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The fruits of Piper longum are called long pepper, which are well-known culinary spice as well as traditional medicine. In present work, thirteen sesquiterpenes including four undescribed compounds were isolated from P. longum fruits. Compound 1 was a rare methylated bisabolane-type sesquiterpene. Compounds (-)-3 and (+)-3 were a pair of enantiomers of an uncommon humulane which were separated by chiral HPLC. The absolute configurations of compounds 1-3 were confirmed through the means of spectroscopic data analyses, 13 C NMR calculations employing DP4+ probability analyses, and ECD calculations. Compounds 2 and 11 presented moderated inhibitory effect on the NO release in LPS-induced RAW264.7 cells with IC 50 values of 30.65 ± 0.90 and 38.48 ± 2.42 μM, respectively. Above results enriched the chemical information of P. longum fruits, and meanwhile provided scientific evidences for the anti-inflammatory function of P. longum fruits., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2024. Published by Elsevier B.V.)

Three previously undescribed sesquiterpenes, along with three known ones were isolated from the seeds of Cichorium glandulosum. The structures of them were elucidated by the analysis of spectroscopic data. The isolated compounds were tested for their neuroprotective effects against LPS-induced neuroinflammation in BV-2 cells. Santamarine (5) exhibited inhibitory activity on LPS-induced NO production in BV-2 cells with IC 50 of 0.89 ± 0.12 μM. The mechanism of the compound 5 was related to activating the NF-κB, MAPK and cGAS/STING pathways., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2024. Published by Elsevier B.V.)

Prunus cerasifera Ehrhart fruit polysaccharide (PCP) was obtained after determining the optimal extraction conditions for complex enzyme-assisted hot buffer extraction based on single-factor experiments and response surface methodology, followed by characterization of its physicochemical, processing, rheological, and biological properties. PCP was a thermally stable carbohydrate with acidic functional groups and a molecular weight of 1398.69 kDa, exhibiting smooth, dense flake and honeycomb network microstructures. PCP had favorable hygroscopicity, moisturizing properties, water and oil-holding capacity, proemulsification capability, and in vitro antioxidant activity. The apparent viscosity of PCP in an aqueous system was dependent on concentration and temperature and was altered by the variety and amount of metal ions added; its aqueous solutions exhibited strong viscosity and hydrogel-forming tendencies at suitable concentrations, along with excellent hydrogel properties after gelation. Furthermore, PCP favored the growth of beneficial gut microbiota and associated microbes responsible for producing essential short-chain fatty acids. Overall, PCP displayed high potential as a multifunctional additive for applications in the food, pharmaceutical, and cosmetic industries., Competing Interests: Declaration of competing interest All authors have no competing interests., (Copyright © 2024 Elsevier B.V. All rights reserved.)

Eleven undescribed sesquiterpenes, vachanins A-K covering types of germacrane, eudesmane, guaiacane, and cadinane, along with fifteen known analogs were isolated from the aerial parts of Artemisia vachanica Krasch. ex Poljakov. Their structures were established on the basis of HRMS and NMR data, and their absolute configurations were successfully determined by single-crystal X-ray diffraction analysis, 13 C-NMR calculations and DP4+ probability analysis, and ECD data in corporation with quantum chemical calculations. Vachanin A is the first example of germacrane bearing an uncommon C 5 , C 10 -oxygen bridge. All isolated compounds were assayed for anti-inflammatory and anti-diabetic activities. Compounds 15 and 22 presented weak anti-inflammatory activity by inhibiting the release of NO in RAW 264.7 cells induced by LPS with IC 50 values of 42.82 ± 1.43, and 63.37 ± 3.28 μM., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2024 Elsevier Ltd. All rights reserved.)

Eight undescribed guaianolide sesquiterpene lactones cicholosumins A-H and twelve known ones were isolated from the aerial parts of Cichorium glandulosum Boiss et Huet. Their structures were established by 1D and 2D NMR spectroscopic data, electronic circular dichroism, quantum chemical calculations and single crystal X-ray diffraction analysis. Compounds 9α-hydroxy-3-deoxyzaluzanin C, epi-8α-angeloyloxycichoralexin, 8-O-methylsenecioylaustricin and lactucin showed strong anti-neuroinflammation activity with IC 50 values of 1.69 ± 0.11, 1.08 ± 0.23, 1.67 ± 0.28 and 1.82 ± 0.27 μM, respectively. The mechanism research indicated that epi-8α-angeloyloxycichoralexin inhibited neuroinflammation through the NF-κB and MAPK pathways., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2024 Elsevier Ltd. All rights reserved.)

Twelve undescribed alkaloids, including eight pyrrolo[3,2-g]isoquinoline alkaloids (+)/(-)-anacyquinoline A (1a/1b), (±)-anacyquinoline B (2), (+)/(-)-anacyquinoline C (3a/3b), (±)-anacyquinoline D (4), (±)-anacyquinoline E (5), and (±)-anacyquinoline F (6), together with four pyrrolo[2,3-g]quinoline alkaloids (+)/(-)-anacyquinoline G (7a/7b), (±)-anacyquinoline H (8), and (±)-anacyquinoline I (9), were isolated from the roots of Anacyclus pyrethrum (L.) DC. Their structures were determined via spectroscopic analyses (UV, IR, NMR), HRESIMS, quantum chemical calculations of ECD, DP4+ analysis, and single-crystal X-ray diffraction analysis (Cu Kα). Furthermore, in bioassay, (+)/(-)-anacyquinoline G (7a/7b) and (±)-anacyquinoline H (8) showed inhibition on nitric oxide production in lipopolysaccharide -induced RAW 264.7 cells with IC 50 values of 41.4, 44.1, and 31.4 μM, respectively, indicating their potential anti-inflammatory bioactivity., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2024 Elsevier Ltd. All rights reserved.)

Three undescribed seco-iridoid glycosides, one undescribed flavonoid glycoside, and three known glycosides were isolated and identified from Gentiana olivieri Griseb. The structures of these compounds were determined through spectroscopic analysis and ECD calculations. Olivierisecosides NP (1-3) were identified as aromatic conjugated seco-iridoid glucosides, among them olivierisecoside N was representing a particularly rare subtype known as the morroniside seco-iridoids. The compounds 2, 3, 5, and 6 exhibited significant inhibition of COX-2 expression, particularly compound 5 which demonstrated the most pronounced inhibitory activity with IC 50 value of 23.33 ± 0.51 μM. This study provides evidence for the potential development and utilization of G. olivieri as a source of anti-inflammatory components., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2024 Elsevier B.V. All rights reserved.)

