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1.
Zhongguo Zhong Yao Za Zhi ; 46(12): 2900-2911, 2021 Jun.
Artigo em Chinês | MEDLINE | ID: mdl-34467680

RESUMO

Paridis Rhizoma(PR) is prepared from the dried rhizome of Paris polyphylla var. yunnanensis(PPY) or P. polyphylla var. chinensis(PPC) in Liliaceae family. The rapid development of PPY or PPC planting industry resulted from resource shortage has caused the waste of a large number of non-medicinal resources. To clarify the chemical compositions in rhizomes, fibrous roots, stems, leaves, seeds and pericarps of PPC, and explore the comprehensive application value and development prospect of these parts, the qualitative and quantitative analyses on the different parts of PPC were carried out by ultra-high performance liquid chromatography tandem quadrupole time-of-flight mass spectrometry(UPLC-Q-TOF-MS/MS) and high performance liquid chromatography(HPLC). A total of 136 compounds were identified, including 112 steroidal saponins, 6 flavonoids, 11 nitrogen-containing compounds and 7 phytosterols. Rhizomes, fibrous roots, and seeds mainly contained protopennogenyl glycosides and pennogenyl glycosides; leaves and stems mainly contained protodiosgenyl glycosides and diosgenyl glycosides; pericarps mainly contained pennogenyl glycosides, followed by diosgenyl glycosides. The total level of four saponins was the highest in fibrous roots and rhizomes, followed by those in the pericarps and arillate seeds, and the lowest in the stems and exarillate seeds. This study can provide data support for the comprehensive development and rational application of non-medicinal parts of PPC.


Assuntos
Liliaceae , Melanthiaceae , Saponinas , Cromatografia Líquida de Alta Pressão , Rizoma , Espectrometria de Massas em Tandem
2.
Zhongguo Zhong Yao Za Zhi ; 46(12): 2912-2922, 2021 Jun.
Artigo em Chinês | MEDLINE | ID: mdl-34467681

RESUMO

The dried fruit body of Phylloporia ribis(Hymenochaetaceae), which prefers to live on the stumps of Lonicera japonica(Caprifoliaceae), has a variety of activities, whereas its pharmacodynamic material basis is not completely clear and there are few reports on its quality control and evaluation. In this study, an UPLC-Q-TOF-MS method was used to analyze the nucleosides and nucleobases in P. ribis and a HPLC method was established for simultaneous determination of 10 nucleosides and nucleobases. MS and MS/MS data were acquired in positive ion mode. Based on the data comparison of the sample and the reference substance, the literature data and the compound databases of ChemSpider and PubChem, 18 nucleosides and nucleobases were identified qualitatively from the water extract of P. ribis for the first time. After optimization, the HPLC was performed using a Welch Ultimate AQ C_(18) column(4.6 mm×250 mm, 5 µm) by gradient elution with acetonitrile and water as mobile phase, the flow rate of 1.0 mL·min~(-1), the detection wavelength of 260 nm, and the column temperature of 30 ℃. Through the investigation of the extraction method, solvent and time, it was determined that the test solution should be obtained by cold water extraction for 18 h. At the present HPLC conditions, 10 components of uracil, cytidine, hypoxanthine, uridine, thymine, inosine, guanosine, 2'-deoxyinosine, 2'-deoxyguanosine and thymidine could be well separated(R > 1.5) and showed good linearity(r > 0.999 9) in the concentration ranges of 0.247-24.7, 0.283-28.3, 0.273-27.3, 0.256-25.6, 0.257-25.7, 0.318-31.8, 0.245-24.5, 0.267-26.7, 0.250-25.0 and 0.267-26.7 mg·L~(-1), respectively. The average reco-veries of 10 components were 95.78%-104.5%, and the RSDs were 2.2%-5.2%(n=6). The contents of 10 nucleosides and nucleobases in different samples of P. ribis varied greatly, which were 0.021-0.122, 0.004-0.029, 0.014-0.226, 0.009-0.442, 0.003-0.014, 0.002-0.146, 0.007-0.098, 0-0.054, 0.005-0.069, 0.004-0.081 and 0.072-1.28 mg·g~(-1) for uracil, cytidine, hypoxanthine, uridine, thymine, inosine, guanosine, 2'-deoxyinosine, 2'-deoxyguanosine, thymidine and total 10 components, respectively. These results demonstrated that the components had significant differences in the internal quality, and good quality control was needed to ensure the medical efficacy. This study provides a scientific basis for the discovery of pharmacodynamic ingredients, quality control and evaluation of P. ribis.


