Spectrum-effect Relationship Research Articles

A new method for studying the mechanism of “Feature Identification based quality assessment” of Traditional Chinese Medicine, taking Gastrodiae Rhizoma as an example

Aim of the studyThe research group proposed that the mechanism of “Feature Identification based Quality Assessment” (FIQA) of Traditional Chinese Medicine (TCM) can be explained according to the relationship between the “Feature” of TCM and the Pharmacodynamic Components representing the holistic effect of TCM. Gastrodiae Rhizoma (GR) was selected as the research object to reveal the close relationship between “Feature” and the quality of TCM. Materials and methodsIn this study, the “Feature” such as “Shape”, “Color”, “Odour” and “Taste” of GR are quantified by the electronic nose, electronic tongue, and other instruments. Then, the Pharmacodynamic Components Group (PCG) of GR was determined which could reflect the holistic effect of GR by spectrum effect relationship analysis. By analyzing the correlation between the “Feature” and the content of PCG, the mechanism of FIQA of GR was determined. ResultsThe quantitative results of “Shape”, “Color”, “Odour” and “Taste” of GR from different sources were significantly different. Six components were selected as the PCG, which can represent the holistic effect of GR in the aspect of the neuroprotective effect. There was a good correlation between the components in the PCG and “Feature”. ConclusionsThe quality of GR can be determined quantitatively according to its “Shape”, “Color”, “Odour” and “Taste”. The mechanism of FIQA of TCM can be explained according to the relationship between the Shape of TCM and the Pharmacodynamic Components representing the quality of TCM. The revelation of this mechanism reflects the holistic characteristics of the multi-component synergistic effect of TCM. This study provides a reference research method for revealing the mechanism of FIQA of TCM.

Spectrum-effect relationship between HPLC fingerprint and antioxidant of “San-Bai Decoction” extracts

“San-Bai Decoction” (SBD) has been a traditional Chinese medicine compound preparation for replenishing Qi and promoting blood circulation, whitening skin, and removing blemishes since ancient times. However, its chemical composition and antioxidant activity are not clear thus far, which limits the in-depth study on its pharmacodynamic material basis and efficacy. The objective of this study was to establish the fingerprint profile of SBD, assess its antioxidant activity by measuring 2,2-diphenyl-1-picrylhydrazyl (DPPH) radical scavenging ability, and find the spectrum-effect relationship of SBD by Grey Relation Analysis (GRA) and Partial Least Squares Regression (PLS). In this study, the fingerprint of SBD was established by high performance liquid chromatography (HPLC), and 20 common peaks were found, among which 6 peaks were designated. The similarities between the fingerprints of 12 batches of SBD and the reference fingerprint (R) were all greater than 0.900. Meanwhile, the antioxidant activities of all batches were concentration-dependent in their linear regression equation. The result of GRA showed that the correlation order of 20 common peaks for DPPH radical scavenging was X13 > X7 > X3 > X6 > X10 > X11 > X4 > X12 > X2 > X18 > X9 > X5 > X19 > X1 > X20 > X16 > X17 > X15 > X8 > X14. At the same time, PLS study demonstrated that the contribution of six identified characteristic peaks to DPPH radical scavenging ability was X1 = X7 > X6 > X19 > X20 > X16. In this study, the spectrum-effect relationship of SBD between its HPLC fingerprint and the antioxidant activity can be used to screen the pharmacodynamic substance basis of its antioxidant action and lay the foundation for establishing quality standards and product development.

Compound synthesizing profiling based on quantitative HPLC fingerprints combined with antioxidant activity analysis for Zhizi Jinhua pills

