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Preparation and recognition property of molecularly imprinted covalent organic framework of chlorogenic acids
WANG Youdan, JI Wenhua, WANG Xiao
Shandong Science    2024, 37 (6): 22-30.   DOI: 10.3976/j.issn.1002-4026.20240002
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In this study, an imine-linked molecularly imprinted covalent organic framework (MCOF) was successfully prepared using chlorogenic acids as the template. Adsorption isotherm, adsorption kinetics, and selective recognition capacity were utilized to assess the performance of the MCOF and its non-imprinted counterpart, the covalent organic framework (NCOF). MCOF exhibited good site accessibility, taking 15 min to attain 97.1% of the maximum adsorbing capacity. Compared with the selective adsorption capacity of the NCOF to the analogs of chlorogenic acids, the MCOF showed higher selectivity to a family of related molecules with a structure similar to that of chlorogenic acids. This study shows that the MCOF provides an innovative opportunity to develop a highly selective material for the extraction and separation of a family of molecules from a high polarity medium.

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Quality evaluation of Ganoderma lucidum as a medicinal material based on polysaccharides and entropy-weighted TOPSIS
YANG Zhicheng, SUN Caihong, YE Guan
Shandong Science    2024, 37 (6): 31-41.   DOI: 10.3976/j.issn.1002-4026.20240044
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A comprehensive quantitative model that evaluates Ganoderma lucidum as a medicinal material was established based on polysaccharides and entropy-weighted technique for order preference by similarity to ideal solution(TOPSIS) to provide a reference for the quality evaluation of G. lucidum as a medicinal material and selecting the best batches. Initially, the yield, sugar composition, total sugar content, protein content, and uronic acid content of crude polysaccharides were determined formultiple batches of G. lucidum medicinal materials from the same origin. Subsequently, the data were nondimensionalized. Finally, entropy-weighted TOPSIS was used to comprehensively evaluate the quality of G.lucidum polysaccharides from different batches to establish the optimal standard. The yield, component content detection, and cluster heat map analysis of the polysaccharides showed that the polysaccharide yield and the total sugar and uronic acid content of G. lucidum medicinal materials from different batches varied significantly, whereas differences in the sugar composition and protein content were relatively minor. Polysaccharide yield and intrinsic indicators of the G. lucidum medicinal materials were not related to their origin. Entropy weight analysis showed that the polysaccharide yield weight coefficient was the largest at 23.68%, followed by total sugar at 21.35% and uronic acid content at 13.24%. The TOPSIS ranking and grouping results showed that cultivated G. lucidum fruiting bodies and red G. lucidum polysaccharides had better comprehensive scores. The quality of G. lucidum medicinal materials differ widely among different batches from the same origin. Entropy-weighted TOPSIS based on multi-index comprehensive evaluation achieved rapid, efficient, and accurate optimization of the source for G. lucidum polysaccharide extractasa medicinal material and has broad application prospects in production and comprehensive quality evaluation. This study provides a reference for the quality evaluation of other Chinese medicinal and decoction materials.

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To explore the pharmacodynamic substance basis of Cervi Cornus Colla based on cell membrane chromatography
SUN Tiefeng, ZHAO Yu, WANG Ping, DING Xianglong, DING Lijun, WANG Jinguo
Shandong Science    2024, 37 (5): 1-9.   DOI: 10.3976/j.issn.1002-4026.20230175
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Cell membrane chromatography/ultrahigh-phase liquid chromatography-mass spectrometry (CMC/UPLC-MS) was used to screen the active ingredients, i.e., peptides, in the traditional Chinese medicine tablet Cervi cornus Colla, and the obtained spectra were analyzed using Maxquant software, Perseus software, and Uniprot database. Structures of these peptides were identified using Protein Data Bank, and their molecular properties such as their biological activity, adverse reactions, relative molecular mass, isoelectric point, and stability index were predicted using a bioinformatics platform. With an activity probability of 0.09, the peptides were identified as nontoxic, nonhemolytic, sensitizing, and highly hydrophilic, with a relative molecular mass of 1 541.68, a peptide chain length of 14, an isoelectric point of 3.92, and an instability index of 34.39.This method provides a feasible research approach for rapidly screening and identifying active ingredients(e.g., peptides and proteins) that exhibit pharmacological effects.