Assuntos
Nucleosídeos , Espectrometria de Massas em Tandem , Basidiomycota , Cromatografia Líquida de Alta Pressão , Guanosina
3.
Zhongguo Zhong Yao Za Zhi ; 46(12): 2931-2941, 2021 Jun.
Artigo em Chinês | MEDLINE | ID: mdl-34467683

RESUMO

As a new strategy capable of uncovering the characteristics of traditional Chinese medicines, the quantitative analysis of multi-components by single-marker(QAMS) has been widely employed for the quality evaluation of Chinese medicinal materials, slices, and extracts. However, its application in the assessment of Chinese patent medicines is yet to be explored. By referring to the determination of three bufogenins in Bufonis Venenum by QAMS described in Chinese Pharmacopoeia(2020 Edition), this paper selected seven representative preparations containing Bufonis Venenum and explored whether the relative correction factors(RCFs) of cinobufagin(CB) to bufalin(BF) and resibufogenin(RB) could be directly used for the quality control of Bufonis Venenum-contained preparations. Based on the qualitative analyses under the same chromatographic conditions as used for toad venom, combing specificity test, five preparations such as Yatong Yili Pills, Houzheng Pills, Xiongdan Jiuxin Pills, Liushen Pills and Niuhuang Xiaoyan Pills, were expected to use validated RCFs for the direct determination of three components. Taking Houzheng Pills as an example, the methodological validation of bufalin, cinobufagin and resibufogenin was carried out, and the recoveries of bufalin, cinobufagin and resibufogenin were 90.64%-106.1%. The obvious difference was not observed between the contents of bufalin and resibufogenin in 24 batches of preparation samples by QAMS and external reference method. In the tested samples, the content of bufalin, cinobufagin and resibufogenin were 1.27-2.61, 2.44-5.66 and 0.988-3.16 mg·g~(-1) in 10 batches of Liushen Pills samples. The contents of bufalin, cinobufagin and resibufogenin were 0.760-1.32, 1.35-2.39 and 0.600-1.55 mg·g~(-1) in 10 batches of Houzheng Pills samples from three manufacturers. The obtained data contribute to improving the quality standard of Bufonis Venenum-contained preparations, and they also provide some ideas for the application of QAMS in the quality evaluation and control of Chinese patent medicines.


Assuntos
Medicina Tradicional Chinesa , Medicamentos sem Prescrição , China , Cromatografia Líquida de Alta Pressão , Controle de Qualidade
4.
Zhongguo Zhong Yao Za Zhi ; 46(12): 2889-2899, 2021 Jun.
Artigo em Chinês | MEDLINE | ID: mdl-34467710

RESUMO

Sophorae Flavescentis Radix,derived from the root of Sophora flavescens in the Leguminosae family,has been widely used in the medicine,agriculture,animal husbandry,and daily chemical industry. A pharmacophore model-based method for rapid discovery of tyrosinase inhibitors( TIs) from S. flavescens was established by molecular docking under Lipinski rules,and verified by enzyme assays. Briefly,the chemical constituent database of S. flavescens( CDSF) was established based on the previous papers. Theoptimal pharmacophore model( OPM) was constructed by DS 2019 on the basis of known active TIs. Eighty-three hits predominated by flavonoids having higher fitting scores with OPM than the positive control were screened out,and subjected to molecular docking based on the three-dimensional structure of tyrosinase crystal protein. The potential TIs such as kurarinone and nor-kurarinone were rapidly discovered from the compounds with higher docking scores than the positive control under the Lipinski rules. The results were verified by the in vitro enzyme assays. The inhibition activities of tyrosinase from non-medicinal parts of S. flavescens were also tested to explore the relationship between the inhibition activity and chemical compositions. This study is expected to provide data support for the comprehensive application and development of S. flavescens and also a new method for the rapid discovery of active substances or functional constituents in the complex systems.


