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ObjectiveTo compare the effects of different processing methods in ancient and modern times on the chemical components of Lilii Bulbus decoction， and to provide experimental support for the origin processing， decoction piece processing and clinical application of this herb. MethodUltra high performance liquid chromatography tandem quadrupole electrostatic field orbitrap high resolution mass spectrometry（UHPLC-Q-Orbitrap HRMS） was used for structural identification of the compounds using excimer ions， secondary MS and characteristic fragment ions， and referring to relevant literature and database information. Principal component analysis（PCA） and orthogonal partial least squares discriminant analysis（OPLS-DA） were used to screen the main differential components， the differential components were quantitatively studied by high performance liquid chromatography（HPLC）， in order to compare the types and contents of chemical components in the decoction of different processing products of Lilii Bulbus. ResultA total of 24 chemical components were identified from the decoction of different processed products of Lilii Bulbus， water extract and scalding liquid of fresh Lilii Bulbus， including 17 phenols， 5 saponins and 2 alkaloids. Compared with the fresh Lilii Bulbus decoction， the contents of regaloside A， p-coumaric acid， colchicine and other components in the decoction of dry Lilii Bulbus processed by scalding method decreased， the content of regaloside C in the decoction of dry Lilii Bulbus processed by steaming method decreased， and the contents of regaloside A and regaloside C in the decoction of fresh Lilii Bulbus processed by water immersion also decreased. Compared with the decoction of dry Lilii Bulbus processed by scalding method， the overall content of components in the fresh Lilii Bulbus decoction and the decoction of fresh Lilii Bulbus processed by water immersion was higher， the contents of components in the decoction of dry Lilii Bulbus processed by steaming method was higher， except for the slightly lower content of regaloside C. ConclusionDifferent processing processes have a certain effect on the types and contents of chemical components in Lilii Bulbus decoction. Scalding process is beneficial to the preservation of Lilii Bulbus， but can cause the loss of effective components. Compared with scalding method， steaming method can prevent browning of Lilii Bulbus and reduce the loss of its active ingredients. The processing method of removing foam after overnight immersion proposed by ZHANG Zhongjing may be more conducive to the treatment of Baihe disease， which can provide reference for the clinical rational application and mechanism research of different processed products of Lilii Bulbus.
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Xanthoceras sorbifolium seeds have a wide range of applications in the food and pharmaceutical industries. To compare and analyze the chemical compositions of different parts of X. sorbifolium seeds and explore the potential value and research prospects of non-medicinal parts, this study used ultra-high-performance liquid chromatography quadrupole Orbitrap high-resolution mass spectrometry(UHPLC-Q-Orbitrap HRMS) to detect the chemical composition of various parts of the seeds. A total of 82 components were preliminary identified from X. sorbifolium seeds, including 5 amino acids, 4 polyphenols, 3 phenylpropionic acids, 7 organic acids, 15 flavonoids, 6 glycosides, and 23 saponins. Mass spectrometry molecular networking(MN) analysis was conducted on the results from different parts of the seeds, revealing significant differences in the components of the seed kernel, seed coat, and seed shell. The saponins and flavonoids in the seed kernel were superior in terms of variety and content to those in the seed coat and shell. Based on the chromatographic peaks of different parts from multiple batches of samples, multivariate statistical analysis was carried out. Four differential components were determined using HPLC, and the average content of these components in the seed kernel, seed coat, and seed shell were as follows: 0.183 6, 0.887 4, and 1.440 1 mg·g~(-1) for fraxin; 0.035 8, 0.124 1, and 0.044 5 mg·g~(-1) for catechin; 0.032 9, 0.072 0, and 0.221 5 mg·g~(-1) for fraxetin; 0.435 9, 2.114 7, and 0.259 7 mg·g~(-1) for epicatechin. The results showed that catechin and fraxetin had relatively low content in all parts, while fraxin had higher content in the seed coat and seed shell, and epicatechin had higher content in the seed kernel and seed coat. Therefore, the seed coat and seed shell possess certain development value. This study provides rapid analysis and comparison of the chemical compositions of different parts of X. sorbifolium seeds, which offers an experimental basis for the research and clinical application of medicinal substances in X. sorbifolium seeds.