Four undescribed sesquiterpene compounds (1-4) and six known compounds (5-10) were isolated from A. mongolica. Furthermore, compound 5 was a new natural product previously synthesized. The LPS-stimulated BV2 cells were used as a model to evaluate the anti-inflammatory activity of the isolated compounds, among them, compounds 2, 3 and 4 showed significant inhibition of NO levels with IC 50 values of 27.48, 27.39 and 24.96 μM, respectively., Competing Interests: Declaration of competing interest None., (Copyright © 2024 Elsevier B.V. All rights reserved.)

Six undescribed bicyclic sesquiterpene coumarins, kuhistanin A, ferukrin isovalerate, 9'β,12'α - ferukrin isovalerate, (17'E)- 9'α, 12'β - isomarcandin, (17'Z)- 9'α, 12'β - isomarcandin and (17'E) - isomarcandin, together with nine known ones were isolated from the roots of Ferula kuhistanica Korovin. The structures of them were elucidated using NMR and HRESIMS data analysis. The relative configurations of the isolates were confirmed by NOE correlations and NMR calculation. The absolute configurations of them were confirmed by X-ray diffraction analysis and ECD calculation. Anti-vitiligo, anti-inflammatory and cytotoxicity of the isolates were tested. Acetyl feselol, feselol, ferusingensine I and farnesiferol A significantly increased the melanin content at the concentration of 10 μM. (17'E) - 9'α, 12'β - isomarcandin exhibited strong cytotoxicity against HT-29 cell line with IC 50 values of 8.94 ± 0.47 μM, and (17'E) - isomarcandin demonstrated strong cytotoxicity against Hela, A549 and HT-29 cell lines with IC 50 values of 5.29 ± 0.25, 4.01 ± 0.20, and 4.16 ± 0.21 μM, respectively. This study concluded that, isolated compounds from F. kuhistanica demonstrated strong bioactivity towards anti-vitiligo and cytotoxicity and active compounds are suggested as anti-vitiligo and cytotoxicity agent for future drug development., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2024 Elsevier B.V. All rights reserved.)

Twelve undescribed alkaloids, including eight pyrrolo[3,2-g]isoquinoline alkaloids (+)/(-)-anacyquinoline A (1a/1b), (±)-anacyquinoline B (2), (+)/(-)-anacyquinoline C (3a/3b), (±)-anacyquinoline D (4), (±)-anacyquinoline E (5), and (±)-anacyquinoline F (6), together with four pyrrolo[2,3-g]quinoline alkaloids (+)/(-)-anacyquinoline G (7a/7b), (±)-anacyquinoline H (8), and (±)-anacyquinoline I (9), were isolated from the root of Anacyclus pyrethrum (L.) DC. Their structures were determined via spectroscopic analyses (UV, IR, NMR), HRESIMS, quantum chemical calculations of ECD and NMR data, and single-crystal X-ray diffraction analysis (Cu Kα). In bioassay, (+)/(-)-anacyquinoline G (7a/7b), and (±)-anacyquinoline H (8) showed inhibition on NO production with IC 50 values of 41.4, 44.1, and 31.4 μM, respectively., Competing Interests: Declaration of Competing Interest ☒ The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper. ☐The authors declare the following financial interests/personal relationships which may be considered as potential competing interests:, (Copyright © 2024. Published by Elsevier Ltd.)

Seven undescribed sesquiterpenes, including three dimeric guaianolide sesquiterpenes artemongolides G-I (1-3) and four sesquiterpene lactones artemanomalide D-G (16-19), along with seventeen known compounds isoabsinthin (4), absinthin (5), 11-eptabsinthin (6), 11, 11'-bis-epiabsinthin (7), 10', 11'- epiabsinthin (8), anabsinthin (9), isoanabsinthin (10), absinthin D (11), anabsin (12), caruifolin D (13), gnapholide (14), caruifolin C (15), 1β(R),10β(S)-dihydroxy-3-oxo-11β (S)H-4,11(13)-guaien-6α(S),12-olide (20), 1α,6α,8α-trihydroxy-5α,7βH-guaia-3,10(14),11(13)-trien-12-oic acid (21), 1α,6α,8α-trihydroxy-5α,7βH-guaia-3,9,11(13)-trien-12-oic acid (22), argyinolide J (23), artabsinolide A (24) were isolated from the plant Artemisia mongolica. The structures were determined by interpreting NMR, HRESIMS and ECD data. The X-ray crystal structure of 4, 7 and 8 were reported for the first time. In the anti-vitiligo activity test, compounds 2, 7, 12, 23 and 24 demonstrated activity in promoting melanogenesis at a concentration of 50 μM in B16 cells, with 8-methoxypsoralan (8-MOP) as a positive control. Further research on the mechanism revealed that artemongolides H (2) enhance the expression of MITF and TRPs by upregulating p-Akt and p-GSK-3β, leading to an increase in β-catenin content in the cell cytoplasm. Subsequently, β-catenin translocates into the nucleus, resulting in melanogenesis. The results supported the regulation of melanogenesis by artemongolide H (2) through the Akt/GSK3β/β-catenin signaling pathway. The anti-inflammatory results demonstrated that compounds 4, 5, 6, 9 and 14 can inhibit the upregulation of IL-6 mRNA and CCL2 mRNA expression. Compound 12 specifically inhibited the upregulation of IL-6 mRNA expression. These compounds exhibited significant anti-inflammatory activities. The activity results revealed that these sesquiterpene compounds have the potential to become lead compounds for the treatment of vitiligo and inflammatory diseases., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2024 Elsevier Ltd. All rights reserved.)

Investigation on the chemical constituents of Artemisia scoparia resulted in the isolation of sixteen compounds, including undescribed six pairs of diprenylated phenolic enantiomers (±)-scopacoumaricin A-F, and two pairs of cis-trans isomers cis/trans-scopacoumaricin G and cis/trans-artepillin A. Trans-artepillin A was obtained from this plant for the first time. The structures of the isolates were proposed by analysis of their 1D, 2D-NMR and HRESIMS spectroscopic data. Their absolute configurations were determined by comparison of their experimental and calculated electronic circular dichroism spectra. Evaluations of the anti-inflammatory activity revealed that (-)-scopacoumaricin D, (+)-scopacoumaricin F and cis-scopacoumaricin G showed moderate anti-inflammatory activity on lipopolysaccharide-induced nitric oxide production in RAW264.7 cell., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2024 Elsevier Ltd. All rights reserved.)

