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Farfarae Flos (FF), also known as "Kuandonghua" in Chinese, is a commonly used traditional Chinese medicine (TCM) with various therapeutic properties, including antitussive, expectorant, antioxidant, and anti-inflammatory effects. Despite the widespread consumption of processed FF, there has been limited progress in improving quality control measures for both raw FF and honey-processed Farfarae Flos (PFF). This study aimed to establish a comprehensive strategy for quality evaluation and distinguish between FF and PFF by integrating high-performance liquid chromatography-mass spectrometry (HPLC-MS) analysis with chemometric techniques. Additionally, the antioxidant activities of FF and PFF were assessed using radical-scavenging experiments. The spectrum-effect relationship is the association of chemical composition information of the fingerprint with antioxidant activity, which was used to predict the primary active components that influence the antioxidant activity of FF. The results indicated that FF and PFF samples showed a clear distinction, and the most potent pharmacologically active ingredients were hyperoside, quercetin, caffeic acid, isoquercitrin, neochlorogenic acid, rutin, cryptochlorogenic acid, and isochlorogenic acid C. Moreover, the comprehensive efficacy of the honey-processed FF was better than for raw FF. In conclusion, the findings of this study provide a scientific foundation for future evaluation of the quality, further research, and practical use of FF herbs. [ABSTRACT FROM AUTHOR]

Introduction: Qi‐Fu‐Yin has been used to treat Alzheimer's disease (AD) in China. Oxidative stress has been recognized as a factor in AD progress. To date, there is no quality control method to ensure batch‐to‐batch consistency of Qi‐Fu‐Yin, and the potential antioxidant compounds in Qi‐Fu‐Yin remain uncertain. Objectives: The aim of this study is to identify the potential antioxidant compounds of Qi‐Fu‐Yin and establish quality control standards for Qi‐Fu‐Yin. Methods: High‐performance liquid chromatography was used to establish and quantify the fingerprints of Qi‐Fu‐Yin from various batches. Ultrahigh‐performance liquid chromatography coupled with quadrupole time‐of‐flight tandem mass spectrometry (UHPLC‐Q‐TOF/MS) was used to identify the common peaks. Bivariate correlation analysis, partial least squares regression analysis, and gray correlation analysis were used to establish the spectrum–effect relationship. Results: Forty‐nine common peaks were determined through the establishment of fingerprints. Among them, 35 common peaks were preliminarily characterized. The multiple statistical correlation analysis methods identified six compounds as potential antioxidant constituents of Qi‐Fu‐Yin, and their antioxidant activities were validated in vitro. All six antioxidant compounds derived from two herbs. Therefore, three chemical index compounds derived from other three herbs were added to the quantitative analysis, while for two herbs, no peaks could be included. Eventually, six antioxidant constituents and three index compounds were quantitatively determined to provide a relatively comprehensive quality control for Qi‐Fu‐Yin. Conclusions: The study elucidated the antioxidant substance basis of Qi‐Fu‐Yin and provided a relatively comprehensive approach for the assay of Qi‐Fu‐Yin, which is a promising advance in the quality control of Qi‐Fu‐Yin. Firstly, common peaks of Qi‐Fu‐Yin from batch‐to‐batch were determined and identified using HPLC fingerprints and UHPLC/MS. Subsequently, multiple statistical correlation analysis methods established a spectrum‐effect relationship, identifying potential antioxidant compounds, which were validated in vitro. Ultimately, by combining antioxidant and index compounds, quality control standards for Qi‐Fu‐Yin were established, providing crucial scientific evidence for its standardization and consistency. [ABSTRACT FROM AUTHOR]

Litchi chinensis Sonn (Litchi) has been listed in the Chinese Pharmacopeia, and is an economically and medicinally valuable species within the family Sapindaceae. However, the material basis of its pharmacological action and the pharmacodynamic substances associated with its hypoglycemic effect are still unclear. The predominant objective of this study was to establish the fingerprint profile of litchi leaves and to evaluate the relationship between the components of the high‐performance liquid chromatography (HPLC) fingerprint of litchi leaves, assess its hypoglycemic effect by measuring α‐glucosidase and α‐amylase inhibition, and find the spectrum–effect relationship of litchi leaves by bivariate correlation analysis, Grey relational analysis and partial least squares regression analysis. In this study, the fingerprint of litchi leaves was established by HPLC, and a total of 15 common peaks were identified that clearly calibrated eight components, with P1 being gallic acid, P2 being protocatechuic acid, P3 being catechin, P6 being epicatechin, P12 being rutin, P13 being astragalin, P14 being quercetin and P15 being kaempferol. The similarities between the fingerprints of 11 batches of litchi leaves were 0.766–0.979. Simultaneously, the results of the spectrum–effect relationship showed that the chemical constituents represented by peaks P8, P3, P12, P14, P2, P13, and P11 were relevant to the hypoglycemic effect. [ABSTRACT FROM AUTHOR]

Astragali Radix (AR) is one of the famous traditional Chinese medicines (TCMs) for boosting immunity, whereas the quality markers (Q‐markers) of AR have not been clearly researched. The immunomodulatory activities of the bioactive extractions and components were evaluated by NO inhibition rate; phagocytic index; IL‐10, TNF‐α, IL‐1β, and IL‐6 cytokines in RAW264.7 cells; and the relative proliferation rate of spleen cells. The total saponins (TS) and the grade 2 (Xiaoxuan, XX) of AR showed the strongest immunomodulatory activities. At the concentration of 40 μg/mL, the TS increased spleen cells proliferation by 48.0% and upregulated the level of IL‐1β and IL‐6. Cytokines in the XX‐treated group were at least 1.6 times higher than the control group. A total of 190 common peaks were detected in AR by ultrahigh‐performance liquid chromatography coupled with quadrupole‐time‐of‐flight mass spectrometry (UHPLC‐QTOF‐MS). The multivariate statistical analyses revealed that 41 compounds were positively correlated with immune responses, and bioactive compounds were verified by using RAW264.7 cell assay. Subsequently, the contents of six compounds in different commercial grades were determined, and the results showed the same trend in contents and activities. Finally, calycosin‐7‐O‐β‐D‐glucoside, astragaloside IV, astragaloside II, astragaloside I, isomucronulatol‐7‐O‐glucoside, and 9,10‐dimethoxypterocarpan‐3‐O‐glucoside were screened out as immunomodulatory Q‐markers of AR. [ABSTRACT FROM AUTHOR]

This research aimed to investigate the pharmacological components for liver stagnation and spleen deficiency syndrome (LSSDS) of Evodia rutaecarpa (also called Yu HuangLian [YHL]) by exploring the spectrum–effect relationship between fingerprints and pharmacological actions. The fingerprints of 17 batches of YHL with different preparation conditions according to Box–Behnken Design were generated and analyzed to identify the common peaks by HPLC and FT‐IR. Vasoactive intestinal peptide (vip), substance P, and 5‐HT levels in colon sample were measured by ELISA. Gray degree correlation and orthogonal partial least squares were employed to explore the correlation degree between components and pharmacologic activity. The presumed pharmacological components were further confirmed by network pharmacology, molecular docking, and qRT‐PCR. The columbamine, jatrorrhizine, coptisine, berberine, rutecarpine, and evodiamine of the 14 common peaks in HPLC fingerprints were significantly correlated with the pharmacological indexes. Similarly, there was a strong correlation with ‐OH, δNC‐H, and νC‐O‐C of the 10 common peaks in FT‐IR fingerprints. PTGS2 and CHRM3 were the main targets intervening LSSDS, and the presumed pharmacological components could markedly increase the expression of CHRM3 and obviously reduce the expression of PTGS2 compared with the model group. [ABSTRACT FROM AUTHOR]

Objective: To study the spectrum-effect relationship between the extracts of Tetrastigma hemsleyanum and its antioxidant activity, and to clarify the quality markers of its antioxidant activity. Methods: The extract was prepared and separated by macroporous resin elution, six different elution sites were obtained using ethanol at concentrations of 10%, 30%, 50%, 70%, 90% and 100%. The fingerprints of the Tetrastigma hemsleyanum extract and each elution site were established by UPLC-Q-TOF-MS and the characteristic peaks were screened. The free radical scavenging rate of 1,1-diphenyl-2-trinitrophenylhydrazine (DPPH) was used as an antioxidant index to investigate the antioxidant activity of the extract and each elution site of Tetrastigma hemsleyanum. The Pearson correlation coefficient method and orthogonal partial least squares (OPLS) method were combined to analyze and study the spectrum-effect relationship between the characteristic peaks and the antioxidant activity, to screen the quality markers, and to analyze and identify the chemical compositions. Results: Under the positive and negative ion modes, 57 and 92 characteristic peaks were identified in the extract and each elution site of Tetrastigma hemsleyanum, respectively. The combined results of Pearson correlation coefficient and OPLS analysis showed that 14 ion peaks contributed more to the antioxidant activity, which was vanillin (P2), catechin (P13, N19), rutin (P27, N54), and isoquercitrin (P28), kaempferol-3-O-rutinoside (P33, N61), proanthocyanidin B (N18), proanthocyanidin C (N22), and ion peaks N23, N25, N26, and N29, respectively. Conclusion: UPLC-Q-TOF-MS fingerprints of Tetrastigma hemsleyanum extract and each elution site were established, and the quality markers of Tetrastigma hemsleyanum antioxidant activity were revealed to provide technical support for the formulation of quality standards and resource development and utilization of Tetrastigma hemsleyanum.