Subject(s)
Chromatography, High Pressure Liquid/methods , Catechin/analysis , Flavonoids/analysis , Seeds/chemistry , Saponins/analysisABSTRACT
ObjectiveUltra-high performance liquid chromatography-quadrupole-electrostatic field orbitrap high resolution mass spectrometry（UHPLC-Q-Orbitrap HRMS） was used to identify the metabolites of limonin in rats， and to explore the gender differences in the distribution of prototype components and metabolites in rats after single dose intragastric administration of limonin， as well as to speculate the metabolic pathways. MethodThe separation was performed on a Thermo Scientific Accucore™ C18 column（3 mm×100 mm， 2.6 μm） with 0.1% formic acid aqueous solution（A）-0.1% formic acid acetonitrile solution（B） as mobile phase in a gradient elution mode（0-1 min， 5%B； 1-6 min， 5%-20%B； 6-18 min， 20%-50%B； 18-23 min， 50%-80%B； 23-25 min， 80%-95%B； 25-30 min， 95%B） at a flow rate of 0.3 mL·min-1 and a column temperature of 30 ℃. MS data of biological samples were collected under the positive ion mode of electrospray ionization（ESI） and in the scanning range of m/z 100-1 500. Plasma， tissues（heart， liver， spleen， lung， kidney， stomach and small intestine）， urine and fecal samples were collected and prepared after intragastric administration， and the prototype component and metabolites of limonin were identified. ResultThe prototype component of limonin were detected in the feces， stomach， small intestine of female and male rats， and in the heart， liver， spleen， lung and kidney tissues of female rats. A total of 23 metabolites related to limonin were detected in rats， of which 2， 1， 5， 4， 23 metabolites were detected in liver， stomach， small intestine， urine and feces， respectively， and the main metabolic pathways were hydrolysis， reduction， hydroxylation and methylation， etc. The distribution of some metabolites differed between male and female rats. ConclusionThe prototype component of limonin are mainly distributed in the stomach and small intestine in rats， and the distribution of prototype component and some metabolites are different by gender. Limonin is mainly excreted through feces with phase Ⅰ metabolites as the main ones. The results of this study can provide a reference for further elucidation of the effect of gender differences on the metabolism of limonin in vivo and its mechanism of action.
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ObjectiveTo analyze the differential components in water extract of Chuanxiong Rhizoma before and after processing with wine， and to explore the molecular mechanism of Chuanxiong Rhizoma processed with wine in enhancing anti-cerebral ischemia injury. MethodUltra high performance liquid chromatography tandem quadrupole orbitrap high resolution mass spectrometry （UHPLC-Q-Orbitrap HRMS） was used to qualitatively analyze the main chemical components in water extract of Chuanxiong Rhizoma based on the spectral information of compound， comparison of reference substance and references. The chemical pattern recognition method was used to screen the differential components of Chuanxiong Rhizoma before and after processing. Based on these differential components， the potential targets of differential components were predicted by online databases， and the related targets of cerebral ischemia were searched. Cytoscape 3.6.0 was used to establish the network diagram of differential components-action targets-diseases of Chuanxiong Rhizoma processed with wine. The protein-protein interaction （PPI） network of intersection targets was constructed by STRING 11.5. The potential targets of differential components against cerebral ischemia were analyzed by Gene Ontology （GO） and Kyoto Encyclopedia of Genes and Genomes （KEGG） enrichment analysis through DAVID 6.8. At the same time， the chemical compounds with high relative content and increased peak area after wine processing were docked with their corresponding targets to verify the mechanism of enhanced effect after wine processing. ResultA total of 71 chemical components were identified from Chuanxiong Rhizoma， 34 differential components and 603 potential targets were screened out. At the same time， a total of 769 disease targets and 60 intersection targets were obtained. Seven key targets were identified through PPI network analysis， including JUN， signal transducer and activator of transcription 3 （STAT3）， mitogen-activated protein kinase 3 （MAPK3）， interleukin-1β （IL-1β）， vascular endothelial growth factor A （VEGFA）， Caspase-3 （CASP3） and mtrix metalloproteinase 9 （MMP9）. Tumor necrosis factor （TNF） signaling pathway was the main differential signaling pathway. The results of molecular docking showed that differential components （senkyunolide K， senkyunolide F， 3-n-butylphthalide， Z，Z′-6，8′，7，3′-diligustilide， ferulic acid and Z-ligustilide） and corresponding targets had good binding activities. ConclusionThe synergistic mechanism of Chuanxiong Rhizoma processed with wine may be related to the enhanced inhibitory effect of inflammatory reaction.
