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1.
Article in Chinese | WPRIM | ID: wpr-873333

ABSTRACT

Objective::To identify and analyze the chemical constituents in Bufei Jianpi formula by UPLC-Q-TOF-MS/MS. Method::An Agilent Poroshell SB-C18 column (4.6 mm×100 mm, 2.7 μm) was used with a mobile phase system of 0.1% formic acid solution (A)-acetonitrile (B) for gradient elution (0-10 min, 3%B; 10-100 min, 3%-50%B; 100-120 min, 50%-100%B) under positive ion mode and water (A)-acetonitrile (B) for gradient elution (0-5 min, 3%B; 5-60 min, 3%-100%B) under negative ion mode, the flow rate was 0.6 mL·min-1, and the column temperature was 30 ℃. Mass spectrometric data were obtained under electrospray inoization (ESI) in positive and negative ion modes, the collection range was m/z 50-1 000.Agilent MassHunter Qualitative Analysis software was used to extract and match chromatographic peaks. Result::Combined with reference, related literature and database analysis, 95 compounds were identified by mass spectrometry information, including 41 flavonoids, 23 alkaloids, 12 lignans, 9 organic acids, and 10 other compounds. Conclusion::The chemical composition of Bufei Jianpi formula is complex, and the cracking rules of different components are different. Flavonoids are prone to deglycosylation, dehydration, Diels-Alder reaction (RDA) cleavage of the ring during lysis, and loss of some neutral molecules such as CO, CO2, CHO. Lignans has a substituent such as a hydroxyl group, a carbonyl group or a methoxy group on the benzene ring, and it is easy to obtain a fragment ion which loses H2O or CO. The basic structure of organic acids is a phenolic hydroxyl group-substituted aromatic ring, acrylic acid, fatty acid or the like, this kind of compound is easy to lose H2O and COOH in negative ion mode, and it is easy to break at the carbonyl to form fragment ions. This established method is rapid, sensitive and accurate, which can quickly identify the chemical constituents in Bufei Jianpi formula and provide evidences for clarifying efficacy material base of this formula.

2.
Acta Pharmaceutica Sinica ; (12): 222-227, 2019.
Article in Chinese | WPRIM | ID: wpr-780108

ABSTRACT

The chemical composition of traditional Chinese medicine (TCM) compounds is complex, the treatment is broad, and the quality control indexes cannot accurately reflect the functional properties. According to the above problems, the authors take the research process of quality markers of Qizhiweitong granules as an example to innovate the research ideas and technical methods, and constructed five progressive steps of TCM compounds quality control and evaluation model: "based on function, to figure out the attending", "components and pharmacodynamics correlation, multiple components with multiple effects", "to analyze the components, and systematically integrate them", "spectrum and effect correlation, from a spectrum to see the efficiency", and "from the content-effect colour atla to see the quality". Based on the multiple effects of components, multiple components of multi-effect pharmacological efficacy evaluation system were established. All-time isobaric multiwavelength fusion fingerprint technology was improved and developed. "Spectrum-effect colour atla" software was research and developed for the first time, to realize the "visualization" of TCM efficacy. The aim of this work is to provide an exploratory solution for the integrated quality control of TCM compounds.

3.
Article in Chinese | WPRIM | ID: wpr-798517

ABSTRACT

Objective:To define the anti-gastric cancer activity in vitro of petroleum ether fraction of Boehmeria nivea root and reveal the material basis of its efficacy, so as to lay the foundation for the development and utilization of B. nivea root. Method:Methyl thiazolyl tetraolium(MTT) method was used to evaluate the inhibitory rate and time-dose relationship of petroleum ether fraction of B. nivea root with different doses and delivery times on human gastric cancer HGC-27 cells. Flow cytometry was used to detect the change of cell apoptosis and cell cycle after petroleum ether fraction of B. nivea root acted on human gastric cancer HGC-27 cells. GC-MS was used to detect the components of petroleum ether fraction of B. nivea root. Result:Experiment data showed significant cell proliferation inhibition in an obvious time-dose-effect manner, with statistically significant differences (PB. nivea root. The effect of petroleum ether fraction of B. nivea root on human gastric cancer HGC-27 cells could induce apoptosis,which affects the normal changes of cell cycle. The percentage of cells was decreased significantly in G0/G1 phase,and that in S phase was significantly increased. GC-MS was used to identify 26 chemical constituents in petroleum ether of B. nivea root,including sitosterol and stigmasterol. Conclusion:Petroleum ether fraction of B. nivea root is the active anti-gastric cancer part,and its main effective component is sterol compounds. This lays the foundation for the rational application of B. nivea root in clinic and the further research in tis anti-tumor effect.