Objective: The study was designed to test solvent extracts of Rubus suavissimus (RS) for compounds that regulate lipid metabolism and to measure their relative activity as quantitative markers of lipid metabolism-regulating activities based on the spectrum-effect relationship. Method: RS was extracted with 95% ethanol, the different extraction parts were successively extracted with petroleum ether, methylene chloride, ethyl acetate and n-butanol, respectively. The solution of different extraction parts was applied to the induced differentiated 3T3-L1 preadipocytes, and the oil red O staining and triglyceride release from the cells were determined to screen the best metabolism-regulating site. Analysis of different extraction sited by UPLC-Q-TOF-MS/MS technique to separate and identify the components. Based on specific assays, image intensity analysis, grey correlation and partial least squares regressions, the spectrum-effect relationship of the most abundant active components and their ability to regulate lipid metabolism were determined, and the quality markers were screened. Results: Ethyl acetate and n-butanol extraction site was the best metabolism-regulating site. Four components, including ellagic acid, centaurin-3-O-rutinoside, rubusoside and enantio-kauri-16-ene-19-carboxylic acid-13-O-β-D-glucoside were highly associated with metabolism-regulating effects. It could be used as quality markers for regulating lipid metabolism. Conclusion: Investigation of the quality markers of RS extracts based on the spectrum-effect relationship is of great importance for elucidating the pharmacodynamics, screening the core quality markers for therapeutic activity, and ensuring the safety and rational application of traditional medicines.

The objectives of this study were to optimize the ultrasonic-assisted flavonoid extraction process from PR and to establish fingerprints in order to analyze the spectrum–effect relationship of antioxidant activity. The ultrasonic-assisted flavonoid extraction process from PR was optimized using RSM, and the fingerprints of twenty-eight batches of flavonoids from PR were established using UHPLC. Meanwhile, the in vitro antioxidant activity of PR was evaluated in DPPH and ABTS free radical-scavenging experiments. Then, the peaks of the effective antioxidant components were screened using the spectrum–effect relationships. The results show that the optimal extraction yield of flavonoids from PR was 3.24 ± 0.01 mg/g when using 53% ethanol, a 1:26 (g/mL) solid–liquid ratio, and 60 min of ultrasonic extraction. Additionally, the clearance of two antioxidant indices by the flavonoids extracted from PR had different degrees of correlation and showed concentration dependence. Simultaneously, the similarity of the UHPLC fingerprints of twenty-eight batches of PR samples ranged from 0.801 to 0.949, and four characteristic peaks, namely peaks 4, 12, 21, and 24, were screened as the peaks of the components responsible for the antioxidant effect of PR using a GRA, a Pearson correlation analysis, and a PLS-DA. In this study, characteristic peaks of the antioxidant effects of PR were screened in an investigation of the spectrum–effect relationship to provide a scientific basis for the study of pharmacodynamic substances and the elucidation of the mechanism of action of the antioxidant effect of PR. [ABSTRACT FROM AUTHOR]

Copyright of Science & Technology of Food Industry is the property of Science & Technology of Food Industry Editorial Office and its content may not be copied or emailed to multiple sites or posted to a listserv without the copyright holder's express written permission. However, users may print, download, or email articles for individual use. This abstract may be abridged. No warranty is given about the accuracy of the copy. Users should refer to the original published version of the material for the full abstract. (Copyright applies to all Abstracts.)

Introduction: Artemisia absinthium L. is a well‐known medicinal, aromatic, and edible plant with important medicinal and economic properties and a long history of use in treating liver inflammation and other diseases; however, there has been insufficient progress in quality control. Objective: This study aimed to investigate the quality markers for the anti‐inflammatory and antioxidant activities of A. absinthium based on spectrum–effect relationship analysis. Materials and methods: Eighteen batches of A. absinthium from different origins were used. Chemical fingerprints were obtained by ultra‐performance liquid chromatography (UPLC). The chemical compositions were identified by quadrupole‐Orbitrap high‐resolution mass spectrometry. Anti‐inflammatory activity was assessed by inhibition of cyclooxygenase‐2 and 15‐lipoxygenase in vitro and inhibition of nitric oxide release in lipopolysaccharide‐induced BV‐2 cells. Antioxidant activity was assessed by DPPH and ABTS radical scavenging assays. The relationship between bioactivity and chemical fingerprints was then analyzed using chemometrics including gray relational analysis, bivariate correlation analysis, and orthogonal partial least squares analysis. Results: Different batches of A. absinthium extracts possessed significant anti‐inflammatory and antioxidant activities to varying degrees. Eighty compounds were identified from A. absinthium, and 12 main common peaks were obtained from the UPLC fingerprints. P3 (chlorogenic acid), P5 (isochlorogenic acid A), and P6 (isochlorogenic acid C) were screened as the most promising active compounds by correlation analysis and further validated for their remarkable anti‐inflammatory effects. Conclusion: This is the first study to screen the quality markers of A. absinthium by establishing the spectrum–effect relationship, which can provide a reference for the development of quality standards and further research on A. absinthium. The UPLC fingerprints of 18 batches of A. absinthium were established, and their anti‐inflammatory and antioxidant activities were investigated. The chemical compositions were identified. The active compounds were screened by spectrum‐effect relationship. Finally, chlorogenic acid, isochlorogenic acid A, and isochlorogenic acid C were screened as the main active compounds and validated experimentally. These compounds can be used as quality control markers for A. absinthium. This research provides a scientific basis and valuable reference for the quality control of A. absinthium. [ABSTRACT FROM AUTHOR]

Copyright of Journal of Guangdong Pharmaceutical University is the property of Journal of Guangdong Pharmaceutical University and its content may not be copied or emailed to multiple sites or posted to a listserv without the copyright holder's express written permission. However, users may print, download, or email articles for individual use. This abstract may be abridged. No warranty is given about the accuracy of the copy. Users should refer to the original published version of the material for the full abstract. (Copyright applies to all Abstracts.)

Objective: The study was designed to test solvent extracts of Rubus suavissimus (RS) for compounds that regulate lipid metabolism and to measure their relative activity as quantitative markers of lipid metabolism-regulating activities based on the spectrum-effect relationship. Method: RS was extracted with 95% ethanol, the different extraction parts were successively extracted with petroleum ether, methylene chloride, ethyl acetate and n-butanol, respectively. The solution of different extraction parts was applied to the induced differentiated 3T3-L1 preadipocytes, and the oil red O staining and triglyceride release from the cells were determined to screen the best metabolism-regulating site. Analysis of different extraction sited by UPLC-Q-TOF-MS/MS technique to separate and identify the components. Based on specific assays, image intensity analysis, grey correlation and partial least squares regressions, the spectrum-effect relationship of the most abundant active components and their ability to regulate lipid metabolism were determined, and the quality markers were screened. Results: Ethyl acetate and n-butanol extraction site was the best metabolism-regulating site. Four components, including ellagic acid, centaurin-3-O-rutinoside, rubusoside and enantio-kauri-16-ene-19-carboxylic acid-13-O-β-D-glucoside were highly associated with metabolism-regulating effects. It could be used as quality markers for regulating lipid metabolism. Conclusion: Investigation of the quality markers of RS extracts based on the spectrum-effect relationship is of great importance for elucidating the pharmacodynamics, screening the core quality markers for therapeutic activity, and ensuring the safety and rational application of traditional medicines. [ABSTRACT FROM AUTHOR]

Pueraria lobata (P. lobata), a traditional anti-diabetic medicine mainly composed of flavonoids and isoflavones, has a long history in diabetes treatment in China. However, the anti-diabetic active component is still unclear. Recently, protein tyrosine phosphatase 1B (PTP1B) has been a hot therapeutic target by negatively regulating insulin signaling pathways. In this study, the spectrum–effect relationship analysis method was first used to identify the active components of P. lobata that inhibit PTP1B. The fingerprints of 12 batches of samples were established using high-performance liquid chromatography (HPLC), and sixty common peaks were identified. Meanwhile, twelve components were identified by a comparison with the standards. The inhibition of PTP1B activity was studied in vitro by using the p-nitrophenol method, and the partial least squares discriminant analysis, grey relational analysis, bivariate correlation analysis, and cluster analysis were used to analyze the bioactive compounds in P. lobata. Peaks 6, 9 (glycitin), 11 (genistin), 12 (4′-methoxypuerarin), 25, 34, 35, 36, 53, and 59 were considered as potentially active substances that inhibit PTP1B. The in vitro PTP1B inhibitory activity was confirmed by glycitin, genistin, and 4′-methoxypuerarin. The IC50s of the three compounds were 10.56 ± 0.42 μg/mL, 16.46 ± 0.29 μg/mL, and 9.336 ± 0.56 μg/mL, respectively, indicating the obvious PTP1B inhibitory activity. In brief, we established an effective method to identify PTP1B enzyme inhibitors in P. lobata, which is helpful in clarifying the material basis of P. lobata on diabetes. Additionally, it is evident that the spectrum–effect relationship method serves as an efficient approach for identifying active compounds, and this study can also serve as a reference for screening bioactive constituents in traditional Chinese medicine. [ABSTRACT FROM AUTHOR]