Assuntos
Sophora , Animais , Flavonoides , Simulação de Acoplamento Molecular , Monofenol Mono-Oxigenase , Extratos Vegetais/farmacologia , Raízes de Plantas
5.
Zhongguo Zhong Yao Za Zhi ; 46(16): 4023-4033, 2021 Aug.
Artigo em Chinês | MEDLINE | ID: mdl-34467711

RESUMO

Paris polyphylla var. chinensis(PPC) is used as one of the origin plants of Paridis Rhizoma described in the Chinese Pharmacopoeia(2020 edition). Its resources shortage makes the planting scale gradually expand, and plenty of aerial parts are abandoned because of not being effectively used. On the basis of previous research, this study separated steroidal saponins to further clarify the chemical composition of the aerial parts of PPC. As a result, three pairs of 25R or 25S epimers of furostanol saponins were obtained by various column chromatography techniques. Their structures were identified as neosolanigroside Y6(1), solanigroside Y6(2), neoprotogracillin(3), protogracillin(4), neoprotodioscin(5) and protodioscin(6) by spectral data combining with chemical transformation. Compound 1 is a new compound, and compounds 2, 3 and 5 are isolated from Paris plants for the first time. Compounds 4 and 6 are isolated from this plant for the first time. Previously, only several spirostanol glycosides with 25S configuration were isolated from Paris plants. Guided by mass spectrometry, the present study isolated the furostanol saponins with 25S configuration from this genus for the first time, which further enriches the chemical information of Paris genus and provides a reference for the isolation of similar compounds.


Assuntos
Liliaceae , Melanthiaceae , Saponinas , Extratos Vegetais , Rizoma
6.
Zhongguo Zhong Yao Za Zhi ; 46(16): 4034-4039, 2021 Aug.
Artigo em Chinês | MEDLINE | ID: mdl-34467712

RESUMO

As anti-aging ingredients, ß-nicotinamide mononucleotide(NMN) and nicotinamide adenine dinucleotide(NAD~+) have attracted worldwide attention in recent years. After oral administration, NMN can be converted into NAD~+ in vivo and the latter is the actual ingredient which exerts anti-aging effect. In order to explore the "rejuvenating and anti-aging" effect of Dendrobium officinale, which was firstly recorded in Shennong's Herbal Classic of Materia Medica, this study established the quantitative method of UPLC-MS/MS for simultaneous determination of NMN and NAD~+ in D. officinale and the congeneric species for the first time, and 34 batches of samples were detected. UPLC conditions are as follows: ACQUITY UPLC HSS T3 column(2.1 mm × 100 mm, 1.8 µm), gradient elution with acetonitrile-0.1% formic acid in water at the flow rate of 0.3 mL·min~(-1), and column temperature of 40 ℃. MS conditions were scanned electrospray ionization source and multiple reaction monitoring mode. The method was verified by systematic methodology. The mean recoveries of NMN and NAD~+ were 77.58% and 80.70%, respectively, with RSD of 3.6% and 4.3%, separately. All results showed that the content of NMN was higher in D. officinale than in the other congeneric species. Particularly, the content in fresh D. officinale stems was as high as 0.931 9 µg·g~(-1). NAD~+ was only found in D. officinale and the content was three times higher than that of NMN. This may be the reason that D. officinale topped the "nine famous anti-aging herbs". In addition, processing method influences the content of NMN and NAD~+ in Dendrobium. Specifically, the content of NMN and NAD~+ was in the order of fresh Dendrobium stems > dried Dendrobium stem segments > spiral or spring-like dried Dendrobium stems.


Assuntos
Dendrobium , Mononucleotídeo de Nicotinamida , Cromatografia Líquida de Alta Pressão , Cromatografia Líquida , NAD , Espectrometria de Massas em Tandem
7.
Zhongguo Zhong Yao Za Zhi ; 46(16): 4040-4050, 2021 Aug.
Artigo em Chinês | MEDLINE | ID: mdl-34467713

RESUMO

In recent years, the establishment of the commercial grade of Yinpian [traditional Chinese medicine(TCM) pieces for decoction] in the TCM industry has been hotly disputed. In this article, Sophorae Flavescentis Radix(SFR) was selected as a representative example to investigated. Through systematic comparison and analysis, the different grades of SFR slices were traced, verified and evaluated. According to the current published local grade standards of SFR slices, the results showed that the first-class of SFR slices were mostly derived from the wild medicinal materials, the second-class were mostly originated from the cultivated materials in 3-4 years, and the third-class products were from a small number of lateral roots and short-growing years or harsh habitat of wild medicinal materials. On the basis of identifying the sources of different grades of SFR slices, the contents of the active components, including matrine, oxymatrine, oxysophocarpine, sophoridine, N-methyl-cytisine, sophocarpine, were quantitatively determined in typical samples, it was found that the grades were inversely proportional to the contents of active ingredients. In order to ensure the universality of the conclusion, the contents of different grades of commercial SFR slices were determined, and the conclusion was verified as "the commercial grades of SFR slices were inversely linked to their contents of active ingredients". This phenomenon is common in the determination of the commercial grade of Yinpian of radix and rhizome. Therefore, we propose that the method or standard of the commercial grade of Yinpian of radix and rhizome based on the size of Yinpian maybe not proper. Whether and how to classify Yinpian commercial grade is not only a multi-disciplinary issue, especially in combination with clinical efficacy, but also a big problem need to consider the production, commercial circulation and other processes link of quality risk and quality assurance, and should be treated with great caution.