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Objective::Ultra high performance liquid chromatography coupled with Q-Exactive Focus hybrid quadrupole and orbitrap high resolution mass spectrometer (UHPLC-Q-Orbitrap HRMS) was applied for identification of chemical constituents in Pimpinella thellungiana. Method::Chromatographic separation was performed on a WATERS BEH C18 column (2.1 mm ×50 mm, 1.7 μm). The mobile phase consisted of 0.1% formic acid aq (A) and acetonitrile (B) with a gradient elution. Mass spectral analysis were performed on Q-Exactive Focus hybrid quadrupole and orbitrap mass spectrometer. The mass spectrometer was connected to UHPLC instrument via an ESI interface. Samples were analyzed in negative ion mode by the full-scan-dd MS 2(data-dependent MS/MS) scanning mode. Then the constituents of P. thellungiana were identified by compared HRMS data with those of the standard compounds, MS cleavage mechanism and the related literatures. Result::Based on the characteristic mass data of accurate molecular weight and fragmentation ion information, 29 chemical constituents were identified including 19 chlorogenic acids, 7 flavonoids and 3 phenolic acid. Among them, the identified components except luteolin-7-O-β-D-glucuronopyranoside and apigenin-7-O-β-D-glucuronopyranoside were reported in P. thellungiana for the first time. Conclusion::The established UHPLC-Q-Orbitrap HRMS method can be used to identify the chemical constituents of P. thellungiana quickly and accurately, providing the scientific evidence for its quality evaluation and material basis research.
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Objective: To systematically study the main chemical components of Fufang Shangtong Capsule and explore the main mechanism of its effect, and provide some reference for the research of its pharmacodynamic substance. Methods: In this study, UHPLC-Q-Orbitrap HRMS was used to comprehensively analyze the main chemical components of Fufang Shangtong Capsule. The chromatographic column was Waters Acquity UPLC® BEH C18 chromatographic column (50 mm ×2.1 mm, 1.7 μm) and the mobile phase was acetonitrile (A)-0.1% formic acid water (B). According to the MS/MS spectrometry information of compounds, and the comparison with standards or references, the chemical information of drugs can be quickly and accurately identified. On this basis, the network pharmacology method was used to analyze the chemical composition target of the drug, enrich its function, preliminarily select the main effective substances of the drug, and simultaneously explore its mechanism of action. Results: A total of 36 chemicals were identified in this study from Fufang Shangtong Capsule. The target function of enrichment analysis showed that the drug mainly played its therapeutic effect on regulating vascular endothelial, vascular smooth muscle pain, affecting platelet function, promoting energy supply, reducing inflammation and relieving pain, so as to exert its efficacy in promoting blood circulation and removing stasis, invigorating qi and relieving pain. Conclusion: In this study, UHPLC-Q-Orbitrap HRMS combined with network pharmacology was used, wich provided scientific theoretical basis and important reference for the identification of effective ingredients, screening of quality markers and the study of potential mechanism of action of Fufang Shangtong Capsule.