In this study, the researchers produced a pear paste using typical Dangshan pear fruits. The mechanism that enables the paste to treat cough and related inflammatory responses was systematically investigated using an ammonia-induced mice cough model. The pear paste and its polar extracts relieved cough symptoms, as evidenced by 44.0%, 53.4%, and 47.2% decreases in cough frequency and 21.0%, 43.3%, and 53.4% increases in latent period for pear paste, ethyl acetate extract (EAE) and n-butanol extract (WBE), respectively. In addition, the paste and its polar extracts reduced lung injuries, including alveolar dilatation, alveolar wall damage, and airway thickening. The two polar extracts exhibited anti-inflammatory effects in the airway through the suppression of a Th1 cytokine (IFN-γ, significantly suppressed by 15.49% and 16.33% for EAE and WBE, separately). A spectrum-effect relationship analysis was conducted to identify arbutin, protocatechuic acid, chlorogenic acid and naringin as the primary bioactive substances contributing to the antitussive and anti-inflammatory activities of pear paste.

Terminalia chebula Retz. is commonly used in the treatment of diabetes, but its specific ingredients and hypoglycaemic mechanisms remain unclear. In this study, spectrum-effect relationships between common peaks of fingerprint and DPPH, ABTS, PTP1B, α-glucosidase, were used to screen six compounds as the potential hypoglycemic ingredients. Molecular docking studies were conducted on chebulagic acid, chebulinic acid and punicalagin, which were identified by reference standard, revealing the potent in teractions between these bioactive substances and the PTP1B, α-glucosidase protein. Additionally, the cellular level results showed that punicalagin displayed stronger inhibition of PTP1B and α-glucosidase, with IC50 values of 0.0236 and 0.335 μg/mL, respectively, while improving glucose consumption and intracellular glycogen content of insult-resistant L6 muscle cell, and the hypoglycemic effect was achieved by activating the PI3K/AKT signaling pathway. This study demonstrated that T. chebula has the potential to become a hypoglycemic functional food, and offers a strategy for characterization hypoglycemic ingredients.

Objective: This study aimed to investigate the orientated effective components of Astragali Radix Huangqi (HQ) in HQ Jianzhong Tang (HQJZ), a classical formula of traditional Chinese medicine (TCM) used for treating chronic atrophic gastritis (CAG), using HQ as a monarch medicine. Materials and Methods: The spectra of HQJZ containing different polar parts of HQ were obtained using ultra-high-performance liquid chromatography-Q-Exactive mass spectrometry. Furthermore, the efficacy of HQJZ, which contains different polar parts of HQ, in treating rats with CAG was evaluated using traditional pharmacodynamic and nuclear magnetic resonance-based metabonomics. Grey relation analysis and partial least squares analysis were applied to analyze the spectrum–effect relationship and to screen out the orientated effective components related to HQ in the treatment of CAG. Results: Spectrum–effect relationship analysis showed that 24 compounds identified from the fingerprint spectrum were strongly correlated with efficacy. Compounds 8 (calycosin-7-O-glc-6”- O-acetate), 9 (3-hydroxy-9, 10-dimethoxyptercarpan), and 22 (astragaloside II) were ranked among the top three. Conclusions: This study showed that integrating metabolomics and spectrum–effect relationship analysis is a powerful tool for obtaining orientated effective components of Chinese medicine in a given TCM formula.

Cnidii Fructus, derived from the dried ripe fruit of Cnidium monnieri (L.) Cuss, has the effect of warming kidneys and invigorating Yang. This study established the spectrum–effect relationships between ultra‐high‐performance liquid chromatography (UHPLC) fingerprints and the antitumor activities of Cnidii Fructus on human hepatocellular carcinoma (HepG2) cells. In UHPLC fingerprints, 19 common peaks were obtained, and 17 batches of herbs had similarity >0.948. In Cell Counting Kit‐8 (CCK‐8) test, 17 batches of Cnidii Fructus extract significantly inhibited the proliferation of HepG2 cells to different degrees, showing different half‐maximal inhibitory concentration (IC50) values. Furthermore, gray correlation analysis, Pearson's analysis, and orthogonal partial least squares discriminant analysis were performed to screen out eight components. The analysis of mass spectrum data and a comparison with standards revealed that the eight components were methoxsalen, isopimpinellin, osthenol, imperatorin, osthole, ricinoleic acid, linoleic acid, and oleic acid. The verification experiments by testing single compounds indicated that these eight compounds were the major anti‐hepatoma compounds in Cnidii Fructus. This work provides a model combining UHPLC fingerprints and antitumor activities to study the spectrum–effect relationships of Cnidii Fructus, which can be used to determine the principal components responsible for the bioactivity. [ABSTRACT FROM AUTHOR]

To enhance the quality evaluation and control of traditional Chinese medicine (TCM) and ensure the safety and efficacy of clinical medication, it is imperative to establish a comprehensive quality assessment method aligned with TCM efficacy. This study uses a representative Chinese medicine with multi‐origin and multi‐efficacy, Paris polyphylla var. yunnanensis (PY), as an illustrative example. Surprisingly, despite the high fingerprint similarity among the 12 batches of PY samples collected from various regions in Yunnan, a notable variation in the composition and content of components was observed. The chromatographic analysis identified seven common peaks, namely, polyphyllin I, polyphyllin II, polyphyllin V, polyphyllin VI, polyphyllin VII, polyphyllin H, and polyphyllin D. In the bioactivity evaluation, an in vitro antiplatelet aggregation model induced by adenosine diphosphate was established, showcasing excellent stability. The maximum antiplatelet aggregation inhibition rate for all PY samples consistently remained stable at 73.1%–99.1%. However, the 50% inhibitory concentration (IC50) values exhibited a range from 1.615 to 18.200 mg/mL. This approach not only meets high‐throughput screening requirements but also demonstrates remarkable discrimination. The results of chemical and bioactivity evaluations were analyzed using hierarchical cluster analysis and canonical correlation analysis. Polyphyllin I, polyphyllin II, polyphyllin VII, polyphyllin H, and polyphyllin D were identified as the Q‐markers for antiplatelet aggregation in PY samples. Validation of the bioactivity for these monomer components aligned with the previously mentioned findings. Notably, this study established a spectrum–effect model for PY samples, enhancing the scientific robustness of the quality evaluation method. Furthermore, these findings offer valuable research insights for improving the quality assessment of other TCMs. [ABSTRACT FROM AUTHOR]

Ardisia crenata Sims, an important ethnic medicine, is recorded in the Chinese Pharmacopoeia for treating laryngeal diseases and upper respiratory tract infections. This study aimed to evaluate the antimicrobial effect of extracts and potential antimicrobial compounds of A. crenata Sims. It was found that the roots of A. crenata Sims have a potential inhibitory effect on Candida albicans and Aspergillus flavus, with MICs of 1.56 mg/mL and 0.39 mg/mL, and the leaves of A. crenata Sims have a potential inhibitory effect on Pseudomonas aeruginosa and Staphylococcus aureus, with MICs of 3.12 mg/mL and 6.77 mg/mL, respectively. Meanwhile, five compounds including one catechin and four bergenins were obtained from roots. These components were identified on the fingerprint spectrum, representing chromatographic peaks 16, 21, 22, 23, and 25, respectively. Among these, 11-β-d-glucopyranosyl-bergenin and (−)-gallocatechin showed potential inhibition for Staphylococcus aureus and Pseudomonas aeruginosa with MIC of 0.26 and 0.33 mg/mL, respectively. The roots, stems, and leaves of A. crenata Sims are very similar in chemical composition, with large differences in content. Principal component analysis (PCA) and Hierarchical cluster analysis (HCA) showed that 16 batches of A. crenata Sims could be divided into four main production areas: Guizhou, Jiangsu, Guangxi, and Jiangxi. Furthermore, molecular docking results showed that 11-β-d-glucopyranosyl-bergenin had a better affinity for Casein lytic proteinase P (ClpP), and (−)-gallocatechin possessed a strong affinity for LasA hydrolysis protease and LasB elastase. These findings suggest catechin and bergenins from A. crenata Sims can be used as antimicrobial activity molecules. [ABSTRACT FROM AUTHOR]

The fingerprint of Vernonia anthelmintica effective part (VAEP) from 15 different producing areas was established, followed by cluster analysis and principal component analysis. The relationship between the fingerprint and the melanogenesis‐promoting activity of VAEP was then analyzed using the grey correlation degree and the orthogonal partial least square method. The characteristic peaks reflecting the pharmacodynamic effect of VAEP were identified as vernodalin, 3,5‐O‐dicaffeoyl quinic acid (3,5‐diCQA), and butin. Based on the distribution characteristics of these components in plants from different habitats and the verification of results from the spectrum–effect relationship, vernodalin and 3,5‐diCQA can be used as characteristic components for quality control and pharmacodynamic assessment of V. anthelmintica products. This research establishes a theoretical foundation for planting areas and provides a scientific evaluation of the melanogenesis‐promoting effect of V. anthelmintica. [ABSTRACT FROM AUTHOR]