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Characterization and identification of chemical constituents in Sedum sarmentosum Bung based on UHPLC-Q-Exactive Orbitrap-MS technology
ZHU Xinyi, YANG Chunguo, TIAN Haitao, HOU Miao, HAN Liwen, DENG Zhipeng
Shandong Science    2024, 37 (5): 10-16.   DOI: 10.3976/j.issn.1002-4026.20230173
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To develop an ultra-performance liquid chromatograpy-quadrupole electrostatic field orbitrap high-resolution mass spectrometry(UHPLC-Q-Exactive Orbitrap-MS)method for characterization and identification of chemical constituents in Sedum sarmentosum Bung.The separation was performed using a Phenomenex Kinetex C18 column(2.1 mm×100 mm, 2.6 μm) with a mobile phase comprising acetonitrile and water containing 0.1% formic acid via gradient elution at a flow rate of 0.3 mL/min;the injection volume was 3.0 μL.Mass spectrometry was performed in positive and negative ionization modes with electrospray ionization. The chemical constituents were characterized and identified based on retention time, precise molecular weight, fragment ions,and comparison with the reference substances.The results of this study showed that 53 compounds were characterized and identified in Sedum sarmentosum Bung, including 25 flavonoids, 12 megastigmanes,11 organic acids,3 alkaloids and 2 other compounds.Five of these compounds were identified via comparison with reference compounds, and three compounds may have not been reported from Sedum sarmentosum Bung.The UHPLC-Q-Exactive Orbitrap-MS method proposed in this study can rapidly and comprehensively characterize the chemical constituents in Sedum sarmentosum Bung and provide a reference basis for the research on quality control and atherapeutic material basis of Sedum sarmentosum Bung.

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Optimization of activated charcoal impurity removal process for Xiaojianzhong mixture and its impacton the stability of the mixture’s preparations
ZHANG Wei, LIU Zhenyuan, DU Haochen, GUO Tiantian, YANG Mei, WANG Shandong, HAN Pei, SONG Xiangyun, ZHANG Guimin
Shandong Science    2024, 37 (4): 1-8.   DOI: 10.3976/j.issn.1002-4026.20230126
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To improve the clarity and stability of Xiaojianzhong mixture, the activated charcoal impurity removal process was selected to purify Xiaojianzhong mixture. The orthogonal test evaluation method was used; the evaluation factors were the amount of activated charcoal, boiling time, and the temperature of the solution during charcoal removal. Furthermore, the transfer rates of paeoniflorin and dry matter were used as evaluation indicators. Variance and visual analyses as well as accelerated stability tests were conducted to optimize the activated charcoal purification process for Xiaojianzhong mixture.In order to carry out these above experiments, three batches of Xiaojianzhong mixture preparations were produced for long-term stability testing. Results showed that the optimal parameters for the activated charcoal boiling purification process of Xiaojianzhong mixture preparations were 0.4% activated charcoal usage, 30 min of activated charcoal boiling time, and a liquid temperature of 100 ℃ during filtration. The average transfer rates of paeoniflorin and dry matter in expanded production under these process conditions were 75.24% and 89.08%, respectively. The optimal activated charcoal boiling purification process obtained from this test can ensure the clarity and stability of Xiaojianzhong mixture preparations while maximizing the retention of paeoniflorin and dry matter, thereby ensuring stable and uniform drug efficacy. This study provides a scientific and reasonable basis forclarifying and optimizing the parameters of the activated charcoal boiling purification process for Xiaojianzhong mixture.

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Investigation of common diseases and pesticide use in Salvia miltiorrhiza
ZHOU Bingqian, LU Heng, YANG Guohong, WANG Xiao, GUO Lanping, LIU Wei
Shandong Science    2024, 37 (4): 9-16.   DOI: 10.3976/j.issn.1002-4026.20230154
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There is currently an unmet need to improve disease prevention and control in Salvia miltiorrhiza. Here, we reviewed the literature as well as visited and surveyed multiple planting sitesand agricultural management units in Shandong’s main production areas, such as Jinan and Linyi,to investigate and summarize the common diseases, incidence patterns, medication types, and pesticide residue status of S.miltiorrhiza, which may also provide foundational data to aid in S. miltiorrhiza production.The findings showed 10 common diseases in S.miltiorrhiza, and a total of 20 categories and 43 types of pesticides, including biopesticides and compound formulations, were used in its management. The varieties of pesticides used were all in compliance with drug use regulations, but issues, such as the lack of pesticide registration,lack of guidance on prevention and control technology, and insufficient promotion of biological control, were found. This article aims to provide a basis for the scientific prevention and control of S. miltiorrhiza diseases, and to promote the green and sustainable development of the S. miltiorrhiza industry.