Three undescribed compounds (1-3), including two butenolides and one indol alkaloids. Together with twenty-one known compounds (4-24) were isolated and identified from Lepidium obtusum Basin. Their structures were elucidated by spectroscopic analysis and ECD calculations. The isolated compounds were tested for their antimicrobial, antioxidant, and anti-inflammatory activities. Among them, compounds 11, 12, 14, 21 and 23 showed moderated antimicrobial activities against (Candida albicans, E. coli, Staphylococcus aureus). Compounds 11, 12, 14, 15, 17 and 18 exhibited potent antioxidant activities against ABTS and DPPH. Compound 1 exhibited moderated anti-inflammatory activities. Compounds 4-24 were isolated from this plant for the first time., Competing Interests: Declaration of Competing Interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2023 Elsevier B.V. All rights reserved.)

Seventeen undescribed guaianolide sesquiterpene lactones, millefoliumines A-Q, and seven known analogues were isolated from the whole plant of Achillea millefolium L. growing in Xinjiang, China. Their structures were elucidated based on the HRESIMS and NMR data analyses. The absolute configurations of millefoliumines A-Q were determined by single-crystal X-ray crystallography, ECD data analysis along with quantum-chemical ECD calculations. The anti-inflammatory effects of these compounds on the LPS-induced RAW264.7 cell model were evaluated. As a result, millefoliumine G exhibited potential inhibitory effects on the release of NO, the level of pro-inflammatory cytokines including TNF-α and IL-6. Above results indicated a potential of the guaianolides from A. millefolium in the anti-inflammatory drug development., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2023 Elsevier Ltd. All rights reserved.)

The ethanol extract of the Gentiana olivieri Griseb plant was subjected to an investigation to ascertain the presence of its iridoid constituents. By means of HPLC and TLC monitoring, a total of thirteen previously unreported seco-iridoid glucosides olivierisecoside A-M, as well as seven known seco-iridoid glycosides and one known iridoid glycoside were isolated. Their structures were elucidated by a comprehensive spectroscopic data analysis and ECD calculations. The absolute configuration of olivierisecoside D was further confirmed through single-crystal X-ray diffraction analysis. All the identified compounds were characterized as aromatic conjugated seco-iridoid glucosides, with olivierisecoside F-I representing a particularly rare subtype known as the morroniside type seco-iridoids. In vitro testing of the isolated compounds revealed their potential anti-inflammatory and hepatoprotective effects. The results showed olivieroside B and 6'-gentisoyl-8-epi-kingiside have good anti-inflammatory activities in LPS induced RAW264.7 cells. Additionally, olivierisecoside M exhibited some improvements in PA-induced L02 and HepG2 cells damage, known compound loganin showed slight hepatoprotective effect in PA-induced HepG2 cells damage., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2023 Elsevier Ltd. All rights reserved.)

Seven previously undescribed guaianolides, millefolactons A-G, and three known analogues, millefoliumins A-C, were isolated from the whole plant of Achillea millefolium L. growing in Xinjiang, China. Their structures were elucidated using the HR-ESI-MS and NMR data analyses. The absolute configurations of millefolactons A-G were determined by single-crystal X-ray crystallography, ECD data analysis, and quantum-chemical ECD calculations. Millefolactons A-E are rare 3-oxa-guaianolides. Millefolacton C, millefolacton E, millefoliumin A and millefoliumin B exhibited enzymatic inhibition of 15-LOX. Molecular docking simulations were conducted to visualize interactions between the four active compounds and 15-LOX and determine binding mechanisms. Moreover, a LPS-induced BV2 cell model was used to further investigate the anti-inflammatory mechanism of millefolacton C. As a result, millefolacton C significantly inhibited NO release, repressed levels of pro-inflammatory cytokines including TNF-α, IL-18, PGE2 and IL-6, and inhibited the protein expression of iNOS and COX2 proteins. In addition, millefolacton C could potently decreased the expression of NLRP3, ASC, and IL-1β proteins in LPS-stimulated BV2 cells. These results indicate that the 3-oxa-guaianolides from A. millefolium L. offer great potential as leads for anti-inflammatory drug development., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2023 Elsevier Ltd. All rights reserved.)

A total of 29 batches of R. graveolens were used in this study, their fingerprints were obtained by ultra-performance liquid chromatography (UPLC) and their melanogenesis activities were evaluated. The common peaks were identified by quadrupole-orbitrap high-resolution mass spectrometry (Q-Orbitrap-HRMS). Eleven coumarins, six alkaloids, three flavonoids, three phenolic acids, and four other compounds were found. The spectrum-effect relationships between R. graveolens' chemical fingerprints, the melanin synthesis, and tyrosine's activation activities were established through chemometrics methods which in detail principal component analysis (PCA), gray correlation analysis (GRA), bivariate correlation analysis (BCA) and orthogonal partial least squares analysis (OPLS). The results showed that P18 (bergapten), P22 (isoimperatorin), P15 (kokusaginine), P7 (rutin), P12 (psoralen), and P13 (graveolinine) were relevant to intracellular melanin synthesis activity and tyrosinase activity. Among them, P18 (bergapten), P15 (kokusaginine), and P12 (psoralen) were validated with good melanogenesis activities. This study provides a research basis for future quality control and medicinal application of R. graveolens., Competing Interests: Declaration of Competing Interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2023 Elsevier B.V. All rights reserved.)

Chlorine-containing guaianolide sesquiterpenoids are rare natural compounds that are mainly derived from plants of the Asteraceae family. Our previous investigations on the whole plant of Achillea millefolium L. resulted in the discovery of two chlorine-containing guaianolide sesquiterpenoids. In the present study, a LC‒MS tracking strategy based on the characteristic isotropic peak of atomic chlorine was employed to isolate nine undescribed chlorine-containing guaianolide sesquiterpenoids, Millefolactons B1-B9, from A. millefolium L.. The structures of these compounds were elucidated by spectroscopic data analysis, and the corresponding absolute configurations were determined by single-crystal X-ray crystallography and ECD data analysis. Millefolactons B2-B7 displayed inhibitory activities against LPS-induced NO release in BV-2 microglial cells., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2022 Elsevier Ltd. All rights reserved.)