Background: Kai-Xin-San (KXS) is one of the classic famous traditional Chinese medicine prescriptions for amnesia, which has been applied for thousands of years. Modern pharmacological research has found that KXS has significant therapeutic efficacy on nervous system diseases, which is related to its antioxidant activity. However, the antioxidant material basis and qualitymarkers (Q-makers) of KXS have not been studied. Objective: The objective of this study is to explore the Q-makers of antioxidant activity of KXS based on spectrum-effect relationship. Methods: Specifically, the metabolites in KXS extracts were identified by UPLC-Q-Exactive Orbitrap MS/MS. The fingerprint profile of KXS extracts were established by high-performance liquid chromatography (HPLC) and seven common peaks were identified. Meanwhile, 2, 2-diphenyl-1-picrylhydrazyl (DPPH) test was used to evaluate the free radical scavenging ability of KXS. The spectrum-effect relationship between its HPLC fingerprint and DPPH free radical scavenging activity was preliminarily examined by the Pearson correlation analysis, grey relation analysis (GRA), and orthogonal partial least squares discrimination analysis (OPLS-DA). Further, the antioxidant effect of KXS and its Q-makers were validated through human neuroblastoma (SH-SY5Y) cells experiment. Results: The results showed that 103 metabolites were identified from KXS, and the similarity values between HPLC fingerprint of twelve batches of KXS were greater than 0.900. At the same time, the results of Pearson correlation analysis showed that the peaks 8, 1, 14, 17, 18, 24, 16, 21, 15, 13, 6, 5, and 3 from KXSwere positively correlated with the scavenging activity values of DPPH. Combined with the results of GRA and OPLS-DA, peaks 1, 3, 5 (Sibiricose A6), 6, 13 (Ginsenoside Rg1), 15, and 24 in the fingerprints were screen out as the potential Q-makers of KXS for antioxidant effect. Besides, the results of CCK-8 assay showed that KXS and its Q-makers remarkably reduced the oxidative damage of SH-SY5Y cells caused by H2O2. However, the antioxidant activity of KXS was decreased significantly afterQ-makerswere knocked out. Conclusion: In conclusion, the metabolites in KXS were successfully identified by UPLC-Q-Exactive Orbitrap MS/MS, and the Q-makers of KXS for antioxidant effect was analyzed based on the spectrum-effect relationship. These results are beneficial to clarify the antioxidant material basis of KXS and provide the quality control standards for new KXS products development. [ABSTRACT FROM AUTHOR]

AbstractThe quality of Chinese herbal medicine (CHM) directly impacts clinical efficacy and safety. Fingerprint technology is an internationally recognized method for evaluating the quality of CHM. However, the existing quality evaluation models based on fingerprint technology have blocked the ability to assess the internal quality of CHM and cannot comprehensively reflect the correlation between pharmacodynamic information and active constituents. Through mathematical methods, a connection between the “Spectrum” (fingerprint) and the “Effect” (pharmacodynamic data) was established to conduct a spectrum-effect relationship (SER) of CHM to unravel the active component information associated with the pharmacodynamic activity. Consequently, SER can efficiently address the limitations of the segmentation of chemical components and pharmacodynamic effect in CHM and further improve the quality evaluation of CHM. This review focuses on the recent research progress of SER in the field of CHM, including the establishment of fingerprint, the selection of data analysis methods, and their recent applications in the field of CHM. Various advanced fingerprint techniques are introduced, followed by the data analysis methods used in recent years are summarized. Finally, the applications of SER based on different research subjects are described in detail. In addition, the advantages of combining SER with other data are discussed through practical applications, and the research on SER is summarized and prospected. This review proves the validity and development potential of the SER and provides a reference for the development and application of quality evaluation methods for CHM. [ABSTRACT FROM AUTHOR]

Dioscoreae hypoglaucae Rhizoma (DH) and Dioscoreae spongiosae Rhizoma (DS) are two similar Chinese herbal medicines derived from the Dioscorea family. DH and DS have been used as medicines in China and other Asian countries for a long time, but study on their phytochemicals and bioactive composition is limited. This present study aimed to compare the chemical compositions of DH and DS, and explore the anti-xanthine oxidase components based on chemometric analysis and spectrum–effect relationship. Firstly, an HPLC method was used to establish the chemical fingerprints of DH and DS samples, and nine common peaks were selected. Then, hierarchical clustering analysis, principal component analysis and orthogonal partial least squares discriminant analysis were employed to compare and discriminate DH and DS samples based on the fingerprints data, and four steroidal saponins compounds (protodioscin, protogracillin, dioscin, gracillin) could be chemical markers responsible for the differences between DH and DS. Meanwhile, the anti-xanthine oxidase activities of these two herbal medicines were evaluated by xanthine oxidase inhibitory assay in vitro. Pearson correlation analysis and partial least squares regression analysis were subsequently used to investigate the spectrum–effect relationship between chemical fingerprints and xanthine oxidase inhibitory activities. The results showed that four steroidal saponins, including protodioscin, protogracillin, methyl protodioscin and pseudoprogracillin could be potential anti-xanthine oxidase compounds in DH and DS. Furthermore, the xanthine oxidase inhibitory activities of the four selected inhibitors were validated by anti-xanthine oxidase inhibitory assessment and molecular docking experiments. The present work provided evidence for understanding of the chemical differences and the discovery of the anti-xanthine oxidase constituent of DH and DS, which could be useful for quality evaluation and bioactive components screening of these two herbal medicines. [ABSTRACT FROM AUTHOR]

ES contains compounds known to have significant anti-fatigue activity. In recent years, it has received extensive attention because it is efficient. However, its active ingredients on antifatigue effect are still unclear. This study attempts to establish the spectrum-effect relationship of ES antifatigue activity to screen the effective components. The results showed that the similarity of 15 ES fingerprints obtained by LC-MS/MS was 0.533-0.992, and the chemical structures of 22 common peaks were identified. The anti-fatigue activity of 15 batches of ES was characterized by forced swimming test of mice and quantified by CAFI, among which S4, S1 and S5 had better activity. 9 components (caffeic acid, 5-(4-O-β-D-glucosylferoyl)-quinic acid, (±)13-HODE, isofraxidin, eleutheroside E, syringin, pinoresinol diglucoside or its isomer, 7,8-dihydrodehydrocarbinol alcohol-4-O-β-D-glucoside, secoisolariciresinol-4-O-β-D-glucoside) highly related to antifatigue activity may be the effective components of ES. [ABSTRACT FROM AUTHOR]

An integrative strategy of UHPLC/IM-QTOF-MS analysis, MS/MS molecular networking (MN), in-house library search, and a collision cross-section (CCS) simulation and comparison was developed for the rapid characterization of the chemical constituents in Chebulae Fructus (CF). A total of 122 Constituents were identified, and most were phenolcarboxylic and tannic compounds. Subsequently, 1,3,6-tri-O-galloyl-β-d-glucose, terflavin A, 1,2,6-tri-O-galloyl-β-d-glucose, punicalagin B, chebulinic acid, chebulagic acid, 1,2,3,4,6-penta-O-galloyl-β-d-glucose, and chebulic acid, among the 23 common constituents of CF, were screened out by UPLC-PDA fingerprinting and multivariate statistical analyses (HCA, PCA, and OPLS-DA). Then, Pearson's correlation analysis and a grey relational analysis were performed for the spectrum-effect correlation between the UPLC fingerprints and the antioxidant capacity of CF, which was finally validated by an UPLC-DPPH• analysis for the main antioxidant constituents. Our study provides a global identification of CF constituents and contributes to the quality control and development of functional foods and preparations dedicated to CF. [ABSTRACT FROM AUTHOR]

In order to investigate the relationship between antioxidant efficacy and active components of Smilax riparia, the HPLC fingerprint of S. riparia extracts were determined, similarity evaluation and cluster analysis were carried out, while analysis software was used for PLSR to establish the spectra effect relationship, and validation test of in vitro anti-oxidation was carried out. The results were as follows: (1)HPLC fingerprints of 13 batches of S. riparia with 14 main common peaks were established. (2) Thirteen batches of S. riparia samples were grouped into two categories, the samples of S. riparia with close geographical location were clustered into one group, and the chemical fingerprints of S. riparia with close geographical location were highly similar. (3) PLSR showed that the areas of peaks 1, 2, 3, 5, 6, 9 and 14 in the fingerprint were positively correlated with the antioxidant effect, while the areas of peaks 4, 7, 8, 10, 11 and 12 were negatively correlated with the antioxidant effect, the VIP values of peaks 9, 11, 3, 4 and 5 were all greater than 1. (4) Peak 9 was oleanolic acid, Peak 10 was ursolic acid, and Peak 9 had the largest scavenging capacity for ABTS free radicals. Therefore, antioxidant efficacy of S. riparia is contributed by a combined action of multi-components rather than one component, and Peak 9 (oleanolic acid) may be the material basis of the antioxidation effect of S. riparia.