BackgroundCompound drug Zhizi Jinhua Pills (ZZJHP) is composed of 8 herbal medicines (HMs), and it is necessary to control the HMs to ensure its holistic quality. PurposeTo establish a quality monitoring method for ZZJHP from precise control of multiple active ingredients to contour control of fingerprint, to calculate the contribution of HMs and predict the quality of compound drugs. MethodsIn this study, HPLC method was established for content determination of 11 analytes and fingerprint assessment. In vivo and in vitro studies of antioxidant activity were performed, Orthogonal Partial Least Squares analysis was applied for spectrum-effect correlation between antioxidant activity and HPLC fingerprint. The compound synthesizing fingerprint (CSF) of ZZJHP was fitted with 8 HMs, and the contribution of the single herb to prescription was evaluated by Sub-quantified profiling method. ResultsThe content of 11 analytes and fingerprints of ZZJHP were measured simultaneously, 32 batches of samples were divided into 6 grades. In vivo and in vitro researches suggested significant antioxidant activity capacity of ZZJHP. Then, spectrum-effect relationship study showed that 24 of the 30 fingerprint peaks had antioxidant activity. By prescription and decomposition profiling, the qualitative and quantitative contributions of the 8 herbs were revealed in turn. The negative solution experiment proved that CSF could accurately predict the quality of composite drugs. ConclusionThe intelligent prediction strategy could intervene at the source to realize rapid screening of HMs and prediction of the quality of preparations, which could provide guidance for the use of HMs and improve the quality of composite drugs.

Screening of acetylcholinesterase inhibitory and antioxidant active compounds from Terminalia chebula fruits by spectrum‐effect relationship and liquid chromatography‒mass spectrometry analysis

Screening and identification of active components from traditional Chinese medicines is rather challenging due to the diversity and complexity of chemical components. Herein, a comprehensive strategy based on a spectrum-effect relationship model and LC-MS analysis was developed to screen active components from Terminalia chebula fruits. The water extract of T. chebula fruits was subjected to macroporous resin column and then eluted successively with water and 30%, 50%, 70%, and 95% ethanol. The 30% ethanol eluate fractions of eighteen batches from T. chebula fruits were used for the spectrum-effect relationship study. The IC50 values for acetylcholinesterase inhibitory and 2,2-diphenyl-1-picrylhydrazyl scavenging activities were measured, LC fingerprints were established, and 15 common peaks were specified. The spectrum-effect relationship between common peaks and IC50 values was investigated by principal component analysis, gray relational analysis, partial least square and multiple linear regression. The 30% ethanol eluate fraction was further characterized by LC-MS analysis. The chromatographic peaks (Peaks 1, 2, 3, 5, 12, 14, 15) making great contributions to the efficacy were screened through a spectrum-effect relationship model, and sixteen components were further identified. The results suggested that the proposed strategy is simple and effective for acquiring active components from a complex matrix.

Combining ultra-high-performance liquid chromatography quadruple exactive orbitrap mass spectrometry with chemometrics to identify and verify the blood-activating components of hawthorn.

Hawthorn, one of the widely-used Chinese herbal medicines, has been used to treat blood stasis syndrome in the clinic, but its blood-activating components are unclear. This study combined the ultra-high-performance liquid chromatography-quadruple exactive-orbitrap mass spectrometry with chemometrics to identify the blood-activating components of hawthorn. Different polar fractions of hawthorn aqueous extracts were extracted and mixed to prepare 14 samples. The contents of 25 chemical components for 14 samples were determined by the proposed quantitative method which was validated in terms of linearity, precision, stability, repeatability, and recovery, while the blood-activating effect was evaluated by measuring the whole blood viscosity, plasma viscosity, and plasma fibrinogen levels. Then the partial least squares model was established on the spectrum-effect relationship. The result showed that vitexin-2″-O-rhamnoside, rutin, citric acid, malic acid, gallic acid, and fumaric acid could reduce the whole blood viscosity, plasma viscosity, and plasma fibrinogen levels in blood stasis model rats, and these components were the blood-activating components of hawthorn. This study provided a scientific basis for clarifying the blood-activating components of hawthorn, and the spectrum-effect approach proved to be an effective approach to discovering the bioactive components of Chinese herbal medicines.

Spectrum-effect relationship between HPLC fingerprints and inhibitory activity in MUC5AC mucin of Pinelliae Rhizoma Praeparatum Cum Alumine