Six undescribed monoterpenoids, together with twelve known compounds were isolated and identified from Hyssopus cuspidatus Boriss. Their structures were established by spectroscopic analysis, and the absolute configurations were established by ECD calculations and single-crystal X-ray diffraction crystallography. The isolated compounds were tested for their anti-inflammatory, antibacterial and antitumor activities. Most of the compounds showed potent anti-inflammatory activities. Among them, 3β-hydroxy-7,8-dihydro-β-ionone (8), oleanolic acid (17) and acetylpleamolic acid (18) showed strong anti-inflammatory activity against IL-6 and TNF-α in lipopolysaccharide (LPS) stimulated RAW 264.7 cells. Several compounds showed moderate inhibitory activities against Staphylococcus aureus, Candida albicans, and Escherichia coli. And (4S)-p-menth-l-ene-7,8-diol 8-O-β-D-glucopyranoside (16) showed antitumor activities against MCF-8 and HT-29 cell lines with IC 50 values of 93.39 ± 3.69 and 71.89 ± 2.94 μM, respectively. Oleanolic acid (17) showed moderate antitumor activity against HT-29 cell lines with an IC 50 value of 52.62 ± 1.63 μM. In this study, the discovery of anti-inflammatory, antibacterial and antitumor components from H. cuspidatus could benefit further development and utilization of this plant., Competing Interests: Declaration of Competing Interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2023 Elsevier B.V. All rights reserved.)

Antimicrobial bioactivity-guided isolation of the root extract of Rumex dentatus L. resulted in the characterization of nineteen natural products, including three undescribed compounds (rumexs A-C). Rumexs A and B are rare anthraquinone-anthrone dimers consisting of an emodin-10-C-glycoside linked via C-10 to C-7 of a chrysophanol moiety. They differed only in their configuration at C-10; their absolute configurations were determined by NOESY and ECD analysis. LC-HRMS analysis was performed to identify nineteen compounds. Anthraquinone derivatives such as anthraquinone aglycone, oxanthrone C-glycoside, anthraquinone O-glycoside and anthraquinone dimer were found to be the dominant components of R. dentatus. In addition, naphthol, naphthoquinone, chromone, flavonoid, isocoumarin, and lignanamide derivatives were also identified. Chrysophanol and emodin were the most abundant compounds in the crude ethanol extract; their contents were determined by HPLC to be 7.38 and 5.74 mg/g, respectively. The fractions and isolated compounds were tested for their inhibitory activity against Staphylococcus aureus, Candida albicans, and Escherichia coli. Most of them showed inhibitory activity against S. aureus, some fractions and 2-methoxy-6-acetyl-7-methyljuglone exhibited moderate inhibitory activity against C. albicans, and 2-methoxy-6-acetyl-7-methyljuglone had moderate inhibitory effects against E. coli. Emodin exhibited inhibitory activity against NO release in LPS-reduced RAW264.7 cells in a concentration-dependent manner., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2022 Elsevier Ltd. All rights reserved.)

Eight undescribed jatrophane diterpenoids, namely euphomicrophane A-H, together with thirteen known diterpenes were isolated from the whole plant extracts of Euphorbia microcarpa (Prokh.) Krylov. Among them, euphomicrophane C and F were possessed the endo-type core structure that naturally rarely appeared. The structures of the purified undescribed compounds were established by extensive spectroscopic and spectrometric analysis, and the single-crystal X-ray diffraction analysis was used to determine the absolute configuration of euphomicrophane E, elusone A and euphorbesulin G. All the isolates were screened for their reversal abilities on P-glycoprotein-mediated multidrug resistant cancer cell line MCF-7/ADR. Compounds euphomicrophane G-H and 3β,7β,8α,9α,15β-pentaacetoxy-5β-benzoyloxyjatropha-6(17)-11E-dien-14-one were showed potential chemoreversal effect with reversal fold values 18.67, 17.15, and 16.76 at a concentration of 10.0 μM, being equal to or stronger than the positive drug verapamil (16.68)., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2022 Elsevier Ltd. All rights reserved.)

The optimum extraction condition for the Saussurea involucrata polysaccharide (SIP) was determined to be a temperature of 80 °C, time 2 h, and a liquid-solid ratio of 30 mL/g with a yield of 11.37 %. An acidic homogenous polysaccharide, namely SIP-II was isolated from Saussurea involucrate through anion exchange and gel permeation column chromatography. The structure of the SIP-II was elucidated through the combination of HPLC, GC-MS, IC, peroxide oxidation, smith degradation, methylation, NMR analysis, it was mainly composed of arabinose, rhamnose, galactose, galacturonic acid, and glucose with the molar ratio of 19.85:20.30: 27.12:11.95:8.69 with a molecular weight of 237,570 Da. The glycosidic linkages of SIP-II mainly composed of →1)-α-L-Rhap-(2→, T-Araf, →1)-β-D-GalpA-(4→, →1)-β-D-Galp-(3,6→, →1)-β-D-Galp-(6→, →1)-α-L-Rhap-(2,4→, T-Galp, and →1)-α-L-Araf-(5→. Meanwhile, the structures were characterized through extensive analysis of UV, FT-IR, SEM-EDX, CD, XRD, and TG. SIP-II possessed a remarkable anti-inflammatory activity by effectively inhibiting the expression of pro-inflammatory cytokines and inflammation-related mediators in LPS-stimulated RAW264.7 macrophages, and the anti-inflammatory response of SIP-II might be attributed to the regulation of the NF-κB, MAPK and JAK/STAT pathways. The results showed that polysaccharides from Saussurea involucrate could be a potential ingredient in the functional food and pharmaceutical industry., Competing Interests: Declaration of competing interest The authors declare no conflicts of interest., (Copyright © 2022 Elsevier B.V. All rights reserved.)

Investigation on the chemical constituents of Viola kunawurensis resulted in the isolation of seven undescribed megastigmane sesquiterpenoids including four bicyclic megastigmane glucosides, kunawuronoside A-D, two megastigmane glucosides, kunawuronoside E-F, and a megastigmane, kunawurone A, together with ten known megastigmane sesquiterpenoids. Their structures were established by comprehensive 1D, 2D-NMR and HRESIMS analyses, and their absolute configurations were determined by comparing their calculated ECD data with the experimental ones. Evaluations of the anti-inflammatory activity revealed that kunawuronoside A-D and compounds 14-15 inhibited COX-2 expression with inhibition rates ranging from 36.7% to 58.5%, while the NO production induced by lipopolysaccharide (LPS) was suppressed by the kunawuronoside A-D in a dose-dependent manner in RAW264.7 macrophage cell line., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2022 Elsevier Ltd. All rights reserved.)

