Journal of Pharmaceutical and Biomedical Analysis

OBJECTIVE: This study aimed to explore the mechanism of total saponin of black ginseng (TSBG) in treating heart failure (HF) in DOX-induced HF model rats. METHODS: Rats with HF induced by the intraperitoneal injection of DOX were treated with TSBG (low dose, 30 mg/kg/day; medium dose, 60 mg/kg/day; high dose, 120 mg/kg/day) and shakubar trivalsartan (80 mg/kg/day, positive control) for four weeks. Serum BNP and ANP levels were tested by ELISA, and pathological tissue sections were examined...

Chebulae Fructus, was extensively used as a food supplement and medicinal herb, which contained two medicinal forms corresponding to the mature fruit of Chebulae Fructus (CF) and CF pulp. They were widely used in the Chinese clinical medicine and it played a significant role in the Mongolian and Tibetan medicine for the treatment of sore throat, asthma, diarrhea and other diseases. Both of them were recorded in the 2020 Edition (Volume I) of the Chinese Pharmacopoeia. However, the chemical components of CF and CF pulp have not been holistically explored, which seriously hindered its quality evaluation...

We have previously shown that the Tdp1 inhibitor, enamine derivative of usnic acid, the agent OL9-116, enhances the antitumor activity of topotecan. In the present study, we developed and validated LC-MS/MS method for the quantification of OL9-116 in mouse whole blood and studied pharmacokinetics of the agent. The substance OL9-116 was shown to be stable in the whole blood in vitro. Sample preparation included two steps: mixing 10 µL of a blood sample with 10 µL of 0.2 M ZnSO4 aqueous solution, followed by protein precipitation with 100 µL of acetonitrile containing internal standard...

INTRODUCTION: Belimumab is a monoclonal antibody against B cell activating factor (BLyS). This monoclonal antibody (mAb) has been shown to be effective in reducing disease activity in patients with systemic lupus erythematosus (SLE). Belimumab is available in two forms as a lyophilized powder for intravenous (IV) use, or single-dose syringe for subcutaneous (SC) use. The aim of this study was to develop and validate a liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for quantitation of belimumab in human serum...

Raphani Semen (RS) encompasses two distinct application forms in Chinese clinical practice: raw RS (RRS) and stir-fried RS (SRS). They exhibit divergent drug properties and effects, as described in traditional Chinese medicine theory known as "Sheng shu yi zhi, sheng sheng shu jiang". The dissimilarity in RS's drug properties is intrinsically linked to alterations in its internal components during the stir-frying process. Previous studies have demonstrated that stir-frying renders myrosinase inactive, thereby preventing the enzymatic hydrolysis of glucosinolates in RS...

The ever-increasing technological advancement in the (ultra)high-performance liquid chromatography tandem (high-resolution) mass spectrometry platforms have largely contributed to steeply intensify the interest towards lipidomics research. However, mass spectrometers alone are unable to distinguish between enantiomers. This obstacle is especially evident in the case of glycerolipids analysis due the prochiral nature of glycerol. Until a couple of decades ago, the stereoselective analysis of triacylglycerols (TAGs) was performed on the end products generated either from their enzymatic or chemical hydrolysis, namely on mono- or diacyl-sn-glycerols (MAGs and DAGs, respectively)...

A liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed and validated for the determination of methylene-diphosphonate (MDP) in rat bone. This method employed derivatization of MDP and allowed rapid and sensitive quantification of MDP in rat shin bone. The analyte was extracted from the bone tissues with phosphoric acid and derivatized to MDP tetramethyl phosphonate using trimethylsilyl diazomethane (TMS-DAM). MDP tetramethyl phosphonate was then quantified by liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS), with high selectivity, accuracy, and precision...

BACKGROUND: Herbal extracts contain multiple active constituents, so the sample preparation based on the liquid-liquid extraction (LLE) is demanding, especially when a study subsequent to extraction is needed. Since the laminar flow occurring in microchannels can be formed between two miscible organic phases, a new method of extracting polar compounds from the crude extract of Panax ginseng Meyer in aqueous ethanol by pure n-butanol in the three-phase laminar flow microfluidic chip was established...

Phenolic compounds from Cannabis sativa L. (Cannabaceae family), in particular cannflavins, are known to possess several biological properties. However, their antiproliferative activity, being of great interest from a medicinal chemistry point of view, has not been deeply investigated so far in the literature. In the light of this, the aim of this study was to obtain an enriched fraction of polyphenols (namely PEF) from inflorescences of a non-psychoactive C. sativa (hemp) variety and to evaluate its antiproliferative activity against cancer cells, capitalizing on a new and selective extraction method for hemp polyphenols, followed by preparative flash column chromatography...

Several Amaranthus vegetables (Amaranthaceae) have been recognized as valuable sources of minerals, vitamins, proteins, and phytonutrients, with health-promoting characteristics. In this study, three edible Amaranthus species, namely A. hybridus (AH), A. blitum (AB), and A. caudatus (AC), were chemically characterized using non-targeted liquid chromatography-tandem mass spectrometry (LC-MS/MS) technique. Further, multivariate chemometric analyses were conducted, including principal component analysis (PCA) and correlation-covariance plot (C-C plot)...

Sepsis arises from an uncontrolled inflammatory response to infection that can lead to organ failure. The gut microbiome is increasingly recognized as a key modulator of sepsis progression. This study investigated whether Coptis chinensis water extract (CCWE) could attenuate sepsis by modulating the gut microbiome and immune response. A rat model of sepsis induced by cecum ligation and perforation was used. 16 S ribosomal ribonucleic acid (rRNA) sequencing, proton nuclear magnetic resonance (1 H NMR) metabolomics and flow cytometry assays were used to evaluate microbial, metabolic and immune profiles...