ABSTRACTThe spectrum-effect relationship between chemical fingerprints and antioxidant activities was established to evaluate the quality of Eucommiae Folium (EF) extracts and discover potential efficacy-associated quality markers. Characteristic fingerprints of different batches of EF extracts were generated by high-performance liquid chromatography (HPLC), and a similarity analysis was performed by hierarchical cluster analysis (HCA). Then the total antioxidant capacity assay kit with ferric reducing antioxidant assay (FRAP) method was used to determine antioxidant activity. The spectrum-effect relationship was established to identify the chemical constituents that impart antioxidant activities of Eucommiae Folium (EF) extracts using partial least squares regression (PLSR). HPLC fingerprints of EF extracts were established with the optimized chromatographic conditions: the mobile phase consisted 0.1% phosphoric acid -water (A) and acetonitrile (B), the detection wavelength was 326 nm, the column temperature was 30°C, and the flow rate was 0.8 mL/min. The correlation coefficient of similarity between 12 batches of extracts was ≥0.995. Compounds corresponding peaks P1, P2, P6 (chlorogenic acid), and P8 were closely related to the stable antioxidant activities of EF extracts, and could be selected as potential quality markers. An agile and efficient method that can ensure the intra-assay stability of biological activity of EF extracts and discover efficacy-associated quality markers was successfully built based on spectrum-effect relationship.

The objectives of this study were to optimize the ultrasonic-assisted flavonoid extraction process from PR and to establish fingerprints in order to analyze the spectrum–effect relationship of antioxidant activity. The ultrasonic-assisted flavonoid extraction process from PR was optimized using RSM, and the fingerprints of twenty-eight batches of flavonoids from PR were established using UHPLC. Meanwhile, the in vitro antioxidant activity of PR was evaluated in DPPH and ABTS free radical-scavenging experiments. Then, the peaks of the effective antioxidant components were screened using the spectrum–effect relationships. The results show that the optimal extraction yield of flavonoids from PR was 3.24 ± 0.01 mg/g when using 53% ethanol, a 1:26 (g/mL) solid–liquid ratio, and 60 min of ultrasonic extraction. Additionally, the clearance of two antioxidant indices by the flavonoids extracted from PR had different degrees of correlation and showed concentration dependence. Simultaneously, the similarity of the UHPLC fingerprints of twenty-eight batches of PR samples ranged from 0.801 to 0.949, and four characteristic peaks, namely peaks 4, 12, 21, and 24, were screened as the peaks of the components responsible for the antioxidant effect of PR using a GRA, a Pearson correlation analysis, and a PLS-DA. In this study, characteristic peaks of the antioxidant effects of PR were screened in an investigation of the spectrum–effect relationship to provide a scientific basis for the study of pharmacodynamic substances and the elucidation of the mechanism of action of the antioxidant effect of PR.

Pueraria lobata (P. lobata), a traditional anti-diabetic medicine mainly composed of flavonoids and isoflavones, has a long history in diabetes treatment in China. However, the anti-diabetic active component is still unclear. Recently, protein tyrosine phosphatase 1B (PTP1B) has been a hot therapeutic target by negatively regulating insulin signaling pathways. In this study, the spectrum–effect relationship analysis method was first used to identify the active components of P. lobata that inhibit PTP1B. The fingerprints of 12 batches of samples were established using high-performance liquid chromatography (HPLC), and sixty common peaks were identified. Meanwhile, twelve components were identified by a comparison with the standards. The inhibition of PTP1B activity was studied in vitro by using the p-nitrophenol method, and the partial least squares discriminant analysis, grey relational analysis, bivariate correlation analysis, and cluster analysis were used to analyze the bioactive compounds in P. lobata. Peaks 6, 9 (glycitin), 11 (genistin), 12 (4′-methoxypuerarin), 25, 34, 35, 36, 53, and 59 were considered as potentially active substances that inhibit PTP1B. The in vitro PTP1B inhibitory activity was confirmed by glycitin, genistin, and 4′-methoxypuerarin. The IC50s of the three compounds were 10.56 ± 0.42 μg/mL, 16.46 ± 0.29 μg/mL, and 9.336 ± 0.56 μg/mL, respectively, indicating the obvious PTP1B inhibitory activity. In brief, we established an effective method to identify PTP1B enzyme inhibitors in P. lobata, which is helpful in clarifying the material basis of P. lobata on diabetes. Additionally, it is evident that the spectrum–effect relationship method serves as an efficient approach for identifying active compounds, and this study can also serve as a reference for screening bioactive constituents in traditional Chinese medicine.

In order to study the spectrum-effect relationship between fingerprint and antioxidant activity of the leaves of Vitex negundo var. cannabifolia, the fingerprints of 18 batches of V. negundo var. cannabifolia leaves were established by high performance liquid chromatography-electrochemical detection (HPLC-ECD), and the cluster analysis of medicinal materials from different sources was performed simultaneously. The main phenolic compounds from V. negundo var. cannabifolia leaves were identified and determined. The contents of total phenolics and total flavonoids in V. negundo var. cannabifolia leaves were analyzed, and the antioxidant activities in vitro were evaluated by the methods of DPPH radical scavenging capacity, ABTS radical scavenging capacity, oxygen radical absorbance capacity and ferric ion reducing ability power. The spectrum-effect relationships of V. negundo var. cannabifolia leaves were analyzed by Pearson correlation analysis, gray relational analysis and partial least square regression analysis. The results were as follows: (1) The fingerprints of V. negundo var. cannabifolia leaves were established with 21 common peaks and a total of 10 peaks were identified. The order of content was chlorogenic acid > isoorientin > luteoloside > isovitexin > isochlorogenic acid A > isochlorogenic acid C > protocatechuic acid > orientin > isochlorogenic acid B > neochlorogenic acid. The similarity among the samples from different producing areas was high, and the values were ranged from 0.816 to 0.983. (2) The results of the cluster analysis showed that the content of the compounds had a certain influence on the classification and the samples from different sources were divided into three categories, among which the samples from the south and the north were different. (3) The contents of total phenolics and total flavonoids in V. negundo var. cannabifolia leaves were 15.82 to 61.83 mg·g-1 and 27.85 to 157.65 mg·g-1, respectively, and the antioxidant activity of all samples from V. negundo var. cannabifolia leaves existed differences. (4) The spectrum-effect relationship indicated that the antioxidant activity of V. negundo var. cannabifolia leaves was the result of the synergistic effect of many compounds, and compounds such as peak 9 (isoorientin), peak 4 and peak 5 (chlorogenic acid) made the greatest contribution to the antioxidant activity of V. negundo var. cannabifolia leaves. V. negundo var. cannabifolia has good antioxidant activity, and the main activity indexes are isoorientin and chlorogenic acid. This study can provide a reference basis for the screening and quality control of antioxidant components in V. negundo var. cannabifolia.

Valeriana jatamansi Jones (V. jatamansi) is an ethnomedicinal herb widely used worldwide for its excellent anti-inflammatory activity. However, the quality markers that were correlated with the anti-inflammatory activity in V. jatamansi remained unclear. This study aimed to identify combinatorial quality markers based on the anti-inflammatory effects of V. jatamansi for enhancing its quality control. The chemical constituents of V. jatamansi were identify by UPLC-Q-TOF-MS, and 36 compounds were identified. The anti-inflammatory mechanism was predicted by network pharmacology, STAT3 and JAK1 were selected as key targets. The anti-inflammatory activity and predicted targets were validated by using lipopolysaccharide (LPS)-stimulated RAW264.7 cells in vitro. A combination of bivariate correlation analysis (BCA) and grey correlation analysis (GCA) was applied to evaluate the correlation between the chemical spectrum and the anti-inflammatory activities. Hesperidin, acevaltrate and valtrate were screened as potential quality markers. These three compounds exhibited anti-inflammatory effects by inhibiting the production of inflammatory mediators (NO, IL-6, IL-1β and TNF-α) and suppressing the expression of the two key targets (JAK1 and STAT3). The quantitative analysis results showed that the contents of the combinatorial quality markers were positively correlated with the anti-inflammatory activity of V. jatamansi. The contribution rate of the combinatorial quality markers reached 45.0 %. This study provides a comprehensive strategy for the quality control of V. jatamansi based on combinatorial quality markers.

Weichang'an pill (WCAP) is a traditional Chinese patent medicine, which is clinically used for the treatment of bowel syndrome and functional dyspepsia such as diarrhea, abdominal distension, and enteritis. So far, quality control studies of WCAP have mainly focused on the determination of chemical composition content, which has little relevance to biological activity and clinical effects. With the aim of identifying the multi-index ingredients with NF-κB inhibitory activities related to WCAP clinical effect, this present work described the chemical profile of WCAP by UHPLC-QE-MS, established the correlated relationship between chromatographic fingerprints and the NF-κB inhibitory activities based on multivariate statistical analysis, including hierarchical clustering analysis (HCA), Pearson correlation analysis, and Partial least squares regression analysis (PLSR). The spectrum-effect relationship analysis indicated 10 compounds, which were ferulic acid, naringin, narirutin, hesperidin, neohesperidin, aloe emodin, emodin, honokiol, magnolol, and physcion, might be the potential NF-κB inhibitory constituents in the pill. The NF-κB inhibitory effects of the ten compounds were verified by in vitro dual luciferase reporting detection system. Considering that the detection index should be representative of more medicinal materials, a rapid and efficient UPLC-DAD method was eventually developed to determine the content of the 13 components. Our findings will provide data support for WCAP quality control and advance the understanding of the quality assessment of traditional Chinese patent medicines.

