Biomedical Chromatography最新文献

The Tibetan medicine Wuwei Shaji powder (WWSJ) has been extensively applied to treating lung diseases such as chronic obstructive pulmonary disease (COPD). However, there are significant limitations in its quality control and evaluation. The purpose of this study was to analyze the overall chemical composition of WWSJ and to predict potential quality markers for WWSJ in the treatment of COPD. Using UHPLC-Q-Exactive Orbitrap-MS, 83 chemical constituents of WWSJ were identified or preliminarily characterized by 14 authentic reference standards, accurate mass counts, and characteristic fragment ions. In addition, serum pharmacology methods were employed to detect 13 blood-migrating components. Further network pharmacological research found that the potential mechanism of WWSJ in the treatment of COPD may be related to the regulation of the immune system and inflammatory response and identified 10 chemicals as key molecules in the treatment of COPD. Finally, the contents of six potential quality markers were determined simultaneously by high-performance liquid chromatography (HPLC). This study lays the foundation for further research on the mechanism of WWSJ in the treatment of COPD.

The present study was designed to optimize the processing of Inonotus hispidus (I. hispidus) by single-factor studies and response surface methodology (RSM). Stir-frying temperature, stir-frying time, and rotational speed of the stir-frying machine were considered as the variables under investigation, whereas ergosterol, total polysaccharides, alcohol-soluble leachate, appearance, and shape were the parameters being studied. Based on single-factor studies, the optimal stir-frying process parameters for I. hispidus were determined using the subjective evaluation analytic hierarchy process (AHP)–entropy weighting method in conjunction with the Box–Behnken design-response surface method (BBD). Correlation analysis of the indicator components and colorimetric values was conducted using correlation and stepwise regression analysis methods. Compositional changes during processing of the concoction were analyzed using UHPLC-Q-Exactive Orbitrap/MS. The optimal process conditions for stir-frying I. hispidus were a stir-frying temperature of 160°C, a stir-frying time of 9 min, and a rotational speed of the stir-frying machine of 40 r/min. Indicators that have a correlation with colorimetric values include alcohol-soluble leachate, appearance and shape. The composition has changed during the concoction process, particularly the styrylpyrones. The preferred formulation process is stable and feasible, providing a reference for researching the formulation process of I. hispidus and clinical medication.

The implementation of ‘Analytical Quality by Design’ (AQbD) is currently recognised as a methodical and scientific approach to liquid chromatographic (LC) method development. It begins with defining the Analytical Target Profile (ATP), identifying Critical Method Parameters (CMPs) and Critical Quality Attributes (CQAs) or responses. This process also includes risk assessment study by Design of Experiment (DoE) and to optimise LC effectively. The next step is to create an analytical design space and implement a control strategy that will allow for continuous method improvement over the life of the method. Understanding the AQbD principles, methodologies, techniques and applications towards the high-performance liquid chromatography (HPLC) method lifecycle is considered as essential in today's pharmaceutical landscape. As industry demands for quality assurance and regulatory compliance, this review paper briefly discusses the AQbD principles and methodology in HPLC method lifecycle. Also, the paper covers AQbD components such as identification of ATP, CQA, MODR (method operable design region), control strategies and continuous method monitoring. In addition, it also covers regulatory perspectives on AQbD, obstacles and potential outcomes in the development of pharmaceutical analytical methods. These aspects provide valuable insights into the application of AQbD in the field of LC.

Mume Fructus (MF), a representative substance in the field of medicine-food homology, has been extensively utilized in clinical treatments and daily diets for its raw and processed forms. This study aimed to establish the spectrum-effect relationship between ultra–high-performance liquid chromatography coupled with quadrupole tandem time-of-flight mass spectrometry (UHPLC-Q-TOF-MS/MS) fingerprints and anti-inflammatory and antitussive activities of raw and processed MF extracts. In UHPLC-Q-TOF-MS/MS fingerprints, a total of 21 common peaks were identified. Bioactivity assays demonstrated that the raw and processed MF extracts exhibited varying degrees of anti-inflammatory and antitussive effects. Subsequently, the relevant pharmacologically active ingredients were screened by grey relation analysis and partial least squares regression. The results showed that nine components were associated with anti-inflammatory effects, namely, citric acid, isochlorogenic acid B, isochlorogenic acid A, isochlorogenic acid C, fumaric acid, gallic acid, neochlorogenic acid, chlorogenic acid, and ononin. Additionally, three components were linked to antitussive activity: amygdalin, syringic acid, and succinic acid, respectively. This work developed a model combining UHPLC-Q-TOF-MS/MS fingerprints with anti-inflammatory and antitussive activities to study the spectrum-effect relationship of raw and processed MF extracts. The findings provide a reference for the discovery of bioactive components and contribute to the clinical rationalization of medications.