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A study on the quality standards of Huanglian Hupo Qingxin pills
ZHANG Xiaodan, HE Xiaodong, GAO Yan, YANG Longfei, ZHANG Guanqun, YU Zixiang, LIU Mingjun, WANG Yafei, GENG Zangjia, ZHAO Bonian
Shandong Science    2024, 37 (4): 17-25.   DOI: 10.3976/j.issn.1002-4026.20230165
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To establish a method for the qualitative and quantitative assay of Huanglian Hupo Qingxin pills and provide abasis for the subsequent establishment of quality standards, the six ingredients in the formula (Aquilariae Lignum Resinatum, Fructus Choerospondiatis, Terminalia Chebula, CoptidisRhizoma, Flos Gossampini, and Semen Myristicae)were identified through microscopical observation. Thin-layer chromatography was used to identify Terminalia Chebula. Berberine hydrochloride concentration was assessed using high-performance liquid chromatography.Microscopical and thin-layer identifications of Huanglian Hupo Qingxin pills were conducted,which revealed a berberine hydrochloride concentration of 0.018 0~0.902 0 mg/mL,exhibiting a good linear relationship. The assay method was found to bescientific, sensitive, and reproducible, with relative standard deviations(RSDs)for precision, stability, and reproducibility tests all below 3.0%. The average recovery rate from spike-and-recovery testing was 101.29%, with an RSD of 2.30%.The established quality standardis simple and reproducible and can be used for studying the quality standards of Huanglian Hupo Qingxin pills.

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Screening of potential antiepileptic active ingredients in Rhizoma Gastrodiae based on zebrafish model and metabolomics technology
CHEN Shanjun, WANG Huan, HU Kaiqing, BI Wenjie, CHENG Guidong, WANG Songsong, HAN Liwen, WANG Xiaojing
Shandong Science    2024, 37 (3): 1-9.   DOI: 10.3976/j.issn.1002-4026.20230089
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Identifying potential antiepileptic active ingredients in Rhizoma Gastrodiae is of immense significance for the prevention and treatment of epilepsy. In this study, we used a larval zebrafish epilepsy model to evaluate the antiepileptic activity of Rhizoma Gastrodiae from two different regions. In addition, we employed metabolomics technology based on liquid chromatography tandem mass spectrometry/QE plus to detect the ingredients in Rhizoma Gastrodiae and performed pattern analysis to identify key differential metabolites. The metabolites were further identified using primary and secondary mass spectrometry data and literature references. This step was followed by the confirmation of their antiepileptic activity using the zebrafish epilepsy model. The results showed that nine extracts of Rhizoma Gastrodiae significantly reduced the number of whirls in zebrafish, and significant differences in antiepileptic activity were observed between the Rhizoma Gastrodiae samples from the two regions (P<0.05). Metabolomics and pattern analysis identified six important differential metabolites (Parishin E, Gastrodin, Parishin C, Parishin D, N6-p-hydroxybenzyl adenosine, and 4,4'-dihydroxydibenzyl ether). Activity verification results showed that Parishin E, Gastrodin, and N6-p-hydroxybenzyl adenosine significantly inhibited zebrafish epilepsy-like behavior. This study utilized the zebrafish model and metabolomics to identify and determine several active antiepileptic ingredients in Rhizoma Gastrodiae. Of these, Parishin E and N6- p-hydroxybenzyl adenosine were reported for the first time to exhibit antiepileptic activity, thereby serving as a valuable reference for further research on the antiepileptic effects of Rhizoma Gastrodiae.

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Lignan constituents from the leaves of Dysoxylum gotadhora
YAN Huijiao, CHEN Yujie, SONG Xiangyun, LI Enxia, GENG Yanling
Shandong Science    2024, 37 (3): 10-17.   DOI: 10.3976/j.issn.1002-4026.20230094
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To study the constituents of the leaves of Dysoxylum gotadhora, the 70% ethanol extract was separated using macroporous resin column chromatography, silica gel column chromatography, Sephadex LH-20 gel column chromatography, combined with semi-preparative HPLC and other methods. Four compounds 4,4'-dihydroxy-3,3',5,5'-trtramethoxy-7,9':7',9-diepoxylignane (1), 4'-hydroxy-3,4,5,3'-trtramethoxy-7,9':7',9-diepoxylignane (2), 4',4″-dihydroxy-3,3',3″,5,5',5″ -hexamethoxy-7,9':7',9-diepoxy-4,8″-oxy-8,8'-sesquineolignan-7″,9″-diol (3), 4',4″-dihydroxy-3,3',3″,5,5'-pentamethoxy-7,9':7',9-diepoxy-4,8″-oxy-8,8'-sesquineo lignan -7″,9″-diol (4) were isolated. Their structures were established by 1H NMR, 13C NMR and MS spectroscopy techniques. Compounds 1 to 4 were obtained from the genus Dysoxylum for the first time. DPPH(1,1-diphenyl-2-picryhydrazyl radical 2,2-diphenyl-1-(2,4,6-trinitrophenyl)hydrazyl) radical scavenging rate were used to determine the antioxidant activity. The results show that lignans have significant DPPH free radical scavenging ability.

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