Background: Kai-Xin-San (KXS) is one of the classic famous traditional Chinese medicine prescriptions for amnesia, which has been applied for thousands of years. Modern pharmacological research has found that KXS has significant therapeutic efficacy on nervous system diseases, which is related to its antioxidant activity. However, the antioxidant material basis and quality markers (Q-makers) of KXS have not been studied. Objective: The objective of this study is to explore the Q-makers of antioxidant activity of KXS based on spectrum-effect relationship.Methods: Specifically, the metabolites in KXS extracts were identified by UPLC-Q-Exactive Orbitrap MS/MS. The fingerprint profile of KXS extracts were established by high-performance liquid chromatography (HPLC) and seven common peaks were identified. Meanwhile, 2, 2-diphenyl-1-picrylhydrazyl (DPPH) test was used to evaluate the free radical scavenging ability of KXS. The spectrum-effect relationship between its HPLC fingerprint and DPPH free radical scavenging activity was preliminarily examined by the Pearson correlation analysis, grey relation analysis (GRA), and orthogonal partial least squares discrimination analysis (OPLS-DA). Further, the antioxidant effect of KXS and its Q-makers were validated through human neuroblastoma (SH-SY5Y) cells experiment.Results: The results showed that 103 metabolites were identified from KXS, and the similarity values between HPLC fingerprint of twelve batches of KXS were greater than 0.900. At the same time, the results of Pearson correlation analysis showed that the peaks 8, 1, 14, 17, 18, 24, 16, 21, 15, 13, 6, 5, and 3 from KXS were positively correlated with the scavenging activity values of DPPH. Combined with the results of GRA and OPLS-DA, peaks 1, 3, 5 (Sibiricose A6), 6, 13 (Ginsenoside Rg1), 15, and 24 in the fingerprints were screen out as the potential Q-makers of KXS for antioxidant effect. Besides, the results of CCK-8 assay showed that KXS and its Q-makers remarkably reduced the oxidative damage of SH-SY5Y cells caused by H2O2. However, the antioxidant activity of KXS was decreased significantly after Q-makers were knocked out.Conclusion: In conclusion, the metabolites in KXS were successfully identified by UPLC-Q-Exactive Orbitrap MS/MS, and the Q-makers of KXS for antioxidant effect was analyzed based on the spectrum-effect relationship. These results are beneficial to clarify the antioxidant material basis of KXS and provide the quality control standards for new KXS products development.

Edible chrysanthemum is a common food resource for tea and functional foods with potential benefits for human health. Studies have indicated that chrysanthemum has the potential effect on inflammatory diseases, while the effects on gouty inflammation remain underexplored. The present study aimed to investigate the anti-gout activity and characterize the active ingredients of chrysanthemums by using metabolite profiles, in vitro experiments, and spectrum-effect analysis. Results showed that ‘Boju’ (BJ), ‘Hangbaiju’ (HBJ), and ‘Huaiju’ (HJ) exhibited regulatory effects on monosodium urate (MSU)-induced inflammation. At the dose of 50 µg/mL, the inhibitory rates of IL-1β secretion were 24.53 %, 14.36 %, and 38.10 %, respectively. A total of 32 phenolic compounds were identified or preliminarily assigned in UPLC-Q/TOF-MS analysis. And seven phenolics related to anti-gout activity were identified by spectrum-effect relationships. According to ADME (absorption, distribution, metabolism, excretion) evaluation and experiments verification, luteolin, acacetin-7-O-glucoside, and apigenin-7-O-glucoside were critical constituents potentially associated with the reduction of inflammation in gout. Additionally, these phenolics might be suitable as quality control indicators. This study clarified the anti-gout properties of different cultivars of chrysanthemums and active compounds, providing a theoretical basis for its scientific utilization in functional foods.

The aim of the test was to study the relationship between HPLC fingerprint of Forsythia suspensa leaves from different producing areas in Shiyan area and its antioxidant and antibacterial activity, and preliminarily determine its antioxidant and antibacterial active substance basis, and provide reference for its quality control methods. HPLC fingerprints of forsythia leaves from ten different producing areas in Shiyan area were constructed, and the common peaks were determined by TCM chromatographic fingerprint similarity evaluation system (2012 edition). The antioxidant activity was determined by ABTS+ free radical scavenging method, and the antibacterial activity of Forsythia suspensa leaves water extract against Staphylococcus aureus was determined by Oxford cup method. Grey correlation degree and principal component analysis were combined to elucidate the spectral effect relationship between multi-component and pharmacodynamic data in fingerprint. The results showed that 13 common peaks were identified by the fingerprint of water extracts from Forsythia suspensa leaves, and the correlation degree between the 12 common peaks and the antioxidant and antibacterial effects was greater than 0.6, and the comprehensive score of principal component analysis was also consistent with the actual pharmacological activity results. The study indicates that Forsythia suspensa leaves in Shiyan area have potential development, and the quality of Forsythia suspensa leaves in Hualongyan and Qingshi village is the best. The antioxidant and antibacterial activity of Forsythia suspensa leaves are the result of synergistic action of many components. Forsythia glucoside A, forsythia glucoside and rutin are strongly correlated with the pharmacodynamic base substances, and the overall activity of Forsythia suspensa leaves water extract was positively correlated with the content of these characteristic components. [ABSTRACT FROM AUTHOR]

In order to investigate the relationship between antioxidant efficacy and active components of Smilax riparia, the HPLC fingerprint of S. riparia extracts were determined, similarity evaluation and cluster analysis are carried out, while analysis software was used for PLSR to establish the spectra effect relationship, and validation test of in vitro anti-oxidation was carried out. The results were as follows: (1) HPLC fingerprints of 13 batches of S. riparia with 14 main common peaks were established. (2) Thirteen batches of S. riparia samples were grouped into two categories, the samples of S. riparia with close geographical location were clustered into one group, and the chemical fingerprints of S. riparia with close geographical location were highly similar. (3) PLSR showed that the areas of peaks 1, 2, 3, 5, 6, 9 and 14 in the fingerprint were positively correlated with the antioxidant effect, while the areas of peaks 4, 7, 8, 10, 11 and 12 were negatively correlated with the antioxidant effect, the VIP values of peaks 9, 11, 3, 4 and 5 were all greater than 1. (4) Peak 9 was oleanolic acid, Peak 10 was ursolic acid, and Peak 9 had the largest scavenging capacity for ABTS free radicals. Therefore, antioxidant efficacy of S. riparia is contributed by a combined action of multi-components rather than one component. Peak 9(oleanolic acid)may be the material basis of the antioxidation effect of S. riparia. [ABSTRACT FROM AUTHOR]

Objective To study the spectrum-effect relationship of Wuziyanzong pill on sperm damage protection. Methods The fingerprint of 12 batches of Wuziyanzong was established by UPLC method, and similarity evaluation was simultaneously performed with Similarity Evaluation System of Traditional Chinese Medicine Chromatographic Fingerprint. The common peaks were identified by comparing with the peaks of mixed chemical reference standards. Sperm suspension was prepared, and the oxidative damage model was induced by H202 system-produced reactive oxygen species (ROS). The effect of each batch of Wuziyanzong pill on the level of superoxide dismutase ( SOD) in the sperm model were investigated with vitamin C as the positive control. The spectrum-effect relationship of Wuziyanzong pill on sperm damage protection was elucidated based on the grey correlation analysis and the active ingredients were verified. Results There were 17 common peaks in the 12 batches of samples, and the similarity with the control fingerprint was more than 0. 9. A total of 12 common peaks were identified by comparison with the peaks of the mixed chemical reference standards including genipiganic acid, chlorogenic acid, ellagic acid, hypericin, isoquercetin, verbascoside, astragalin, quercetin, kaempferol, gomisin A, schisandrin A and schisandrin B. Each batch of Wuziyanzong all significantly increased the content of SOD, and showed a certain protection effect on sperm oxidative damage. Grey correlation coefficient showed that the synergistic effect of multiple components, and the contribution of hypericin, chlorogenic acid and isoquercetin to pharmacodynamic activity was 0. 85, 0. 82 and 0. 78, respectively. Different concentrations of hypericin all increased the level of SOD, and the activity of SOD in medium and high dose groups was significantly higher than that in model group ( P < 0. 001) . Conclusions The protective effect of Wuziyanzong pill on sperm damage attributed to the synergistic action of several components. The identified hyperoside, chlorogenic acid and isoquercetin were major components that contributed to antioxidant effect, and the protective effect of hyperoside on sperm oxidative damage was verified. [ABSTRACT FROM AUTHOR]

