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Makyo‐kanseki‐to has been used for the treatment of pneumonia, becoming a basic formula for coronavirus disease 2019. However, the chemical profile of Makyo‐kanseki‐to granule and its possible mechanism against acute lung injury from terminal metabolic regulation have been unclear. The aim of this study was to characterize the constituents in Makyo‐kanseki‐to granule and reveal the potential related mechanism of Makyo‐kanseki‐to granule treatment for acute lung injury using a rat model of lipopolysaccharide‐induced acute lung injury. Totally, 78 constituents were characterized based on ultra‐performance liquid chromatography coupled with quadrupole time‐of‐flight mass spectrometry. Makyo‐kanseki‐to granule could alleviate acute lung injury through modulating rectal temperature, pulmonary edema, histopathology, and processes of inflammatory and oxidative stress. Twenty‐two potential biomarkers in acute lung injury rats were identified by metabolomics based on ultra‐performance liquid chromatography coupled with quadrupole exactive high‐field mass spectrometry. They were mainly involved in amino acids and glycerophospholipid metabolism, which were regulated by Makyo‐kanseki‐to granule. The present results not only increase the understanding of the chemical profile and molecular mechanism of Makyo‐kanseki‐to granule mediated protection against acute lung injury but also provide an experimental basis and new ideas for further development and clinical application of Makyo‐kanseki‐to granule. [ABSTRACT FROM AUTHOR]

The present investigation showed that each of the three different liquid chromatography modes may be successfully used for the qualitative analysis of nusinersen metabolites in a patient's serum sample extract. However, the smallest number was detected by the hydrophilic interaction liquid chromatography. Furthermore, the response of the mass spectrometry is several times greater for ion pair chromatography compared to reversed-phase one. Various extraction methods were applied for the extraction of nusinersen metabolites from serum. Silica with bonded capture strand for hybridization was applied, as well as silica modified with amino and carboxyl groups for dispersive solid phase extraction. The hybridization allows selective extraction of nusinersen analogs, however, it fails in extraction of short metabolites. On the contrary, the efficiency of weak ion exchange-based extraction was high, even in the case of the direct extraction of nusinersen metabolites from diluted serum samples without a protein removal step. The new material is a great alternative to liquid-liquid extraction and hybridization for the isolation of nusinersen metabolites from the serum of patients with spinal muscular atrophy (SMA). It is a very simple method that uses a low concentration of organic salt and desorption occurs after changing its pH. Such complex studies were performed for the first time for nusinersen metabolites extracted from the serum of SMA patients treated with Spinraza. [Display omitted] • IP RP HPLC gave higher sensitivity and number of metabolites compared to RP HPLC, HILIC • Hybridization failed for extraction of very short nusinersen metabolites from serum • Successful extraction of nusinersen metabolites directly from serum for new material • New weak anion-exchange material is agreat alternative to LLE and hybridization • The newly developed oligo extraction from serum procedure is environmentally friendly [ABSTRACT FROM AUTHOR]

Summary: Brown seaweeds contain a number of bioactive compounds. The xanthophyll, fucoxanthin, has in vivo efficacy against disorders such as type 2 diabetes, obesity and cancer. Organic solvents are traditionally employed to extract fucoxanthin, but carry a toxic chemical and environmental burden. The aim of this study was to optimise a fucoxanthin extraction method using enzymes, water, low‐temperature dehydration and mechanical blending, to produce yields comparable to those achieved with an organic solvent (acetone). Response surface methodology was applied, using Fucus vesiculosus as a model species. A fucoxanthin yield of 0.657 mg g−1 (dry mass) was obtained from F. vesiculosus blade using the enzymatic method, equivalent to 94% of the acetone‐extracted yield. Optimum extraction parameters were determined to be enzyme‐to‐water ratio 0.52%, seaweed‐to‐water ratio 5.37% and enzyme incubation time 3.05 h. These findings may be applied to the development of value‐added nutraceutical products from seaweed. [ABSTRACT FROM AUTHOR]

Licorice ( Glycyrrhiza uralensis Fisch.) is one of the most popular herbal medicines worldwide. This study aims to identify the metabolites of seven representative bioactive licorice compounds in rats. These compounds include 22β-acetoxyl glycyrrhizin ( 1 ), licoflavonol ( 2 ), licoricidin ( 3 ), licoisoflavanone ( 4 ), isoglycycoumarin ( 5 ), semilicoisoflavone B ( 6 ), and 3-methoxy-9-hydroxy-pterocarpan ( 7 ). After oral administration of 250 mg/kg of 1 or 40 mg/kg of 2 – 7 to rats, a total of 16, 43 and 31 metabolites were detected in the plasma, urine and fecal samples, respectively. The metabolites were characterized by HPLC/DAD/ESI–MS n and LC/IT-TOF-MS analyses. Particularly, two metabolites of 1 were unambiguously identified by comparing with reference standards, and 22β-acetoxyl glycyrrhizin-6″-methyl ester ( 1 - M2 ) is a new compound. Compound 1 could be readily hydrolyzed to eliminate the glucuronic acid residue. The phenolic compounds ( 4 – 7 ) mainly undertook phase II metabolism (glucuronidation or sulfation). Most phenolic compounds with an isoprenyl group (chain or cyclized, 2–5 ) could also undertake hydroxylation reaction. This is the first study on in vivo metabolism of these licorice compounds. [ABSTRACT FROM AUTHOR]