Five previously undescribed steroidal glycoalkaloids(SGAs)and a rare ring B-seco isosteroidal alkaloid, were isolated from Fritillaria pallidiflora Schrenk, along with six known alkaloids. The structures of these alkaloids were established by comprehensive analyses of the 1D, 2D-NMR and HR-ESI-MS data. Configurations of sugar moieties were resolved by chemical derivations. The isolated compounds showed nitric oxide (NO) inhibitory activities in lipopolysaccharide (LPS) induced RAW264.7 cells, and yibeinone exhibited the strongest inhibitory effects among them. This study revealed that the alkaloids from F. pallidiflora might have significant anti-inflammatory potentials., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2022 Elsevier Ltd. All rights reserved.)

Eleven undescribed oxygen heterocyclic Diels-Alder-Type sesquiterpenoid dimers, vernodalidimer I-K and M-T, along with a known one, vernodalidimer B were isolated from the seeds of Vernonia anthelmintica. The structures of them were elucidated based on 1D, 2D-NMR experiments and HRESIMS. The absolute configurations of vernodalidimer I-K and M-T were determined by comparison of their experimental and calculated electronic circular dichroism spectra. Cytotoxicity of the isolates against HCT-15, PC-3, A549, and HeLa cell lines were tested. Vernodalidimer K and Q exhibited significant cytotoxic activity against HCT-15 cell line with IC 50 values of 9.8 ± 5.4 μM and 9.4 ± 1.3 μM, respectively., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2022. Published by Elsevier Ltd.)

Twelve undescribed sesquiterpene lactones and seven known sesquiterpene lactones were isolated from the whole plant of Artemisia mongolica. Their structures were elucidated based on the interpretation of NMR, HRESIMS, and electronic circular dichroism (ECD) data. The absolute configurations of mongolicolide A (1), mongolicolide C (3), 1R, 3S-Dihydroxy-7S, 11R-germacra-4Z.9Z-dien-12, 6S-olide (5), indicumolide E (9), indicumolide F (10), and indicumolide G (11) were determined by single-crystal X-ray crystallography. The X-ray crystal structure of artabsinolide E (15) was reported for the first time. In addition, beibersteneolide-B (13) showed moderate anti-inflammatory activity and marked antitumor activity, artemyriantholide E (18) show moderate antitumor activity., (Copyright © 2022 Elsevier Ltd. All rights reserved.)

Eight undescribed guaianolides (macrocephalolides A-H) and two known analogues (parishin C, artabsinolide E) were isolated from the whole plant of Artemisia macrocephala growing in Xinjiang, China. Their structures were determined on the basis of extensive spectroscopic analysis, with absolute configurations established by comparison of experimental and calculated ECD data, as well as confirmation of single-crystal X-ray diffraction crystallography. Macrocephalolides A-B featured an unusual type of 3-oxa-guaianolide with a cyclopentenone moiety. Macrocephalolides C-E possessed a dihydro-2H-pyran acetal segment, representing an unprecedented 2, 3-secoguaianolide skeleton with 6/7/5 tricyclic ring system in natural sesquiterpenes. The X-ray crystal structures of parishin C and artabsinolide E were reported for the first time., (Copyright © 2022 Elsevier Ltd. All rights reserved.)

Ruta graveolens L. has been widely used to treat various skin ailments, especially vitiligo. In this study, we isolated a new furanocoumarin named Rutagrarin (1) along with 14 known compounds (2-15) from the aerial parts of R. graveolens and elucidated their chemical structures via various spectroscopy. We found that compound 5 promoted melanogenesis and tyrosinase activity in B16 cells. Further investigation on underlying mechanisms revealed that compound 5 activated the transcription of microtia-related transcription factors and promoted the production of melanin in B16 cells via the Akt/GSK-3β/β-catenin pathway. Therefore, we confirmed the traditional efficacy of R. graveolens and speculated that compound 5 could be used as a natural drug to treat vitiligo., (Copyright © 2021 Elsevier B.V. All rights reserved.)

Four undescribed pyrrolizidine alkaloids (seneciojanine A-D), two enantiomeric pairs of unusual alkaloids (millingtojanine A-B) with a unique tricyclic core, and nine known pyrrolizidine alkaloids were isolated from whole plant extracts of Jacobaea vulgaris Gaertn. The structures of the undescribed compounds were established by extensive spectroscopic and spectrometric analyses and comparison of theoretical and experimental ECD data. Several of the structures were also confirmed by X-ray diffraction analysis. Seneciojanine A-D possess a rare natural necine moiety with an α,β-unsaturated carbonyl group located at C-3 and a hydroxyl substituent at C-8., (Copyright © 2021 Elsevier Ltd. All rights reserved.)

Eight undescribed sesquiterpenes, including three dimeric guaianolides and five sesquiterpens, together with ten known ones, were isolated from the aerial parts of Artemisia sieversiana. Their structures were elucidated by extensive spectroscopic techniques and ECD calculation. The isolated compounds were tested for their anti-inflammatory effects against IL-1β, IL-6 and TNF-α in LPS-induced RAW 264.7 cells. Compounds 4, 9, 12, 15, 16 and 17 showed potent anti-inflammatory activities., (Copyright © 2021 Elsevier B.V. All rights reserved.)

In this study, a special orthogonal separation method, named as dual-tautomerism separation (DTS), was developed for the purification of tautomeric compounds from complex matrixes. In DTS, isomers of these compounds are individually collected and asymmetrically transformed to the mixtures of isomers. After separating the mixture with an identical method, high-purity compounds can be prepared from the newly generated isomers but impurities remain in another one. To validate the effectiveness, a DTS was developed to prepare punicalagin in gram-scale from pomegranate peel waste. Isomerization kinetic and thermodynamic of punicalagin were accurately assayed by dynamic HPLC built on low-temperature or/and loop-based stop-flow two-dimensional liquid chromatography. After the isomerization based on it, 9.3 g of pomegranate peel extract was firstly separated on C18 column, and F α and F β around α-punicalagin and β-punicalagin were obtained. Then, the proportion of α-punicalagin in F α and F β was optimized to 52.7% and 32.0% based on isomerization kinetics and thermodynamic. With the aid of low-temperature injection, F α and F β were loaded and secondly purified. After waste recycling, totally 3.0 g of punicalagin with the purify of 99.5% was obtained within two days, which would strongly support the resource utilization of pomegranate peel waste. Because only an individual method was employed in the two-step purification, the separation in DTS was fully compatible., Competing Interests: Declaration of Competing Interest The work presented in this report is the subject of pending patents (CN 201910711349.9, CN 201910713229.2, CN 201910711427.5) filed by Xinjiang Technical Institute of Physics and Chemistry, Chinese Academy of Sciences. The authors declared that there are no conflicts of interest to this work and these patents., (Copyright © 2021 Elsevier B.V. All rights reserved.)