Purpose: To investigate the spectrum-effect relationship between HPLC fingerprints and the inhibitory effect on MUC5AC mucin of Pinelliae Rhizoma Praeparatum Cum Alumine (PRPCA).Methods: The fingerprints of 20 PRPCA batches were established using HPLC and their similarities or differences were analyzed using hierarchical cluster analysis (HCA) and principal component analysis (PCA). The inhibitory effects of MUC5AC mucin were evaluated in LPS-treated NCI-H292 cells. The spectrum-effect relationship between common chromatographic peaks and MUC5AC inhibition was established using a partial least squares-discriminant analysis (PLS-DA).Results: Fifteen common chromatographic peaks were identified by analyzing HPLC fingerprints, with uridine, tyrosine, uracil, and inosine found as possible markers to distinguish the PRPCA from different sources. Spectrum-effect relationship analysis showed that the chromatographic peaks 5, 6, 10 (vernine), 12 (5-hydroxymethylfurfural), 14 (tryptophan) and 15 (adenosine) were closely associated with the inhibitory effect on MUC5AC mucin.Conclusion: The spectrum-effect relationship between HPLC fingerprints and the inhibitory effect on MUC5AC mucin of PRPCA was successfully established in the present study. Our findings further reveal the material basis of PRPCA and provide an effective method for its quality control.

Exploring the Q-markers of Angelica sinensis (Oliv.) Diels of anti-platelet aggregation activity based on spectrum-effect relationships.

The radix of Angelica sinensis (Oliv.) Diels (RAS) is widely used in medicinal and dietary applications in China, and has the function for replenishing and invigorating the blood, stopping pain and moistening the intestines. In this study, RAS from the main geoherb regions showed better efficacy in inhibiting Adenosine diphosphate- or arachidonic acid-induced platelet aggregation than those from non-geoherb regions. In addition, the HPLC fingerprints of 30 batches of RAS, as part of the comprehensive evaluation of RAS, were established and used for spectral efficiency to screen the quality markers for anti-platelet aggregation activities. Five compounds in RAS-senkyunolide I, uridine, guanine, ferulic acid and adenosine-were demonstrated to contribute significantly to the anti-platelet aggregation activity. These bioactive compounds, especially senkyunolide I and ferulic acid with stronger activities, could be used as quality markers of RAS for quality control of RAS.

The effect of anti-alcoholic gastric ulcer before and after vinegar-processed Yuanhu Zhitong prescription based on spectral-effect relationship.

The aim of this study was to screen out the active ingredients of Yuanhu Zhitong prescription (YZP) before and after vinegar processing to play an anti-alcoholic gastric ulcer role through spectrum-effect relationship. First, the fingerprint of 16 batches of YZP was studied using the ultra-high-performance liquid chromatography-quadrupole mass spectrometry detector analysis (UPLC-QDA) method. Second, gastric lesion was induced by anhydrous ethanol. The degree of gastric mucosa injury was evaluated by hematoxylin and eosin staining, and the contents of malondialdehyde and tumor necrosis factor α and superoxide dismutase were detected using the enzyme-linked immunosorbent assay kit. Sixteen batches of YZP were analyzed using the spectrum-effect relationship method. Finally, absorption, distribution, metabolism, and excretion (ADME) was used to evaluate the bioavailability of potential compounds. The results showed that the UPLC-QDA method could successfully establish the fingerprint of YZP. Hematoxylin and eosin staining and biochemical indicators showed that YZP had obvious anti-alcoholic gastric ulcer action. Coptisine chloride, corydaline, berberine chloride, palmatine, imperatorin, and phellopterin were screened out using the spectrum-effect method, and all of them possessed good bioavailability. The results of this study suggest that YZP plays an anti-ulcer role by exerting antioxidant and anti-inflammatory effects through six main active components.

Quality Markers of Dendrobium officinale by "Oligosaccharide-Spectrum-Effect" Relationships.

Dendrobium officinale Kimura et Migo has been used as a traditional Chinese medicine (TCM) and a functional food for thousands of years. Carbohydrate is one of the most important effective substances and indicative components in D. officinale. However, since the qualitative and quantitative analysis of polysaccharides in D. officinale remains a challenge and limitation, herein, an oligosaccharide-quality marker approach was newly developed for quality assessment of D. officinale by spectrum–effect relationships between high performance liquid chromatographic (HPLC) fingerprints and anti-inflammatory effects. The HPLC fingerprints of 48 batches of oligosaccharides from D. officinale (DOOS) were developed and analyzed with similarity analysis (SA) and hierarchical cluster analysis (HCA), and eight common peaks were identified. In vitro screening experiment indicated that DOOS potentially inhibited nitric oxide (NO) production and effectively reduced the release of inflammatory cytokines, such as TNF-α, IL-6, and IL-1β in RAW 264.7 cells, thereby reducing the inflammatory response of cells. Finally, the HPLC fingerprint of different batches of DOOS was combined with in vitro anti-inflammatory activity to assess the spectrum–effect relationships of DOOS by gray correlation analysis (GCA), in addition, the purified oligosaccharide components were identified and validated for NO inhibitory activity. Our results showed four DOOS (maltotetraose, maltopentaose, maltohexaose, and mannohexaose) were relevant to anti-inflammatory effects and could be as quality markers for the quality control of D. officinale. It suggests that the “oligosaccharide-spectrum-effect” relationships approach is a simple and reliable method for the quality control of herb medicines or nutritious foods.