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Objective: To systematically study the chemical components of Tenghuang Jiangu Capsule, explore the main mechanism of action, and provide some evidences for the research of its pharmacodynamic substances. Methods: In this study, UHPLC-Q-Orbitrap HRMS was used to comprehensively analyze the main chemical components of Tenghuang Jiangu Capsule. According to the MS/MS spectrometry information of compounds, the chemical information of this herbal formula can be quickly and accurately identified by comparison with standards or references. Next, the BAT-MAN-TCM database was used to predict the targets of the identified chemical components. The KEGG pathway annotation analysis and GO enrichment analysis were further carried out through the DAVID database to screen out the main pharmacodynamic substances of Tenghuang Jiangu Capsule and explore the potential mechanisms. Results: A total of 34 chemical components were identified in Tenghuang Jiangu Capsule. The "component-target" network analysis indicated that the major components including kaempferol, isoflavoues aglycone, ursolic acid, formononetin, and stigmasterol might act on some key targets such as Bcl-2, BAX, AKt, PPARG, PTGS1, PTGS2, TNF, IL6, F7, IL1B, etc. The results indicated that osteoclast differentiation, NF-κB, PI3K-Akt, renal cell, and platelet activation might be the main action pathways of exerting the therapeutic effect of bone protection, nourishing kidney, promoting blood circulation and relieving pain of Tenghuang Jiangu Capsule. Conclusion: In this study, UHPLC-Q-Orbitrap HRMS combined with network pharmacology was used to preliminarily clarify the chemical composition and reveal potential mechanism of Tenghuang Jiangu Capsule. The results provided scientific theoretical basis for screening the effective ingredients and further clarifying the mechanism of action of Tenghuang Jiangu Capsule.
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Objective: In order to establish a rapid and efficient analysis method for identification of the complex components in Jingzhi Guanxin Soft Capsule, and provide the basic research data for the systematic elaboration of its chemical constituents. Methods: An ultra-high performance liquid chromatography-quadrupole/Orbitrap high resolution mass spectrometry (UHPLC-Q-Orbitrap HRMS) was used for the identification analysis of the components in Jingzhi Guanxin Soft Capsule, and the multistage fragments ions data was compared with the standard substance and literature consulting. Results: Forty-three compounds were identified in this study, including flavones, phthalides, organic acids, quinones and other categories. Conclusion: The chemical constituents of Jingzhi Guanxin Soft Capsule are identified systematically, accurately and efficiently, which provide the theory basis for the further research of its pharmacodynamic material basis and quality control.
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OBJECTIVE: To establish an analytical method of ultra performance liquid chromatography-quadrupole/orbitrap high resolution mass spectrometry (UHPLC-Q-Orbitrap HRMS) for identification and quantitation of the multi-constituents of Danshen-chuanxiongqin injection. METHODS: The method of UHPLC-HRMS was developed to identify the complex chemical composition and full ms scan mode was used to determine the main active ingredients precisely, then the means of principal component analysis (PCA) was used to comprehensively assess the quality of Danshen-chuanxiongqin injection. RESULTS: A total of 23 chemical constituents were identified in Danshen-chuanxiongqin injection, 14 of which were unambiguously identified by comparing with chemical standards, and seven major compounds, ligustrazine, danshensu, salvianolic acid A, succinic acid, rosmarinic acid, protocatechuic aldehyde, caffeic acid, in Danshen-chuanxiongqin Injection were determined accurately. The analysis by multivariate data processing software SIMCA 14.0 indicated that the quality of most batches of samples were stable except ligustrazine, danshensu, and salvianolic acid A which were a bit unstable in some individual batches, and it was essential to monitor the content of salvianolic acid A to control the drug quality. CONCLUSION: The established HPLC-TOF-MS/MS method has the properties of rapid identification, high specificity, simpliness, and feasibility, which can be used as a better means for the qualitative and quantitative analysis of danshen-chuanxiongqin injection. Moreover, it lays the ground for quality control of the drug and provides data reference for the rational use in clinic.