Assuntos
Medicamentos de Ervas Chinesas , Sophora , Medicina Tradicional Chinesa , Raízes de Plantas , Rizoma
8.
Zhongguo Zhong Yao Za Zhi ; 46(16): 4051-4060, 2021 Aug.
Artigo em Chinês | MEDLINE | ID: mdl-34467714

RESUMO

This research established the HPLC methods for the determination of perillaketone, perillaldehyde, caffeic acid, scutellarin, and rosmarinic acid in 33 batches of Perillae Folium. Kromasil C_(18)(4.6 × 250 mm, 5 µm) chromatographic column was used, and the mobile phase for determination of the perillaketone and perillaldehyde was methanol-water(55∶45) solution, at a flow rate of 1.0 mL·min~(-1), with the column temperature at 30 ℃. The mobile phase for the determination of caffeic acid, scutellarin and rosmarinic acid was methanol(A)-0.2% phosphoric acid aqueous solution(B) with gradient elution(0-20 min, 25%-30% A; 20-60 min, 30%-43% A). The flow rate was 1.0 mL·min~(-1) and the column temperature was set at 30 ℃. The results showed that the established method can achieve good separation of the five components in samples, with a good linear relationship and high accuracy, indicating that the methods can be used for the determination of Perillae Folium. The results showed that all samples contained five components. And the content of rosmarinic acid(0.04%-1.57%) > scutellarin(0.03%-0.77%) > perillaldehyde(0.02%-0.66%) > perillaketone(0.03%-0.30%) > caffeic acid(0.006%-0.07%). Thirty-three Batches of Perillae Folium can be grouped into 5 categories. There are certain content rules and region specificities under different clusters. Perillaketone, perillaldehyde, and rosmarinic acid can be used as the main markers to evaluate the quality of Perillae Folium.


Assuntos
Medicamentos de Ervas Chinesas , Folhas de Planta , Cromatografia Líquida de Alta Pressão , Extratos Vegetais
9.
J Ethnopharmacol ; 275: 114045, 2021 Jul 15.
Artigo em Inglês | MEDLINE | ID: mdl-33831463

RESUMO

ETHNOPHARMACOLOGICAL RELEVANCE: The Dang-Gui-Si-Ni (DGSN) decoction as a classic prescription has been widely used for thousands of years in the clinical practice of traditional Chinese medicine (TCM). Especially in recent years, the potential efficacy of TCM for the treatment of Raynaud's syndrome has attracted great attention as there are still no specific remedies for this disease. However, the active constituents and underlying mechanisms responsible for the therapeutic benefits are not well understood, which makes it difficult to ensure quality control or to design research and drug development strategies. To identify the potential pharmacodynamic ingredients (PPIs) of TCM will help to achieve suitable process control procedures for industrial production and large-scale manufacturing. AIM OF THE STUDY: In the present study, we propose a multi-dimensional qualitative analysis method combining water-decoction spectra, in-vitro intestinal absorption spectra, in-vivo plasma spectra, and molecular docking of components to quickly identify the PPIs for the DGSN decoction of TCM. MATERIALS AND METHODS: Water-based decoctions of DGSN were prepared in accordance with the clinical use registered in ancient books. Ultra-high-performance liquid chromatography-quadrupole-time of flight mass spectrometry (UHPLC-Q/TOF-MS) coupled with computerized modelling activity screening was used to quickly identify the PPIs of the DGSN decoction. Bioactive compounds absorbed in vitro were identified using the everted intestinal sac model from rats and compounds absorbed in vivo were confirmed in portal vein blood samples obtained following oral administration in rats. Molecular docking validation experiments were adopted to predict the binding activity to coagulation factors I, II, VII, X, and IX. The active components were further confirmed by pharmacodynamics analysis. The anticoagulant activity of the DGSN decoction was verified using rat models. RESULTS: Thirty-one compounds were identified in the DGSN decoction. According to the in vivo experiments, 22 compounds that could be absorbed in vivo were detected by the everted intestinal sac model in rats. This model greatly reduces the scope of PPIs and is easy to perform. Ten compounds were detected in the portal vein blood in rats. The compounds detected in plasma provide stronger evidence supporting the PPIs. Molecular docking in vitro experiments indicated that 7 compounds exhibited better binding activity with coagulation factors I, II, VII, X, and IX. The animal experiments confirmed that the DGSN decoction could improve the microcirculation, providing indirect proof of anticoagulant activity suggested by the molecular docking studies. Finally, based on the multi-dimensional methods, 9 potential compounds present in the DGSN decoction were identified as PPIs (i.e., ferulic acid, paeoniflorin, albiflorin, chlorogenic acid, cryptochlorogenic acid, liquiritin, liquiritin apioside, cinnamaldehyde and glycyrrhizic acid). CONCLUSION: Overall, this study combined the water-decoction spectra, intestinal absorption spectra in vitro, plasma spectra in vivo, and molecular docking studies to establish a multi-dimensional qualitative analysis method of the DGSN decoction. Meanwhile, 9 compounds in DGSN decoction were identified as PPIs using this method, and are proposed for application as quality standards for complex TCM prescriptions.