Schisandra chinensis (Turcz.) Baill. essential oil exhibits antidepressant-like effects and against brain oxidative stress through Nrf2/HO-1 pathway activation.

The present study aimed to evaluate the antidepressant-like effect of essential oils from Schisandra chinensis (Turcz.) Baill. (SEO) and its possible mechanisms of SEO. The behavioral despair mouse model in vivo and H2O2-induced PC12 cells model in vitro were employed. And the potential effective components were identified by the spectrum-effect relationships analysis. SEO significantly decreased the immobility time in the forced swimming test and tail suspension test, which indicated a promising antidepressant-like effect of SEO in depressed mice. The decreased levels of SOD, GSH, and CAT, and increased levels of MDA were significantly reversed by SEO treatment, which showed good antioxidant activities both in vitro and in vivo. Besides, SEO significantly promoted the nuclear translocation of Nrf2 and the expression of HO-1 in depressed mice and H2O2-induced PC12 cells. The histopathological examination results showed a potential neuronal protective effect of SEO in the hippocampus and cortex. Furthermore, the upregulation of PI3K/AKT/GSK3β signaling was observed after SEO treatment in the H2O2-induced PC12 cells. Additionally, based on the spectrum-effect relationship analysis, 9 peaks were identified as positively correlated with the antioxidant activity of SEO. These results suggested that SEO promoted Nrf2/HO-1 pathway to improve the oxidative stress status and exerted the antidepressant-like effects.

Anti-inflammatory active component in raw materials of Ligustici Rhizoma et Radix based on spectrum-effect relationship

The present study investigated the correlation of UPLC fingerprints of raw materials of Ligustici Rhizoma et Radix samples with the anti-inflammatory effect and explored the pharmacodynamic material basis for the anti-inflammatory activity. UPLC fingerprints of 18 batches of raw materials of Ligustici Rhizoma et Radix samples were established for the determination of the content of eight components. The toe swelling rate and the content of IL-1β, IL-6, and PGE2 in rats with toe inflammation induced by carrageenin were measured. Canonical correlation analysis was used to study the spectrum-effect relationship. Cluster analysis indicated that chemical components of Ligusticum sinense and L. jeholense were similar. Methanol extracts of L. sinense, L. jeholense, and Conioselinum vaginatum significantly reduced the toe swelling rate and the content of IL-1β, IL-6 and PGE2 in swollen tissues. The anti-inflammatory effect of C. vaginatum was weaker than that of L. sinense and L. jeholense. The results of spectrum-effect relationship indicated that there was an obvious correlation between chemical components and pharmacodynamic indexes. In UPLC fingerprints, compounds 1, 3(chlorogenic acid), 4(cryptochlorogenic acid), 5, 6(ferulic acid), 7(isochlorogenic acid B), 9, 11, 13, 15, 16, 17, 18(coniferyl ferulate), 19, 20(N-butylphthalide), 21, 22, and 23 were significantly correlated with anti-inflammation, among which compounds 5, 11, 13, 15, 17, 21, and 23 had negative correlation. This study screened out the effective components with anti-inflammatory activity in raw materials of Ligustici Rhizoma et Radix, which was of great significance to improve the quality evaluation system of raw materials of Ligustici Rhizoma et Radix.

Screening of hypoglycemic components in Platycladi Cacumen by phytochemical investigation, spectrum-effect relationship, and chemometric methods.