We aim to establish the fingerprint profile of Er Miao San (EMS) that aims to accurately evaluate the quality of EMS samples and to identify quality markers for different batches of EMS and explore its related targets and pathways for the treatment of rheumatoid arthritis. HPLC was employed with an Agilent C18 column. Cluster analysis and principal component analysis were conducted by using SPSS and SIMCA software. Network pharmacology techniques were utilized to explore the potential targets and pathways of EMS in the treatment of rheumatoid arthritis. The HPLC fingerprint profile of EMS was established, featuring a total of 15 common peaks, among which nine were identified. The 10 batches of medicinal materials could be clustered into three categories. With VIP > 1 as the criterion, four index differential components were screened out. These intersections were imported into the STRING database and Cytoscape software, resulting in 228 intersection targets. GO and KEGG enrichment analyses were performed on the related targets and pathways. The established method can effectively analyze the quality differences of EMS from different origins. The screened targets and pathways are of great significance for analyzing the differences in the treatment of rheumatoid arthritis by different batches of EMS.

Dalbergia hancei Benth (D. hancei) is a plant belonging to the Fabaceae family. It has analgesic and anti-inflammatory effects and is used by the Zhuang people to relieve pain. However, the mechanism underlying its analgesic effects remains unclear. This study investigates the analgesic effect of D. hancei based on metabolomics to explain the mechanism of its analgesia from a metabolomics perspective. The analgesic effect was evaluated through the acetic acid-induced writhing test and hot plate test. Three treatment groups received different dosages of D. hancei (0.91 g/kg, 3.64 g/kg, 7.28 g/kg). Its analgesic mechanism was investigated using analgesic behavioral tests and metabolomics. The results of analgesic behavioral experiments showed that all dose groups of D. hancei could relieve pain. A total of eight differential metabolites were identified in the metabolomics results. These biomarkers are associated with five metabolic pathways. Following treatment with D. hancei, eight differential metabolites were identified as regulated, primarily affecting amino acid metabolism, pantothenate and CoA biosynthesis, and steroid hormone biosynthesis. This study revealed the mechanism of analgesia from a metabolomic perspective to provide a basis for screening TCM drugs in pain treatment.

The precise separation of enantiomers is crucial in the pharmaceutical industry for the production of single enantiomer drugs. In this study, a novel chiral composite membrane was developed by embedding L-alanine glutaraldehyde condensation product (L-AGCP) onto a polysulfone (PSf) matrix for enantioselective separation. The PSf-L-AGCP membranes were systematically characterized using spectroscopic techniques to confirm the successful incorporation of L-AGCP and to evaluate the structural properties. Permeation studies using DL-alanine demonstrated that the membrane achieved an enantiomeric excess (ee) of 94% for D-alanine, with a flux of 68.1 mmol·m⁻²·h⁻¹ under optimal conditions of 4 bar of transmembrane pressure and 25 mL·min⁻¹ flow rate. The enantioselective performance of the membrane was influenced by varying in feed concentration, transmembrane pressure, and flow rate, achieving the highest ee at lower feed concentrations and moderate pressures. Computational study using density functional theory (DFT) revealed a significant interaction energy difference between L-AGCP and the alanine enantiomers, with values of −32.63 kJ·mol⁻¹ for L-alanine and −16.94 kJ·mol⁻¹ for D-alanine, explaining the selective retention of L-alanine on the membrane. This study demonstrates the potential of L-AGCP embedded PSf membranes in overcoming the permeability-selectivity trade-off in enantioselective separations, offering a promising avenue for scalable, efficient chiral separations in pharmaceutical applications.

Pectolinarin is a flavonoid compound known for its wound-healing properties, including anti-inflammatory and antibacterial effects. In this study, we employed UPLC-MS/MS to quantify pectolinarin in rat plasma and investigate its pharmacokinetics. Plasma samples were processed using an acetonitrile precipitation method. Chromatographic separation was performed on a UPLC BEH column with a gradient mobile phase of acetonitrile-water (containing 0.1% formic acid). Detection was carried out using electrospray ionization (ESI) tandem mass spectrometry in multiple reaction monitoring (MRM) mode with positive ionization, targeting transitions of m/z 623.3 → 315.3 for pectolinarin and m/z 370.5 → 125.0 for the IS. The results demonstrated that pectolinarin exhibited acceptable linearity in rat plasma within the concentration range of 1.2 to 2300 ng/mL (r > 0.995). The intraday and interday precision, expressed as relative standard deviation (RSD), was below 9.2%. Accuracy ranged from 97.3% to 108.3%, with average recovery exceeding 94.7%. The matrix effect was between 97.8% and 105.3%. The method was successfully applied to evaluate the pharmacokinetics of pectolinarin in rats following both oral and intravenous administration. The absolute bioavailability of pectolinarin in rats was determined to be 0.28%.