High performance liquid chromatography-electrochemical detection (HPLC-ECD) fingerprints of Cichorium intybus L. (chicory) of different origins were established. The antioxidant activities of chicory were evaluated in vitro by 1,1-diphenyl-2-picrylhydrazyl (DPPH), [2,2'-azino-bis-(3-ethylbenzothiazoline-6-sulfonic acid)] (ABTS+) radical scavenging assays and ferric reducing antioxidant power (FRAP) assays. The "spectrum-effect" relationship between the fingerprint and antioxidant activities of chicory was analyzed using Pearson correlation analysis, partial least squares regression (PLSR) analysis, and gray correlation analysis (GRA) to identify the active antioxidant compounds. In total, 13 phenolic compounds were identified from the fingerprint of 21 batches of chicory from different regions. The total phenol content of chicory extract was up to 30.76 mg GAE/g, and the correlation coefficient between peak areas and antioxidant activity was >0.92. According to "spectrum-effect" relationship analyses, chicoric acid, caftaric acid, isochlorogenic acid B, isochlorogenic acid A, 1,5-dicaffeoylquinic acid, and isochlorogenic acid C comprised the components primarily contributing to the antioxidant activity of chicory, indicating significant correlations between these chemical compounds and antioxidant activity (P<0.01). The HPLC-ECD fingerprint of chicory established in this study combined with the statistical analysis method exploring the "spectrum-effect"not only indicate the differences in chemical compounds between samples but also directly demonstrate the antioxidant activity of samples. This method is simple and reliable, providing a reference for improving the quality evaluation and product development of chicory. [ABSTRACT FROM AUTHOR]

Ardisia crenata Sims, an important ethnic medicine, is recorded in the Chinese Pharmacopoeia for treating laryngeal diseases and upper respiratory tract infections. This study aimed to evaluate the antimicrobial effect of extracts and potential antimicrobial compounds of A. crenata Sims. It was found that the roots of A. crenata Sims have a potential inhibitory effect on Candida albicans and Aspergillus flavus, with MICs of 1.56 mg/mL and 0.39 mg/mL, and the leaves of A. crenata Sims have a potential inhibitory effect on Pseudomonas aeruginosa and Staphylococcus aureus, with MICs of 3.12 mg/mL and 6.77 mg/mL, respectively. Meanwhile, five compounds including one catechin and four bergenins were obtained from roots. These components were identified on the fingerprint spectrum, representing chromatographic peaks 16, 21, 22, 23, and 25, respectively. Among these, 11-β-d-glucopyranosyl-bergenin and (−)-gallocatechin showed potential inhibition for Staphylococcus aureus and Pseudomonas aeruginosa with MIC of 0.26 and 0.33 mg/mL, respectively. The roots, stems, and leaves of A. crenata Sims are very similar in chemical composition, with large differences in content. Principal component analysis (PCA) and Hierarchical cluster analysis (HCA) showed that 16 batches of A. crenata Sims could be divided into four main production areas: Guizhou, Jiangsu, Guangxi, and Jiangxi. Furthermore, molecular docking results showed that 11-β-d-glucopyranosyl-bergenin had a better affinity for Casein lytic proteinase P (ClpP), and (−)-gallocatechin possessed a strong affinity for LasA hydrolysis protease and LasB elastase. These findings suggest catechin and bergenins from A. crenata Sims can be used as antimicrobial activity molecules.

Essential hypertension (EH) is a leading cause of cardiovascular morbidity and mortality. Fructus Tribuli (FT), as a traditional medicine, has been frequently used for thousands of years. The crude Fructus Tribuli (CFT), decoction pieces being processed to remove impurities, have been listed as an important medicine for the treatment of hypertension in the elderly. According to the theory of traditional Chinese medicine, the CFT can enhance the EH treatment after being stir-fried into stir-fried Fructus Tribuli (SFT). At present, whether the SFT can enhance the EH treatment and its potential pharmacodynamic substances and mechanism are unknown. In this study, an integrated ''spectrum-effect relationship-network pharmacology-metabolomics'' strategy was used. Using male spontaneously hypertensive rats as an experimental model, we compared the therapeutic effects of CFT and SFT on EH. Subsequently, to define the pharmacodynamic material basis of SFT in enhancing the EH treatment, the steroidal saponins (main active components of FT) were selected for spectrum-effect relationship analysis. Furthermore, we applied the joint pathway analysis of network pharmacology and metabolomics to explore the underlying mechanism of SFT in enhancing the EH treatment. Results showed that SFT was better than CFT in the EH treatment. The steroidal saponins transformed by stir-frying were the potential pharmacodynamic substances that SFT could enhance the EH treatment. And the mechanism of action might be associated with regulating glycerophospholipid metabolism and arachidonic acid metabolism, especially arachidonic acid metabolism. This study provided a scientific basis for the clinical use of SFT as an important medicine for the EH treatment.

Introduction: The current quality evaluation of traditional Chinese medicine (TCM) is difficult to attribute to clinical efficacy due to the complexity of TCM. Zishen Yutai pill (ZYP), a well-known traditional Chinese patent medicine, has been widely used to prevent recurrent miscarriage and treat threatened abortion. However, the chemical components of ZYP are unknown, and there is no convincing quality control method applied on ZYP. Although ZYP has been found to promote endometrial receptivity and treat impending abortion, the substantial basis of the therapeutic effects is unclear. The aim of this study was to clarify the quality markers correlated with the potential medicinal activities and provide a theoretical foundation for scientific quality control and product quality improvement of ZYP. Methods: The chemical constituents of ZYP were comprehensively analyzed by offline two-dimensional liquid chromatography-mass spectrometry (2DLC-LTQOrbitrap-MS). The efficacy of the 27 ZYP orthogonal groups was investigated using the HTR-8/SVneo oxidative damage model and migration model in vitro, as well as the endometrial receptivity disorder mouse model and premature ovarian failure mouse model in vivo. Based on the efficacy and mass spectral results, spectrum-effect relationship analysis was used to identify the chemical components with corresponding pharmacological activities. Results: A total of 589 chemical components were found in ZYP, of which 139 were not identified in the literature. The potential quality markers for ZYP were successfully identified through orthogonal design and spectrum-effect relationship analysis. By combining mass spectrum data and pharmacological results of 27 orthogonal groups, 39 substances were identified as potential quality markers. Conclusion: The approaches used in this study will provide a feasible strategy for the discovery of quality markers with bioactivity and further investigation into the quality evaluation of TCM. [ABSTRACT FROM AUTHOR]

In order to study the spectrum-effect relationship between fingerprint and antioxidant activity of the leaves of Vitex negundo var. cannabifolia, the fingerprints of 18 batches of V. negundo var. cannabifolia leaves were established by high performance liquid chromatography-electrochemical detection(HPLC-ECD), and the cluster analysis of medicinal materials from different sources was performed simultaneously. The main phenolic compounds from V. negundo var. cannabifolia leaves were identified and determined. The contents of total phenolics and total flavonoids in V. negundo var. cannabifolia leaves were analyzed, and the antioxidant activities in vitro were evaluated by the methods of DPPH radical scavenging capacity, ABTS radical scavenging capacity, oxygen radical absorbance capacity and ferric ion reducing ability power. The spectrum-effect relationships of V. negundo var. cannabifolia leaves were analyzed by Pearson correlation analysis, gray relational analysis and partial least square regression analysis. The results were as follows:(1)The fingerprints of V. negundo var. cannabifolia leaves were established with 21 common peaks and a total of 10 peaks were identified. The order of content was chlorogenic acid > isoorientin > luteoloside > isovitexin > isochlorogenic acid A > isochlorogenic acid C > protocatechuic acid > orientin > isochlorogenic acid B > neochlorogenic acid. The similarity among the samples from different producing areas was high, and the values were ranged from 0.816 to 0.983.(2)The results of the cluster analysis showed that the content of the compounds had a certain influence on the classification and the samples from different sources were divided into three categories, among which the samples from the south and the north were different.(3)The contents of total phenolics and total flavonoids in V. negundo var. cannabifolia leaves were 15.82 to 61.83 mg·g-1 and 27.85 to 157.65 mg·g-1, respectively, and the antioxidant activity of all samples from V. negundo var. cannabifolia leaves existed differences.(4)The spectrum-effect relationship indicated that the antioxidant activity of V. negundo var. cannabifolia leaves was the result of the synergistic effect of many compounds, and compounds such as peak 9(isoorientin), peak 4 and peak 5(chlorogenic acid)made the greatest contribution to the antioxidant activity of V. negundo var. cannabifolia leaves. V. negundo var. cannabifolia has good antioxidant activity, and the main activity indexes are isoorientin and chlorogenic acid. This study can provide a reference basis for the screening and quality control of antioxidant components in V. negundo var. cannabifolia. [ABSTRACT FROM AUTHOR]