Pomegranate peels are an abundant agricultural waste material with a high content of carbohydrates and bioactive compounds. The aim of this study was to efficiently convert waste pomegranate peels (WPP) into high-value-added products. First, high yields of phenolics (12.2%) and bioactive pectin (24.8%) were obtained via enzymatic pretreatment. The lignin was subsequently degraded using an integrated method combining heteropolyacids as catalyst and biomass-derived γ-valerolactone as sustainable solvent and cellulase-catalyzed hydrolysis. The optimal degradation conditions were found to encompass a temperature of 293 K, reaction time of 3 h and catalyst loading with 30 mM heteropolyacids. Under these conditions, the enzymatic hydrolysis efficiency was enhanced significantly, leading to a yield of 93.3% glucose from the obtained cellulosic feedstock. Finally, the fermentable sugars together with the previously recovered pectin from WPP were firstly used as carbon source to evaluate their suitability as feedstock for butyric acid production using Clostridium tyrobutyricum., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2021 Elsevier B.V. All rights reserved.)

Phytochemical study on the ethanolic extract of the dried roots of Ferula samarkandica Korovin led to the isolation of nine undiscribed sesquiterpene coumarins, samarcandicins A-I, along with thirteen known sesquiterpene coumarins. Their structures were characterized by detailed spectroscopic analysis including NMR and HR-ESI-MS. Mogoltacin and nevskin exhibited high inhibitory activity against MV-4-11 cell with IC 50 values of 3.94 ± 0.06 μM and 3.87 ± 0.10 μM, respectively, and nevskin and feshurin showed high inhibitory activity against mino cell with IC 50 values of 1.48 ± 0.06 μM and 7.88 ± 0.60 μM, respectively., (Copyright © 2021 Elsevier Ltd. All rights reserved.)

Eight new jatrophane diterpenoids, Euphosorophane F-M (1-8), as well as fourteen known jatrophane diterpenoids (9-22) were separated and purified from the fructus of Euphorbia sororia, and the chemical structures were determined based on extensive spectroscopic analysis, 1D, 2D NMR and HRESIMS data included. Their absolute configurations of compounds 1, 2, 9, and 22 were elucidated by X-ray crystallographic analysis. These jatrophane diterpenoids showed lower cytotoxicity and compounds 3, 4, 11, 12, 13, 14, and 20 revealed promising multidrug resistance (MDR) reversal ability as modulators compared to verapamil (VRP) by MTT assay. The structure-activity relationship (SAR) exhibited that the absence of keto-carbonyl at C-9 and C-14 was essential to MDR reversal activity and the acyloxies substitution at C-5, C-7, C-8, and C-14 also made the activity difference. Euphosorophane I (4) particularly unfold greater potency (EC 50  = 1.82 μM) in reversing P-gp-mediated resistance to doxorubicin (DOX). As shown by fluorescence microscopy, 4 promoted intracellular accumulation of rhodamine 123 (Rh123) and DOX in a dose-dependentmanner than VRP. Flow cytometry indicated that 4 inhibitedP-glycoprotein (P-gp) -dependentRh123 efflux in drug-resistant MCF-7/ADR cells. 4 stimulated P-gp-ATPase activity in a concentration-dependent way and inhibited DOX transport activity. Western blot and real-time qPCR results further illustrated that 4 exhibited superior MDR reversal effect in MCF-7/ADR cells attributed to the activation of ATPase rather than the upregulation of P-gp expression and mRNA levels. In addition, 4 bond to the drug-binding site of P-gp predicted by the molecular docking analysis. Collectively, these results indicated that 4 efficiently reversed P-gp-mediated MDR via inhibiting the ABCB1 drug efflux function. 4 with the advantage of low toxicity and efficient could be used as an adjuvanttherapy drug for breast cancer., (Copyright © 2021 Elsevier Inc. All rights reserved.)

Seven undescribed guaianolide sesquiterpene lactones, millefoliumins A-G, and five known analogues were isolated from the whole plant of Achillea millefolium L. growing in Xinjiang, China. Their structures were elucidated by analysis of spectroscopic data and comparison with literatures. The absolute configurations of millefoliumins A-G were determined by single-crystal X-ray crystallography, ECD data analysis along with quantum-chemical ECD calculations. The X-ray crystal structures of 8α-angeloxy-1β,2β,4β,5β-diepoxy-10β-hydroxy-6βH,7αH,11βH-12,6α-guaianolide and 8α-angeloxy-4α,10β-dihydroxy-2-oxo-6βH,7αH,11βH-1(5)-guaien-12,6α-olide were reported for the first time, and the full 13 C NMR data of malaphyllidin were attributed for the first time. Millefoliumins F and G, and austricin could improve the melaogenesis by increasing the melanin content and tyrosinase activity of B16 melanoma cells. Millefoliumins A, C and D, and austricin showed anti-inflammatory activity against the NO production in LPS-induced RAW264.7 cells., (Copyright © 2021 Elsevier Ltd. All rights reserved.)

Nine undescribed lignanamides, limoniumins A-I, together with ten known lignanamides and two known phenolics were isolated from ethyl acetate extract of the roots of Limonium gmelinii (Plumbaginaceae). Their structures were determined by spectroscopic analysis including 1D and 2D NMR and HRESIMS experiments. Limoniumin A is the first hybrid lignanamide of phenylpropanoid and coumarin. All tested lignanamides showed significant inhibitory activity against α-glucosidase stronger than positive control and remarkable inhibitory effect to PTP1B with IC 50 values less than 10 μM. In addition, some lignanamides exhibited moderate cytotoxic activity against HeLa and MCF-7 cells and anti-inflammatory activity against COX-2 in a dose-dependent way., (Copyright © 2020 Elsevier Ltd. All rights reserved.)