In this work, the hypoglycemic components in Platycladi Cacumen, an essential traditional Chinese medicine, were evaluated by combining phytochemical investigation, spectrum-effect relationship analysis, and chemometric methods. The phytochemical studies on Platycladi Cacumen extract lead to the isolation of 21 potential bioactive compounds. The chromatographic fingerprints of Platycladi Cacumen samples were established by high-performance liquid chromatography. The hypoglycemic effects of Platycladi Cacumen samples were further evaluated by inhibition of α-glucosidase and detected by the high-performance liquid chromatography method. The spectrum-effect relationship study by bivariate correlations analysis and orthogonal partial least squares regression revealed that myricitrin (P9), quercitrin (P13), afzelin (P18), and amentoflavone (P24) were more relevant to the α-glucosidase inhibitory activity. The results of α-glucosidase inhibitory activity of 21 isolated compounds and molecular docking studies also indicated these flavonoids had potent α-glucosidase inhibitory activity. Collectively, the present study established the spectrum-effect relationship mode of Platycladi Cacumen and discovered the major hypoglycemic components, which provides a feasible method for screening bioactive components.

An Integrated Strategy to Identify and Quantify the Quality Markers of Xinkeshu Tablets Based on Spectrum-Effect Relationship, Network Pharmacology, Plasma Pharmacochemistry, and Pharmacodynamics of Zebrafish.

Xinkeshu tablets (XKST), a traditional Chinese patent medicine (CPM), have served in the clinical treatment of cardiovascular diseases (CVDs) for decades. However, its pharmacodyamic material basis was still unclear, and the holistic quality control has not been well established due to the lack of systematic research on the quality markers. In this experiment, the heart rate recovery rate of a zebrafish larva was used to evaluate the traditional pharmacological effect of XKST i.e., antiarrhythmic effect. The HPLC fingerprints of 16 batches of XKST samples were obtained, and antiarrhythmic components of XKST were identified by establishing the spectrum-effect relationship between HPLC fingerprints and heart rate recovery rate of zebrafish larva with orthogonal signal correction and partial least squares regression (OSC–PLSR) analysis. The anticardiovascular disease components of XKST were identified by mapping the targets related to CVDs in network pharmacology. The compounds of XKST absorbed and exposed in vivo were identified by ultra-high performance liquid chromatography Q-Exactive high-resolution mass spectrometry (UHPLC-Q-Exactive HRMS). Based on the earlier studies, combined with five principles for identifying quality markers and verified by a zebrafish arrhythmia model, danshensu, salvianolic acid A, salvianolic acid B, daidzein, and puerarin were identified as quality markers of XKST. In total, 16 batches of XKST samples were further quantified with the method established in this study. Our study laid the foundation for the quality control of XKST. The integrated strategy used in the study of XKST could be applied for the identification and quantification of quality markers of other CPMs as well.

Spectrum-effect relationship between UPLC-Q-TOF-MS fingerprint and anti-AUB effect of Clinopodium chinense (Benth.) O. Kuntze

Clinopodium chinense (Benth.) O. Kuntze (C. chinense), a traditional Chinese medicine with significant astringent and hemostatic properties, is mainly used to treat abnormal uterine bleeding (AUB) with remarkable curative effect, but the active ingredients of which remain unclear. This study aimed to screen and identify the main anti-AUB components of C. chinense via spectrum-effect relationship analysis and experiment validation. Firstly, total extract of C. chinense (TEC) of 12 batches samples was prepared by Chinese Pharmacopoeia. The fingerprint chromatogram of TEC was established by UPLC-Q-TOF-MS. The AUB model was established by intragastric administration of mifepristone and misoprostol to pregnant rats, followed by the treatment with TEC. After drug administration lasting 7 days, metrorrhagia volume was measured, pathological changes in uterine tissue were evaluated by HE staining, the levels of TXB-2, TNF-α, and IL-6 were measured by ELISA. The spectrum-effect relationship was investigated by grey relational analysis (GRA) and orthogonal partial least squares discriminant analysis (OPLS-DA). Finally, the potential active ingredients of TEC screened by spectrum-effect relationship analysis were subsequently verified both in vitro and in vivo. A total of 25 common peaks were obtained from the fingerprint chromatogram of the 12 bathes TEC samples, 12 peaks were identified according to the reference substances. Comparing with the model group, TEC significantly reduced the uterine bleeding volume, alleviated endometrial injury, increased plasma TXB2 level, and decreased plasma IL-6 and TNF-α levels. Furthermore, seven components including kaempferol, quercetin, buddlejasaponin Ⅳb, hesperidin, naringenin, apigenin, and saikosaponin a were identified via spectrum-effect relationship analysis. In vitro and in vivo verification indicated that buddlejasaponin Ⅳb, hesperidin, naringenin, apigenin, and saikosaponin a were responsible for the anti-AUB activity of TEC. In conclusion, the present study established a spectrum-effect relationship for C. chinense and identified the main anti-AUB compounds in TEC, which provides insight for the exploration of bioactive components and quality control of C. chinense.