4.
Article in Chinese | WPRIM | ID: wpr-798501

ABSTRACT

Objective:To study on the chemical constituents of total tannins from Spatholobi Caulis,and to analyze the pharmacodynamics and mechanism of total tannins from Spatholobi Caulis on cervical cancer HeLa cells. Method:UPLC-Q-TOF/MS was used to qualitatively analyze the composition of total tannins from Spatholobi Caulis.The appropriate concentration and time of administration were screened by 3 dimensional(3D) microfluidic chip.Flow cytometry was used to determine the effect of total tannins from Spatholobi Caulis on the cell cycle and apoptosis of cervical cancer HeLa cells and analyzed by FlowJo v10.0.7 and ModFit LT 3.2 software.Enzyme-linked immunosorbent assay(ELISA) was used to determine the changes of vascular endothelial growth factor(VEGF)-A and Caspase-3 factors in cervical cancer HeLa cells supernatant treated with total tannins from Spatholobi Caulis. Result:Total of 15 components in total tannins from Spatholobi Caulis were identified or inferred.The low,medium and high dosages of total tannins from Spatholobi Caulis were 0.5,1.0, 2.0 g·L-1 and the best time of administration was 36 h.The proportions of early and late apoptosis of cervical cancer HeLa cells increased significantly in the apoptosis analysis after being treated by total tannins from Spatholobi Caulis.The DNA synthesis early phase(G0/G1 phase) of cervical cancer HeLa cells significantly increased,and the DNA synthesis phase(S phase) and the DNA synthesis late phase(G2/M phase) reduced.After being treated with total tannins from Spatholobi Caulis,the expression of VEGF-A in cervical cancer HeLa cells supernatant was significantly decreased and the expression of Caspase-3 was significantly increased. Conclusion:Spatholobi Caulis is rich in tannins,which can significantly inhibit the proliferation of cervical cancer HeLa cells and promote its apoptosis.This paper can provide the basis for further research of total tannins from Spatholobi Caulis.

5.
Article in Chinese | WPRIM | ID: wpr-350122

ABSTRACT

In order to further clarify the rational use of different medicinal parts of Schizonepeta, microfluidic technology was used in this study to investigate the differences in drug efficacy against lung cancer in vitro. The ethanol extracts were examined with HPLC to establish their fingerprints in order to analyze the relationship between the spectrum and efficacy index through Grey Correlation software, and a rapid HPLC-Q-TOF/MS method was established. The result in vitro shows that the effect and components of different medicinal parts had a certain differences, and apoptosis and necrosis rate from big to small in turn is leaf, flower, root, stem. The chromatographic peaks of the 26, 12, 2, 6 and 15th are the luteolin, icynaroside, rosmarinic, caffeic acid, and hesperidin, while the 20 and 10th may be dan phenolic acid L and benzoic acid. On the one hand, preliminary study reflects that the root of Schizonepeta tenuifolia may be developed into the medicinal parts in future. On the other hand, the major chemical composition of S. tenuifolia was found to have the anti-lung-tumor effects. This new method was established for the quality control and the rational use of different parts of traditional Chinese medicine.

6.
Acta Pharmaceutica Sinica ; (12): 126-131, 2017.
Article in Chinese | WPRIM | ID: wpr-779830

ABSTRACT

This study was designed to elucidate the chemical composition and anti-cancer effects of Schizonepeta tenuifolia's ethanol extracts. Microfluidic technology was used in the study of Schizonepeta tenuifolia from 9 different geographic regions. The ethanol extracts were examined with HPLC to establish their Fingerprints in order to analyze the relationship between the spectrum and efficacy index through Grey Correlation software, and a rapid HPLC-Q-TOF/MS method was established. The result shows that chromatographic peaks of the 19, 6, 11, 16, 18th are the representative diosmetin, luteoloside, hesperidin, luteolin, and apigenin. The 10, 12, 20th peaks may be naringenin-7-O-glucuronide or quercitrin, rosmarinate or acetylcorynoline, and 5,7-dihydroxy-6,4-dimethoxy flavone. The major chemical composition of Schizonepeta tenuifolia was found to have the anti-lung-tumor effects. A new method was established for the quality control of traditional Chinese medicine.