Phytochemical investigation of mastic, a resin produced by Pistacia lentiscus, led to the isolation and identification of 16 tirucallane triterpenoids, 13 (1-13) of which are undescribed. Their structures and absolute configurations were elucidated based on the analysis of spectroscopic data and single-crystal X-ray diffraction. Compounds 12 and 13 are unusual 7(8 → 9)abeo-tirucallane triterpenoids. Anti-inflammatory assays indicated that compounds 7, 8, 14, and 16 exhibited stronger inhibitory NO production activities (IC50 = 7.7-13.4 μM) than that of the positive control dexamethasone (IC50 = 19.5 μM). In addition, compound 1 showed comparable cytotoxic activity against HepG2 cells to that of doxorubicin (IC50 = 4.92 VS 1.34 μM)., (Copyright © 2020 Elsevier Ltd. All rights reserved.)

A molecular and metabolic behaviour of EPS-producing and salt-tolerant bacterium Rhizobium radiobacter SZ4S7S14 along with its practical application in salt-stress was investigated. The research target was identification and expression profiles of a large EPS biosynthesis gene cluster, possible structural modification of EPS under salt-stress effect and analysis of the gene(s) relative expression and structural modification correlation. As expected, transposons insertions were identified within or near the coding regions of exoK and exoM, previously known large gene cluster that is required for EPS I synthesis. Different expression levels of exoK and exoM in different salt-stress models resulted in structural modification of EPS, which was seen basically in monomers molar ratio. As a result of downregulation of the genes the strain produced EPS samples with monomers ratio: (1) Glu:Man:Gal:Xyl:Ara:Rha:Rib = 31.21:3.02:2.77:1:0.91:0.64:0.41 (in 0.25% NaCl); (2) Glu:Man:Gal:Xyl:Ara:Rha:Rib = 7.65:1:0.69:0.22:0.2:0.16:0.1 (in 0.5% NaCl); (3) Glu:Man:Gal:Ara:Xyl:Rha:Rib = 9.39:1.89:1:0.58:0.52:0.46:0.26 (in 1% NaCl); and (4) Glu:Man:Ara:Xyl:Rib:Gal = 7.9:2:2:1.58:1.1:1 (in 2.0% NaCl), whereas in control (without NaCl): Glc:Man:Gal:Xyl:Ara:Rha:Rib = 11.66:1:0.90:0.37:0.37:0.15:0.14. It was found that, salt-stress not only leads to downregulation of a large EPS biosynthesis gene cluster, including exoK and exoM genes, but also impacting on their relative expression degree, re-groups of the monomers within the EPS matrix and dictates molar ratio of the monosaccharides in the final metabolite., Competing Interests: Declaration of competing interest The authors declare that they have no competing interest., (Copyright © 2020. Published by Elsevier B.V.)

A total of twenty abietane quinone diterpenoids including ten new ones (1-10) were isolated from the roots extract of Salvia deserta. Their chemical structures were delineated by extensive spectrometric and spectroscopic techniques including HRESIMS, NMR, UV, IR, and single-crystal X-ray diffraction analysis, calculated 13 C NMR-DP4+ analysis, calculated ECD, and Mo 2 (OAc) 4 -induced ECD. The absolute configurations of salvidesertone A (1), 8α,9α-epoxy-6-deoxycoleon U (18), and 7,20-epoxyroyleanone (19) were determined by single-crystal X-ray diffraction analysis. Salvidesertone A (1) represents the first example of a 9-hydroxyabieta-7(8)-ene quinone diterpenoid. This is the first report of the crystal structures of 8α,9α-epoxy-6-deoxycoleon U (18) and 7,20-epoxyroyleanone (19). Abietane quinone diterpenoids 1, 2, and 4-20 were evaluated for their antiproliferative activities against five cancer cell lines A-549, SMMC-7721, SW480, MCF-7, and HL-60 and a normal epithelial cell line BEAS-2B in vitro. Salvidesertones E (8) and F (9) selectively inhibited the proliferation of A-549, SMMC-7721, and SW480 cancer cell lines. Importantly, salvidesertones E (8) and F (9), horminone (13), taxoquinone (14), 7α-O-methylhorminone (15), and 8α,9α-epoxy-6-deoxycoleon U (18) showed more potent antiproliferative effects against A-549 than the positive control cis-platin. A preliminary structure-activity relationship for the antiproliferative effects of abietane quinone diterpenoids 1-20 was discussed., (Copyright © 2020 Elsevier Inc. All rights reserved.)

The topic in the present paper is to prepare molecularly imprinted polymer (MIP) using the template molecule with low purity. For the first time, a surrounding of macromolecular crowding was established to promote the formation of the complex of the template with functional monomer efficiently thus highly pure template molecule was unnecessary. In this study, the MIP monolith was synthesized using low purity lactucopicrin as template in place of highly pure one, and polystyrene was used as macromolecular crowding agent. 4-Vinylpyridine and ethyleneglycol dimethacrylate were used as functional monomer and crosslinker, respectively. Polymerization parameters, including the ratio of functional monomer/template, various template concentrations, and PS concentration on the affinity of the resulting MIP were systematically investigated. For the lactucopicrin MIP made with the purity of lactucopicrin of 92%, the imprinting factor can be up to 2.2. The resulting MIP was filled in solid phase extraction (SPE) cartridge to purify lactucopicrin from the crude extract of Cichorium glandulosum Boiss. et Huet. After two cycles of MIP SPE for the crude extract, the highest recovery and purity of lactucopicrin was 64.8% and 97.8%, respectively. The results indicated that the use of macromolecular crowding agent is an effective method for improving the performance of the MIP prepared with the template of low purity, particularly valuable to the cases in which the highly pure target molecule is hard to be obtained., Competing Interests: Declaration of Competing Interests None., (Copyright © 2020. Published by Elsevier B.V.)