Spectrum-Effect Relationships Between High-Performance Liquid Chromatography Fingerprints and Hepatoprotective Activities of Cuscutae Semen.

Cuscutae Semen (CS) is a commonly used hepatoprotective traditional Chinese medicine, but the chemical components responsible for its hepatoprotective activity are unclear. The purpose of this study was to evaluate the spectrum-effect relationships between HPLC fingerprints and hepatoprotective effects of CS, and to identify its bioactive components. Phytochemical isolation of CS extracts was first carried out and 14 potential bioactive compounds were obtained. Chemical fingerprinting was performed on 27 batches of CS from different sources by HPLC, and further analyzed by similarity analysis (SA) and hierarchical clustering analysis (HCA). Pharmacodynamic testing was performed in a CCl4-induced, acute liver injury cell model to assess the hepatoprotective activity of CS by measuring the cell viability and levels of alanine transaminase (ALT) and aspartate aminotransferase (AST). Bivariate correlations analysis (BCA) and orthogonal projections to latent structures (OPLS) were used to analyze the spectrum-effect relationships of CS. The results showed that the chemical fingerprints of CS were closely correlated with its hepatoprotective activity. Peaks 1, 10, 18, 19, 21, 22, and 24 might be potential hepatoprotective compounds in CS, and the validation experiments of isolated compounds indicated that chlorogenic acid (P10), hyperoside (P21), isoquercitrin (P22), and astragalin (P24) were the main hepatoprotective components. By combining chemical fingerprints with hepatoprotective evaluation, the present study provides important guidance for QC and clinical use of CS. (1) Ten potential bioactive compounds were isolated from CS; (2) The spectrum-effect relationship of CS was molded by HPLC and analysed by OPLS and BCA. (3) Four compounds including chlorogenic acid were the main hepatoprotective components.

Material Basis Elucidation and Quantification of Dandelion through Spectrum–Effect Relationship Study between UHPLC Fingerprint and Antioxidant Activity via Multivariate Statistical Analysis

The excessive expression of reactive oxygen species is closely connected to many diseases. Considerable studies have demonstrated dandelion as well as its ingredients exhibited antioxidant activity. However, specific material basis reflecting the antioxidant activity has not been comprehensively investigated. In this study, a spectrum–effect relationship study on dandelion between fingerprinting and antioxidant activity was analyzed in detail, while a UHPLC quantification method developed and completely validated for simultaneous determination of active ingredients in dandelion. With the establishment of dandelion fingerprints of different regions, 24 common peaks were characterized. The classic FRAP method and ABTS methods were then used to detect their antioxidant activity. Partial least squares regression analysis, bivariate correlation analysis and grey correlation method were used to accomplish the spectrum–effect relationship. Eventually, the ingredients with antioxidant activity which could be considered as candidate quality markers of dandelion were discovered through spectrum–effect relationship analysis. The six compounds including caftaric acid, chlorogenic acid, caffeic acid, chicoric acid, isochlorogenic acid A, and isochlorogenic acid C were quantitatively determined. The developed UHPLC assay method was accurate, precise, and reliable. The study has elucidated the antioxidant material basis of dandelion and provided a scientific basis for the quality control of dandelion.

Research on Q-markers of Polygoni Perfoliati Herba based on analytic hierarchy process-entropy weight method and fingerprints