To discover new natural compounds from herbal medicines tends to be more and more difficult. In this paper, a strategy integrating orthogonal column chromatography and liquid chromatography/mass spectrometry (LC/MS) analysis was proposed, and was applied for rapid discovery of new ginsenosides from Panax ginseng (PG), Panax quinquefolium (PQ), and Panax notoginseng (PN). The ginsenosides extracts were fractionated by MCI gel×silica gel orthogonal column chromatography. The fractions were then separated on a C18 HPLC column, eluted with a three-component mobile phase (CH3CN/CH3OH/3 mM CH3COONH4 = H2O), and detected by electrospray ionization tandem mass spectrometry. The structures of unknown ginsenosides were elucidated by analyzing negative and positive ion mass spectra, which provided complementary information on the sapogenins and oligosaccharide chains, respectively. A total of 623 comprising 437 potential new ginsenosides were characterized from the ethanol extracts of PG, PQ and PN. New acylations, diversified saccharide chains and C-17 side chains constituted novelty of the newly identified ginsenosides. An interpretation guideline was proposed for structural characterization of unknown ginsenosides by LC/MS. To confirm reliability of this strategy, two targeted unknown trace ginsenosides were obtained in pure form by LC/MS-guided isolation. Based on extensive NMR spectroscopic analysis and other techniques, they were identified as 3-O-[6-O-(E)-butenoyl-β-D-glucopyranosyl(1,2)-β-D-glucopyranosyl]-20(S)-protopanaxadiol-20-O-β-D-glucopyranosyl(1,6)-β-D-glucopyranoside (named ginsenoside IV) and 3-O-β-D-glucopyranosyl(1,2)-β-D-glucopyranosyl-3β,12β,20(S),24(R)-tetra hydroxy-dammar-25-ene-20-O-β-D-glucopyranosyl(1,6)-β-D-glucopyranoside (ginsenoside V), respectively. The fully established structures were consistent with the MS-oriented structural elucidation. This study expanded our understanding on ginsenosides of Panax species, and the proposed strategy was proved efficient and reliable in the discovery of new minor compounds from herbal extracts. [ABSTRACT FROM AUTHOR]

Abstract: Entropy-based methods have been extensively used to measure the uncertainty information in a variety of fields. In this article, a novel information theory-based method for reducing noise of liquid chromatography–mass spectrometry (LC/MS) data was developed. The uncertainty existed in the LC/MS chromatograms was captured and evaluated by information entropy. By comparing the information entropy computationally derived from mass chromatograms, the good quality chromatograms and the noisy chromatograms can be distinguished. The proposed method was applied in processing LC/MS data of “Jing–Zhi–Guan–Xin” troche which is a well-known preparation of traditional Chinese medicine (TCM). The obtained result indicated that this method is beneficial to reduce noise of LC/MS data of complicated chemical samples, such as TCM. [Copyright &y& Elsevier]

As a traditional Chinese medicine (TCM) formula, Wu-tou decoction has been used for treating rheumatoid arthritis (RA) for more than a thousand years. Identifying pharmacodynamic constituents (PCs) of WTD and exploring their in vivo process are very meaningful for promoting the modernization of TCM. However, the pathological state might change this process. Hence, it is necessary and significant to compare the process in vivo of drugs both in normal and disease state and clarify their action mechanism. Taking Wu-tou decoction (WTD) as the research object, a comprehensive strategy based on liquid chromatography coupled with mass spectrometry (LC-MS) was developed to identify PCs, clarify and compare their absorption and distribution in normal and model rats, and then explore the potential mechanism of TCM. Firstly, the PCs in WTD were identified. Then, the pharmacokinetics (PK) and tissue distribution of these ingredients were studied. Finally, the constituents with the difference between normal and model rats were selected for target network pharmacological analysis to clarify the mechanism. A total of 27 PCs of WTD were identified. The absorption and distribution of 20 PCs were successfully analyzed. In the disease state, the absorption and distribution of all these components were improved to have better treatment effects. The results of target network pharmacological analysis indicated that PTGS1, PTGS2, ABCB1, SLC6A4, CHRM2, ESR1, ESR2, CDK2, TNF and IL-6 are 10 key targets for WTD against RA. The regulatory effects of WTD on the expression of PTGS2 and TNF were further verified. Pathway enrichment analysis showed that the key mechanism of WTD against RA is to reduce inflammation and regulate the immune response. These results indicated that this strategy could better understand the in vivo process and mechanism of WTD under the pathological state. Furthermore, this strategy is also appropriate for other TCM. [Display omitted] • The PCs, absorption and distribution of WTD in normal and AIA rats were compared and clarified. • In disease state, the absorption and distribution of PCs were improved to have better treatment effects. • The main mechanism of WTD in treating RA is to regulate inflammation and immune response. [ABSTRACT FROM AUTHOR]