7.
Article in Chinese | WPRIM | ID: wpr-346495

ABSTRACT

<p><b>OBJECTIVE</b>To establish the chromatography-efficacy relation method for analyzing the anti-inflammatory activity of Qizhi Weitong particles, in order to lay a foundation for quality control and pharmacodynamic evaluation of traditional Chinese medicine compounds.</p><p><b>METHOD</b>On the basis of a full-time multi-wavelength fusion fingerprint of Qizhi Weitong particles, the latin hypercube sampling was used to divide six herbs in Qizhi Weitong particles into groups of different proportions to determine their inhibition ratios of TNF-alpha, IL-6 and NO released by LPS-induced RAW264. 7 cells. Pharmaeodynamic data and chemical information of HPLC fingerprints of each group were analyzed with the gray correlation method to get the anti-inflammatory effect of each chromatographic peak, and then fitted with BP neural network to establish the chromatography-efficacy relation.</p><p><b>RESULT</b>There were 25 peaks closely related to the anti-inflammatory activity. With the 25 peaks as input items, the 3-BP network was adopted to establish the neural network model for anti-inflammatory effect of Qizhi Weitong particles.</p><p><b>CONCLUSION</b>With an error of less than 7%, the model could better fit with the complicated non-linear relation of the compound, and applied in studying the chromatography-efficacy relation. In this study on the chromatography-efficacy relation, a new method is established to evaluate the anti-inflammatory activity of Qizhi Weitong particles. It is of practical significance as an effective approach for controlling quality and exploring the material basis for efficacy of traditional Chinese medicine compounds.</p>


Subject(s)
Animals , Anti-Inflammatory Agents , Chemistry , Cell Line , Chromatography, High Pressure Liquid , Drugs, Chinese Herbal , Chemistry , Female , Humans , Interleukin-6 , Allergy and Immunology , Macrophages , Allergy and Immunology , Mice , Neural Networks, Computer , Quality Control , Rats , Rats, Sprague-Dawley , Stomach Diseases , Drug Therapy , Allergy and Immunology , Tumor Necrosis Factor-alpha , Allergy and Immunology
8.
Article in Chinese | WPRIM | ID: wpr-294079

ABSTRACT

<p><b>OBJECTIVE</b>To control the quality of Qizhiweitong granules with the all-time multi-wavelength fusion fingerprint quantification as the major technique.</p><p><b>METHOD</b>Agilent TC-C18 (4.6 mm x 250 mm, 5 microm) chromatographic column was adopted, with 0.02% formic acid water-acetonitrile as the mobile phase for linear gradient elution. The flow rate was 1 mL x min(-1), column temperature was 30 degrees C, and detector wavelength was 230, 254, 283 nm. Matlab was adopted for all-time multiple-wavelength fusion for data in dif format.</p><p><b>RESULT</b>A good relationship was shown for albiflorin in 56.5-452 mg x L(-1) (r = 0.999 8), paeoniflorin in 107-856 mg x L(-1) (r = 0.999 8), licorice glycoside in 73.4-687 mg x L(-1) (r = 0.999 8), naringin in 109-872 mg x L(-1) (r = 0.999 8), neohesperidin in 48.0-384 mg L(-1) (r = 0.999 8), and glycyrrhizic acid in 38.6-308 mg x L(-1) (r = 0.999 8), with recoveries of 0.999 8.</p><p><b>CONCLUSION</b>The method is simple, accurate and highly reproducible, and can provide basis for quality control of Qizhiweitong granules.</p>


Subject(s)
Benzoates , Bridged-Ring Compounds , Chromatography, High Pressure Liquid , Methods , Drugs, Chinese Herbal , Glucosides , Glycosides , Monoterpenes , Quality Control
9.
Article in Chinese | WPRIM | ID: wpr-283770

ABSTRACT

<p><b>OBJECTIVE</b>To establish a high performance liquid chromatographic (HPLC) amalgamated to double UV waves method for simultaneous determination of loganin and paeonol in Liuwei Dihuang pills.</p><p><b>METHOD</b>A HPLC method was developed. The separation was carried out on a Agilent Zorbax SB C18 column (5 microm, 4.6 mm x 250 mm). The mobile phase consisted of water (A) and acetonitrile (B) with linear linear gradient elution [0-8 min, (B) from 1% to 12%; 8-21 min, B keep 12%; 21-40 min, (B) from 12% to 90%; 40-50 min, B keep 90% for 10 min]. The detection was Photodiode Array with the detection wavelengths were at 236 nm and 274 nm. The column temperature being 30 degrees C and the flow rate was 1.0 mL min(-1). Extracting the chromatergraph from 274 nm and 236 nm, we amalgamated the two chromatographs by matlab programmed.</p><p><b>RESULT</b>The calibration curves of loganin and paeonol were linear in the ranges of 0.0362-1.09 microg (r =0. 9998) and 0.0450-1.35 microg (r =0.9998), respectively. The average recoveries of loganin and paeonol were 97.3% (RSD 1.4 %) and 103.0% (RSD 1.9%), respectively. Three different batches of Liuwei Dihuang pills were determined with this method.</p><p><b>CONCLUSION</b>This is a more convenient, reasonable and credible quality control method for the traditional Chinese medicine.</p>


Subject(s)
Acetophenones , Chemistry , Chromatography, High Pressure Liquid , Methods , Drugs, Chinese Herbal , Chemistry , Iridoids , Chemistry , Reproducibility of Results , Spectrophotometry, Ultraviolet
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