The potential quality markers(Q-markers) of Polygoni Perfoliati Herba were studied based on analytic hierarchy process(AHP)-entropy weight method(EWM), network pharmacology, and spectrum-effect relationship analysis. The AHP-EWM was used for quantitative identification of the Q-markers. To be specific, AHP was applied for the weight analysis of the validity, testability, and specificity of the first-level indexes, and EWM for the analysis of the second-level indexes supported by literature and experimental data. Based on literature and network pharmacology, the validity analysis was to study the component-target-disease-efficacy network, and select the components with the strongest correlation with the efficacy of clearing heat and removing toxin, diuresis and alleviating edema, and relieving cough. For the testability analysis, the high performance liquid chromatography(HPLC) and literature research were used to determine the 10 components in Polygoni Perfoliati Herba, and the fingerprints of Polygoni Perfoliati Herba were established at the same time. The specificity analysis was based on the statistics of the number of plants in which the components existed. Thereby, the 11 compounds: quercetin, oleanolic acid, ellagic acid, gallic acid, kaempferol, rutin, esculetin, quercetin-3-O-glucuronide, ursolic acid, protocatechuic acid, and ferulic acid, were identified as potential Q-markers. The 11 compounds were identified to have high anti-inflammatory activity, indicating that the 11 Q-markers may be the functional material basis. The result in this study is expected to serve as a reference for the quality control of Polygoni Perfoliati Herba.

Interbatch quality control of the extract from Artemisia frigida Willd. by spectrum-effect relationship between HPLC fingerprints and the total antioxidant capacity

ABSTRACT 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.

Screening out key compounds of Glechomae Herba for antiurolithic activity and quality control based on spectrum-effect relationships coupled with UPLC-QDA

Glechomae Herba (GH) has been widely used in the treatment of urolithiasis, especially kidney stones, in China and Southeast Asia. Pharmacological studies have suggested that the antioxidant property of GH contributes to its anticalculus effect. CaSR is one of the main locations of kidney stones, and the mechanism of action of CaSR inhibitors in the treatment of kidney stones is similar to that of GH. However, until now, the antiurolithic chemical compounds in GH and their interaction with CaSR remain unknown. In our study, we revealed the interaction between the active compounds in GH and the active compounds in CaSR inhibitors by using spectrum-effect relationship analysis, pharmacodynamics, and molecular docking techniques. The results showed ten common peaks from the fingerprints of GH extracts from different regions. Pharmacological experiments showed that GH could significantly treat renal tissue lesions. Chlorogenic acid (CA), rosmarinic acid (RA), P5, luteolin, apigenin, and P9 were screened after the analysis of spectrum-effect relationships. In vitro validation experiments showed that all the screened compounds had inhibitory effects on the development of kidney stones in our model. The molecular docking results showed that the above compounds could be docked with CaSR in a natural state, and the docking score was less than 7. This work constructs a general model for the combination of UPLC-QDA and antiurolithic drugs, studies the spectrum-effect relationship of GH, and provides a new possibility for the development of new antiurolithic drugs.

Spectrum-Effect Relationship Analysis of Bioactive Compounds in Zanthoxylum nitidum (Roxb.) DC. by Ultra-High Performance Liquid Chromatography Mass Spectrometry Coupled With Comprehensive Filtering Approaches.

Zanthoxylum nitidum (Roxb.) DC. (ZN), with strong effects of anti-inflammation and antioxidant activities is treated as a core herb in traditional Chinese medicine (TCM) preparation for treating stomachache, toothache, and rheumatoid arthritis. However, the active ingredients of ZN are not fully clarified due to its chemical complexity. In the present study, a double spectrum–effect analysis strategy was developed and applied to explore the bioactive components in herbs, and ZN was used as an example. Here, the chemical components in ZN were rapidly and comprehensively profiled based on the mass defect filtering-based structure classification (MDFSC) and diagnostic fragment-ion-based extension approaches. Furthermore, the fingerprints of 20 batches of ZN samples were analyzed by high-performance liquid chromatography, and the anti-inflammatory and antioxidant activities of the 20 batches of ZN samples were studied. Finally, the partial least squares regression (PLSR), gray relational analysis models, and Spearman’s rank correlation coefficient (SRCC) were applied to discover the bioactive compounds in ZN. As a result, a total of 48 compounds were identified or tentatively characterized in ZN, including 35 alkaloids, seven coumarins, three phenolic acids, two flavonoids, and one lignan. The results achieved by three prediction models indicated that peaks 4, 12, and 17 were the potential anti-inflammatory compounds in ZN, whereas peaks 3, 5, 7, 12, and 13 were involved in the antioxidant activity. Among them, peaks 4, 5, 7, and 12 were identified as nitidine, chelerythrine, hesperidin, and oxynitidine by comparison with the standards and other references. The data in the current study achieved by double spectrum–effect analysis strategy had great importance to improve the quality standardization of ZN, and the method might be an efficiency tool for the discovery of active components in a complex system, such as TCMs.