSD < 10.0%), and peak resolution (> 2.0). Analytical ranges were 1.5–90 μg/mL for phenol and meta-cresol, 30–240 μg/mL for benzyl alcohol, and 30–300 μg/mL for chlorobutanol. Method accuracy ranged from 94% to 108% and precision from 4% to 15 %RSD for all the tested preservatives. The method was applied to three marketed teriparatide drug products selected as a model. Preservative concentrations of the biopharmaceutical marketed products were determined and were found to be comparable with the labeled concentrations, except for an expired product with 2.5% of the label claim. The developed headspace GC–MS method can be used to evaluate the drug quality of the parenteral formulations and to support the assessment of biopharmaceutical peptide drug products.

To characterize pharmacokinetic profile of sennoside A in rats after intravenous and oral administration, a simple and sensitive liquid chromatography tandem mass spectrometry method was established and validated for quantitative determination of sennoside A in rat plasma. After prepared by protein precipitation with acetonitrile, sennoside A and internal standard were separated on a Waters ACQUITY HSS T3 (2.1 × 100 mm, 1.8 μm) column using acetonitrile and 5-mM ammonium acetate in water as mobile phase by gradient elution. The method showed excellent linearity over the range of 0.5–1000 ng/mL with acceptable intra- and inter-day precision, accuracy, matrix effect, and recovery. The stability assay indicated that sennoside A was stable in plasma during the sample collection, preparation, and analysis. Next, the method was applied to pharmacokinetic study of sennoside A in rats. After intravenous and intragastric administrated to rats, the concentrations of sennoside A in plasma at different time points were quantitated and the pharmacokinetic parameters were calculated by software of DAS 2.0. Pharmacokinetic parameters suggested that after oral administration, sennoside A was reached to the peak at 2.9–3.6 h with a C_max value of 13.2–31.7 ng/mL. Sennoside A was eliminated slowly from the plasma with T_1/2 value between 15.4 and 18.3 h. The oral absolute bioavailability was among 0.9%–1.3%, which indicated low blood exposure level.

In the past decade, significant advances have been made in the field of chiral separation, which is crucial for biological and pharmaceutical applications. Enantioselective membranes have emerged as a promising platform for efficient chiral separation due to their unique properties such as large surface area, tunable pore size, and high selectivity. These membranes are particularly effective in separating enantiomers because of their ability to facilitate selective interactions between the membrane material and chiral molecules. This article provides a comprehensive review of the recent progress in enantioselective membranes for chiral separation. Key topics discussed include various membrane fabrication methods, functionalization approaches, and the characterization of membrane properties, specifically in the context of applications like drug delivery, biomolecule separation, and pharmaceutical analysis. Furthermore, the review addresses the current challenges, potential solutions, and future prospects in this rapidly evolving field, highlighting the direction for upcoming research.