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Objective: In order to study the chemical profile of Shengui Capsules, a novel ultra high performance liquid chromatography-quadrupole/orbitrap high resolution mass spectrometry (UHPLC-Q-Orbitrap HRMS) was applied to establish a method to recognize and classify the ingredients accurately and rapidly. Methods: ACQUITY UPLC® BEH C18 chromatographic column (100 mm × 2.1 mm, 1.7 μm) was employed and the separation was performed with the mobile phase consisting of acetonitrile-0.1% formic acid aqueous solution. The information of accurate mass and multistage fragment ions were obtained by the novel “monitored simultaneously for positive and negative ions, Full MS scan and automatic trigger secondary mass spectrometry” mode of Q-Orbitrap MS technology. Then, the complex chemical constituents would be identified by comparing the relative retention time and the mass data of the reference substance, and consulting the reference literature or Mass Bank, Chemical Book network database at the same time. Results: Forty chemical components were finally identified in this study, including the 16 tritepene saponins, 6 organic acids, 13 lactones, and 5 other classes. Conclusion: The method established in this study could be used to rapidly, accurately, and systematically identify the main chemical constituents of Shengui Capsules. Moreover, this study will lay a scientific preliminary foundation for the further pharmacodynamic material basis, quality control improvement and the rational clinical use.
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Objective: In order to establish an efficient analysis method for the identification of the complex components in Qianliexin Capsule rapidly, and provide the basic research data for the systematic elaboration of its chemical constituents. Methods: An ultra-high performance liquid chromatography-quadrupole/Orbitrap high resolution mass spectrometry (UHPLC-Q-Orbitrap HRMS) was used for the identification analysis of the components in Qianliexin Capsule accurately, and the multistage fragments ions data was compared with the standard substance and consulting the literatures. Results: Sixty-one compounds were identified in this study, including 12 flavones, 11 coumarins, six terpenes, 19 organic acids and other categories. Conclusion: The accurate and rapid identification of various chemical constituents of Qianliexin Capsule was achieved in this study, which provided the theory basis for the pharmacodynamic material and the quality control study of Qianliexin Capsule.
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Objective: To investigate the chemical composition of Shensong Yangxin Capsule, a novel ultra high performance liquid chromatography-quadrupole/orbitrap high resolution mass spectrometry (UHPLC-Q-Orbitrap HRMS) was employed to establish a method that could identify the ingredients systematically and rapidly. Methods: The information of accurate mass and multistage fragment ions was obtained by the novel UHPLC-Q-Orbitrap technology. Chemical constituents were characterized by comparing the relative retention time and the mass data of the reference substance, meanwhile consulting the reference literature or the Mass Bank, Chemical Book network database. Results: A total of 54 compounds were finally identified in this research, including the phenolic acids, flavones, terpenoids, anthraquinones, alkaloids and others. Conclusion: A method was established in this study to identify various chemical constituents of Shensong Yangxin Capsule systematically, rapidly and accurately. The identified chemical components mostly cover the main constituents of each medicinal material in the formula. Our work will lay a scientific foundation for the bioactive components screening, quality control improvement and further clinical application of this herbal formulation.
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Objective To recognize the chemical profile of Qishen Yiqi Dropping Pills (QYDP) comprehensively, systematically and rapidly; ultra high performance liquid chromatography-quadrupole/orbitrap high resolution mass spectrometry (UHPLC-Q-Orbitrap HRMS) was employed to identify the main chemical composition of this preparation. Methods A gradient elution for separation was achieved through ACQUITY UPLC® BEH C18 column (100 mm × 2.1 mm, 1.7 μm) with acetonitrile-water (containing 0.1% formic acid) as the mobile phase. Then, the novel Q-Orbitrap MS technology was employed to detect the information of accurate mass and multistage fragment ions. Chemical constituents were characterized by comparing their relative retention time and mass data with that of the reference substance, meanwhile the reference literature, Mass Bank database, and Chemical Book network database were also consulted. Results A total of 53 ingredients were finally identified in this study, including 14 organic acids, 10 flavones, 10 authraquinones, 2 saponins, 7 amino acids, and 10 others. Conclusion An efficient method was established in this work to identify the main chemical ingredients of QYDP rapidly and accurately; Meanwhile, this research will lay a scientific foundation for the further research on pharmacodynamic material basis, quality control, and clinical application of this medicine.