Chrysanthemi Flos (Juhua), an edible herbal medicine that possesses efficacies of dispersing wind, clearing heat and detoxifying. Studies have demonstrated that the health benefits of Chrysanthemi Flos are largely attributable to its anti‐inflammatory effects. However, the correlation between the compounds monitored by the current quality control methods and the anti‐inflammatory effects of Chrysanthemi Flos is unclear. In order to better control the quality of Chrysanthemi Flos, the identification of anti‐inflammatory quality markers (Q‐markers) of Chrysanthemi Flos was performed. The chemical components of Chrysanthemi Flos were profiled by HPLC fingerprints combined with chemometrics methods. Simultaneously, the anti‐inflammatory activities of 10 batches of water extracts of Chrysanthemi Flos were evaluated in lipopolysaccharide‐activated RAW 264.7 macrophages cells. Gray correlation analysis was performed to assess the relationship between the anti‐inflammatory activity and chemical properties. The results showed that 13 common peaks were closely correlated with the anti‐inflammatory effect, and further bioactivity re‐evaluation confirmed that 10 known compounds exerted a strong anti‐inflammatory effect. The quantitative analysis of the 10 Q‐markers showed that the 25 batches of samples could be discriminated into different zones according to their producing areas. Conclusively, the present work identified 10 anti‐inflammatory Q‐markers of Chrysanthemi Flos using spectrum–effect relationships combined with bioactivity re‐evaluation. [ABSTRACT FROM AUTHOR]

Nutricines, the nutritionally active substances in feed, play a vital role in enhancing immune function, antioxidant activity, and feed efficiency in dairy cows. Identifying nutricines in total mixed ration (TMR) provides insights into feed quality and their impact on dairy cow health. However, due to the structural diversity of nutricines, data mining using multivariate variable models faces challenges in exploring their relationships. To address this, this study established a hierarchical clustering and optimization factor strategy for 13 common flavonoid peaks detected using apparent data and HPLC-DAD. The establishment of the flavonoid fingerprint of TMR diet in dairy cows detected 13 common peaks, five of which were found using standard products: p-coumaric acid, sinapic acid, tricin, and diosmetin. In vitro fermentation results using different TMR samples in substrate fermentation indicated that the dry matter disappearance rate, NH3-N, acetate, propionate, butyrate, isovalerate, and valerate changes varied significantly (p < 0.05). In spectrum–activity relationship studies, P2, P6, P8, P9, P10, and P11 were all considered possible factors causing this effect. In the analysis of optimization factor strategy, the peak spectrum model of four fermentation parameters, i.e., pH, dry matter digestibility, NH3-N, and acetate, was constructed after optimization (p < 0.05), and the data model is listed in the main text. In structure–activity relationship studies, ferulic acid, isoferulic acid, methyl sinapic acid, methyl 4-hydroxycinnamate, and p-hydroxybenzalacetone may serve as candidate references for compound 10 and may play an important role in affecting the digestibility of dry matter in in vitro fermentation. These findings highlight the role of flavonoids in TMR feed as key factors in maintaining dairy cow health and differentiating nutritional value. This study proposes a novel method for future TMR diet formulation and quality evaluation, with potential implications for improving dairy cow health and performance. Further research is needed to validate these findings and elucidate the mechanisms underlying nutricine effects on dairy cow nutrition and health. [ABSTRACT FROM AUTHOR]

Lonicerae japonicae Flos (LF) is a kind of healthcare food with hepatoprotective function. This study was designed to explore the spectrum-effect relationships between UPLC fingerprints and the hepatoprotective effects of LF. Fingerprints of ten batches of LF were established by UPLC-PDA. The inhibitory levels of AST and ALT were used as pharmacological indexes, and secoxyloganin, isochlorogenic acid A and isochlorogenic acid C were screened as hepatoprotective active compounds by grey relational analysis (GRA) and partial least squares regression analysis (PLSR). Caspase-3 was obtained by network pharmacology as a key target of hepatoprotective active compounds. Molecular docking is used to explore the interaction between small molecules and proteins. This work provided a general model of the combination of UPLC-PDA and hepatoprotective effect to study the spectrum-effect relationship of LF, which can be used to considerable methods and insight for the fundamental research of the material basis of similar healthcare food.

Similarity analysis of complicated chromatographic profiles is a potential protocol for the authentication and quality control of traditional Chinese medicine to guarantee prospective biological activity. In this work, a high-performance liquid chromatography (HPLC) method was established to identify and control the inter-assay quality of extract from Artemisia frigida Willd. Meanwhile, a partial least squares regression (PLSR) was applied to construct a spectrum–effect relationship between the HPLC fingerprints and the total antioxidant capacity of the extract from Artemisia frigida Willd. The similarity correlation coefficient of 10 batches of extract was ≥0.948 could guarantee the 10 batches of showed the inter-assay stability of antioxidant capacity of extract from Artemisia frigida Willd. Moreover, PLSR analysis showed that four efficacy-related components were closely related to antioxidant effect. Therefore, this study provided a flexible and efficient method for the quality and the stable biological activity assessment of Artemisia frigida Willd.

Itea ilicifolia Oliv is a folk medicine with antioxidant potential. In this study, the fingerprints of 14 batches of I. ilicifolia were established by HPLC with 17 common peaks. The similarities evaluated by Similarity Evaluation System for Chromatographic Fingerprint of Chinese Materia (version 2012) were >0.89. Ten compounds were identified with definite structures by comparing the retention time and characteristic UV spectral pattern with those of reference substances. The antioxidant capacities of 14 batches of I. ilicifolia were evaluated based on O2·−, DPPH and ABTS·+ radical scavenging assays in combination with ferric reducing antioxidant power assay. Via multivariate statistical analyses of gray relation analysis, bivariate correlation analysis and partial least squares regression analysis, a study on the spectrum–effect relationship was then performed to screen eight peaks as the antioxidant Q‐markers of I. ilicifolia. The contents of representative antioxidant Q‐markers (isoorientin, orientin, vitexin, isovitexin and iteafuranal A) in samples were accurately determined to be 0.054–0.118%, 0.034–0.080%, 0.018–0.055%, 0.031–0.091% and 0.033–0.140%, respectively. The qualitative and quantitative analytical method based on Q‐markers helps to control the antioxidant quality of I. ilicifolia, which will lay the foundation to promote the rational utilization of I. ilicifolia in curing diseases related to oxidative stress. [ABSTRACT FROM AUTHOR]

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Tetrastigma hemsleyanum Diels et Gilg. (T. hemsleyanum) is an economically and medicinally valuable species within the genus Tetrastigma. However, the material basis of its pharmacological action and the biomarkers associated with its anti-cancer and anti-inflammatory effects are still unclear. Additionally, the T. hemsleyanum industry cannot grow because there is a lack of a scientific, universal, and measurable quality control system. This study aimed to explore the chemical basis quality markers related to the anti-cancer and anti-inflammatory effects of T. hemsleyanum to establish an effective quality evaluation method. UPLC-Q-TOF-MSE fingerprint profiles of T. hemsleyanum from different origins were established. Pharmacodynamic studies used HepG2 and HuH-7 cells and LPS-induced RAW264.7 to evaluate the anti-tumor and anti-inflammatory effects of the active ingredients. The spectrum-effect relationships between UPLC fingerprints and anti-cancer and anti-inflammatory activities were evaluated using PCA and PLSR statistical methods. Moreover, docking analysis was performed to identify specific active biomarkers with molecular targets associated with cancer and inflammation. Chlorogenic acid, quinic acid, catechin, kaempferol 3-rutinoside, apigenin-8-C-glucoside, and linolenic acid were associated with anticancer activity, while chlorogenic acid, quercetin, quinic acid, kaempferol 3-rutinoside, rutinum, apigenin-8-C-glucoside, and linolenic acid were associated with anti-inflammatory activity. The spectrum-effect relationship of T. hemsleyanum was successfully established, and the biomarkers for anti-cancer and anti-inflammatory effects were preliminary confirmed. These findings provide a theoretical basis for the elucidation of the substance basis of T. hemsleyanum and lay the foundation for its rapid identification, quality control, industrial research, and utilization. [ABSTRACT FROM AUTHOR]

Recent studies have demonstrated that the essential oil of Nardostachys jatamansi (EONJ) has potential health benefits, such as reducing blood pressure, protecting the heart, and relaxing blood vessels. However, the active constituents and the underlying molecular mechanisms are still unclear. In this study, we utilized GC–MS to identify the chemical constituents of EONJ and tested its vasodilatory effects on constricted isolated thoracic aorta rings from mice. We then combined network pharmacology with spectrum-effect relationship approaches to select potential marker ingredients and uncover the possible vascular protective mechanism of EONJ. Among the four main chemicals screened in this work, β-maaliene and patchouli alcohol exhibited varying levels of vasodilatory effects on isolated, constricted thoracic aortic rings. Bioinformatics and network pharmacology analyses revealed that EONJ's primary biological regulation targets were NOS3 and PTGS2. Moreover, EONJ may exert its vasodilatory effects by modulating lipid and atherosclerosis and the PI3K-AKT signaling pathways. This study provides the first report on the vasodilatory effects and possible molecular mechanisms of EONJ. The findings may serve as a reference for quality evaluation, identification of bioactive markers, and future applications of EONJ in the prevention and treatment of vascular and cardiac diseases.