This work describes the development of capacity orthogonal chromatography (COC), a new technique for simultaneously determining the loading capacity and orthogonality during the construction of two-dimensional (2D) separations. Three steps were required for the construction of a COC based on the correlation between the selectivity factor (α) and both orthogonality and loading capacity. (1) α values of the impurities-target compound were used to normalize the retention of the impurities around the target compound. (2) α values were input into four quadrants of a coordinate system to identify correlations between orthogonality and loading capacity. α values of the impurities must be greater in the first dimension than the second dimension, with iterated analyses performed until an α max is obtained for the two purification methods. (3) Touch-peak separation using the first-dimensional α max was performed and the target compound was collected. The co-eluted impurities are further separated in the second dimension. To test the efficiency of this technique, a COC using two methods on a standard C18 column was developed to purify corilagin from pomegranate flower extract. Despite its low abundance, 288 mg of corilagin was obtained by COC and further purified by LH-20 gel chromatography to obtain the compound with an 80.0% recovery and 98.4% purity. Compared to COC, the purity of corilagin independently obtained using the same purification methods and identical loading capacity was poor (60.1% and 61.6%). These results indicate that COC is a useful tool for extending loading capacity in the development of preparative 2D separations., Competing Interests: Declaration of Competing Interest The authors have declared no conflict of interest. We declare that we do not have any commercial or associative interest that represents a conflict of interest in connection with the work submitted, (Copyright © 2020. Published by Elsevier B.V.)

Plants of genus Cichorium are famous due to their therapeutic and medicinal properties. They are used as traditional medicine and edible food. To date, several scholars concentrated on compounds belonging to coumarins, flavonoids, sesquiterpenoids, triterpenoids, steroids, organic acids and other chemical constituents. Pharmacological effects such as photo-protective, hepatoprotective, anti-diabetic and lipid lowering, antioxidant, anti-inflammation, antifungal, antimalarial, increased bone mineral density,  as well as vasorelaxant and antitumour activity were wildly reported. In this study, botanical resources, ethnopharmacological application, chemical constituents and bioactivities, as well as safety and toxicity of clinical applications of genus Cichorium were reviewed, which may provide a reliable basis for further development and utilization of Cichorium genetic resources., (© 2020 Tianjin Press of Chinese Herbal Medicines. Published by ELSEVIER B.V.)

A water-soluble polysaccharide, named GPN, with molecular mass 38.7 kDa was isolated from Glycyrrhiza glabra with hot water extraction, ethanol precipitation, and purified by column chromatography. Monosaccharide composition analysis confirmed the presence of predominant glucose (98.03%) and trace amount of mannose, arabinose, and galactose. Methylation and GC-MS analysis revealed that the main glycosidic bonds in GPN comprised 1,4-linked Glcp, T-linked Glcp, 1,4,6-linked Glcp, and 1,6-linked Glcp. Based on these results and 1D/2D NMR spectroscopy, GPN has a linear backbone of 1,4-linked α-D-Glcp and 1,6-linked α-D-Glcp which substituted at C-4 of glucose. The side chain probably composed from 1,4-linked to main side α-D-Glcp and terminal 1-linked β-D-Glcp to the C-3 of D residue. Congo red assay confirmed the existence of triple helix structure. Moreover, SEM and XRD analysis revealed that the GPN had irregular fibrous, filaments like surface; and both crystalline and amorphous structure. GPN also displayed favorable thermal stability. Moreover, G.glabra polysaccharide showed good antioxidant activity., Competing Interests: Declaration of competing interest All authors have no personal or financial conflicts of interest., (Copyright © 2019 Elsevier B.V. All rights reserved.)

In the present study, ultrasonic-assisted extraction (UAE) of polysaccharides from Orchis chusua D. Don (salep) was optimized by response surface methodology (RSM) combined with a Box-Behnken design (BBD), the optimum conditions were determined to be: ultrasonic power of 390 W, extraction temperature of 60 °C, extraction time of 50 min and water/raw material ratio of 40 mL/g. Based on it, 48.30 ± 0.6% yield of crude polysaccharide was obtained. After purification, the chemical compositions, physicochemical and structural property was investigated based on the GC-MS, TGA, XRD, SEM and Congo red test. The results showed that USP-U and USP-N were hetero-polysaccharides, mainly composed of mannose and glucose, and the average molecular weight was 25.57 kDa and 11.64 kDa, respectively. FT-IR spectra and NMR results indicated that the presence of α-linkage glycopyranose via typical peaks. Furthermore, reducing power and antioxidant activities of both purified fractions showed a relatively high ability to scavenge free radicals. Lastly, the cytotoxicity assay showed that purified polysaccharides have no obvious cytotoxicity against RAW267.4 and L6 cells at their effective concentration and had potent anti-inflammatory activity in a concentration-dependent manner. Salep polysaccharide is expected to be developed as a new efficacy factor in the pharmaceutical and food industry., (Copyright © 2019 Elsevier B.V. All rights reserved.)

Three new brassinosteroid analogues, named sulphurenolide A, sulphurenolide B and sulphurenolide C, were isolated from the methanolic extract of fruiting bodies of Laetiporus sulphureus. Their structures were established on the basis of extensive spectroscopic analysis (1D, 2D NMR, and HRESIMS) and ECD calculation. Sulphurenolides A and B are a pair of C-20 epimer, and sulphurenolide B represents the first naturally occurring 20R-brassinosteroid. Moreover, sulphurenolides A-C are firstly reported 5-hydroxylation and homo-6-oxa derivatives of brassinosteroids from natural sources. Anti-inflammatory assay revealed that sulphurenolides B and C exhibited significant inhibitory effects on NO production in lipopolysaccharide-induced RAW264.7 cells, and sulphurenolide C showed stronger inhibition than that of positive control, minocycline., (Copyright © 2019 Elsevier Inc. All rights reserved.)

Pomegranate flowers is an ancient medicine that has commonly been used to treat various diseases such as diabetes. However, no reports are available on the metabolic profile of pomegranate flowers in vivo. In the present study, with the aid of HPLC-Q-TOF-MS 2 , 67 compounds were identified in pomegranate flowers extract, including 18 ellagitannins, 14 gallic acid and galloyl derivatives, five anthocyanins and 18 flavonoids. Seven compounds were firstly identified. In vivo, 22 absorbed compounds and 35 metabolites were identified in rat biosamples (urine, feces, plasma and tissues) after orally administered with pomegranate flowers extract. This result showed that not all compounds abundant in pomegranate flowers extract could be absorbed well in plasma and tissues. This finding also suggested a potential correlation between study on metabolic profile of these compounds in vivo and study on strategy of screening bioactivity of the isolates with in vitro cell systems evaluation. Notably, mono-glucuronide conjugated metabolite of ellagitannin compound (corilagin) was firstly identified. In addition, this is first report to identify phase II conjugate metabolites of ellagitannins in vivo after oral administration of ellagitannins-rich extracts (or foods). Thus, characterizing its multiple constitution, absorption and metabolic fate of these compounds in vivo is helpful to better analyze the active components in pomegranate flowers., (Copyright © 2019. Published by Elsevier B.V.)