Type 2 diabetes mellitus (T2DM) has been the most prevalent disease and has become a serious public health threat worldwide. Gynura bicolor (Willd.) DC. (GB) contains a variety of nutrients and possesses numerous activities, which might benefit those with diabetes. The current study aimed to confirm the improvement of metabolic disorders and explore the potential mechanism of GB in high fat diet-fed (HFD) and streptozotocin (STZ)-induced T2DM mice. The aboveground sample of GB was extracted with alcohol, and identified by highperformance liquid chromatography (HPLC) and liquid chromatography-Mass Spectrometry/Mass Spectrometry (LC-MS/MS) analysis...

Sodium (S)- 2-(dithiocarboxylato((2 S,3 R,4 R,5 R)- 2,3,4,5,6-pentahydroxyhexyl)amino)- 4(methylthio)butanoate (GMDTC) is a compound that removes cadmium from kidney cells. This study aims to investigate the metabolic stability and metabolite identification of GMDTC in various liver microsomes, including those from human, monkey, dog, rat and mouse. The results show that the T1/2 values of GMDTC in human, monkey, dog, rat and mouse liver microsomes were 16.54, 18.14, 16.58, 15...

Erlotinib is an epidermal growth factor receptor tyrosine kinase inhibitor used in the treatment of cancer. Atorvastatin is a statin commonly applied to treat hypercholesterolemia. In humans, both compounds are metabolized by CYP3A4 and are transported by OATP2B1, ABCB1 and ABCG2. We aimed to generate and validate a bioanalytical method for simultaneous determination of atorvastatin, erlotinib and its major metabolite OSI-420 applicable to biological samples. Quantification of erlotinib, OSI-420, and atorvastatin was achieved with an Agilent high-performance liquid chromatography system 1100/1200 coupled to a triple quadrupole G6410B...

As is well documented, Alzheimer's disease (AD) is the most prevalent neurodegenerative disease. Meanwhile, Schisandra polysaccharide (SCP) has been reported to exert a protective effect on the nervous system and can regulate metabolic disorders in AD-like symptoms of amyloid β-peptide (Aβ) 25-35-induced rats. Nevertheless, the underlying mechanisms and metabolic markers for the diagnosis of AD are yet to be determined. This study aimed to explore the neuroprotective effect and potential mechanism of action of SCP in AD-like symptoms of Aβ25-35-induced rats by combining pharmacodynamics, metabolomics, and lipidomics...

Liangyi paste (LY) is a traditional Chinese medicine made from a mixture of Ginseng and Rehmanniae radix praeparata. The present study aimed to investigate the effects of LY on gut microbiota diversity in immunocompromised mice. The chemical composition of LY extract was analyzed using UPLC-Q-Orbitrap-MS/MS, and the differences in the structure and diversity of the intestinal microbiota of LY extract were examined using 16S rRNA. In this study, identified and analyzed 66 compounds from the LY. These compounds included 11 iridoids, 6 oligosaccharides, 21 protopanaxtriols, 23 protopanaxadiols, 2 OLE, 1 Ionone and 2 phenylethanoside, using advanced UPLC-Q-Orbitrap-MS/MS technology...

Zanubrutinib (ZAN) is an orally administered anti-cancer medication used for the treatment of Mantle cell lymphoma. Recently, it has also been approved by FDA for the treatment of chronic lymphocytic leukemia. Determination of impurities formed in drug substances/products as a result of manufacturing or storage forms an important aspect of drug life cycle management. The current study concentrated on understanding the stability of ZAN under various stress conditions as per the ICH Q1 (R2) guidelines. In total, ZAN produced thirteen degradation products under various hydrolytic (acid, base and neutral) and thermal stress conditions...

Biotherapeutics and their biosimilar versions have been flourishing in the biopharmaceutical market for several years. Structural and functional characterization is needed to achieve analytical biosimilarity through the assessment of critical quality attributes as required by regulatory authorities. The role of analytical strategies, particularly mass spectrometry-based methods, is pivotal to gathering valuable information for the in-depth characterization of biotherapeutics and biosimilarity assessment. Structural mass spectrometry methods (native MS, HDX-MS, top-down MS, etc...

Xiaozhong Zhitong tincture (XZZTT), a prominent Traditional Chinese Medicine (TCM) formulation comprising 21 intricate herbal components, poses a challenge in terms of quality control due to its complex composition and the interplay of diverse chemical constituents. To address this issue, a comprehensive assessment strategy was devised by integrating chromatographic and electrochemical techniques to construct a multidimensional fingerprint for XZZTT samples. This study encompassed the evaluation of 42 XZZTT samples through a systematic quantitative fingerprinting method (SQFM), while also quantifying the concentrations of four specific compounds-Geniposide, Palmatine hydrochloride, Paeonol, and Chlorogenic acid...

Silicon dioxide nanoparticles were synthesized and disposable screen-printed electrodes were modified with these nanoparticles to electrochemically detect the interaction between DNA and patulin, a mycotoxin. Firstly, the synthesized silicon dioxide nanoparticles were chemically characterized by X-ray diffraction (XRD) and Fourier Transform Infrared Spectroscopy (FT-IR). Microscopic characterization of the nanoparticles was performed by Transmission Electron Microscopy (TEM) and Energy-dispersive X-ray spectroscopy (EDX)...