Assuntos
Medicamentos de Ervas Chinesas/química , Medicamentos de Ervas Chinesas/farmacologia , Administração Oral , Animais , Fatores de Coagulação Sanguínea/química , Modelos Animais de Doenças , Medicamentos de Ervas Chinesas/administração & dosagem , Medicamentos de Ervas Chinesas/metabolismo , Flavonoides/análise , Flavonoides/química , Hidroxibenzoatos/análise , Hidroxibenzoatos/química , Absorção Intestinal , Masculino , Medicina Tradicional Chinesa , Microcirculação/efeitos dos fármacos , Simulação de Acoplamento Molecular , Nucleosídeos/análise , Nucleosídeos/química , Plasma/química , Ratos Sprague-Dawley , Doença de Raynaud/tratamento farmacológico , Terpenos/análise , Terpenos/química
10.
Zhongguo Zhong Yao Za Zhi ; 46(2): 391-397, 2021 Jan.
Artigo em Chinês | MEDLINE | ID: mdl-33645127

RESUMO

This paper aims to solve the problems of complicated-unstable test solution preparation process and insufficient extraction of the active ingredient astragaloside Ⅳ in the legal method for the determination of astragaloside Ⅳ in Astragali Radix. The continuous single-factor analysis of seven main factors affecting the content of astragaloside Ⅳ was carried out by HPLC-ELSD, and then the pre-paration method of test solution was optimized. This optimized method exhibited excellent performance in precision, repeatability and stability. The average recovery rate of astragaloside Ⅳ was 99.65% with RSD 2.2%. Astragaloside Ⅳ showed a good linearity between the logarithm of peak area and the logarithm of injection quantity in the range of 0.46-9.1 µg(r=0.999 6). The contents of astragaloside Ⅳ in 29 batches of Astragali Radix were determined by the new and the legal methods. The results showed that the average content of astragaloside Ⅳ in these Astragali Radix samples determined by the former method was 1.458 times than that of the latter one, indicating the new method was simple, reliable and more adequate to extract target compound. According to the results, it is suggested to improve the content standard of astragaloside Ⅳ in Astragali Radix in the new edition of Chinese Pharmacopeia.


Assuntos
Astrágalo (Planta) , Medicamentos de Ervas Chinesas , Saponinas , Triterpenos , Cromatografia Líquida de Alta Pressão , Triterpenos/análise
11.
J Asian Nat Prod Res ; : 1-8, 2020 Nov 23.
Artigo em Inglês | MEDLINE | ID: mdl-33225748

RESUMO

A new homo-aro-cholestane glycoside parispolyside H, along with nine known compounds, were isolated from 75% ethanolic extract of the rhizome of Paris polyphylla var. chinensis. Their chemical structures were elucidated on the basic of analysis of detailed spectroscopic and physicochemical properties. In addition, the isolated compounds (1, 6-9) were evaluated for their cytotoxic activity against HepG2 human liver cancer cell lines. Among them, four known compounds (6-9) showed cytotoxicity with IC50 values ranging from 0.41 to 3.6 µM.

12.
Zhongguo Zhong Yao Za Zhi ; 45(7): 1545-1557, 2020 Apr.
Artigo em Chinês | MEDLINE | ID: mdl-32489033

RESUMO

An ultra-performance liquid chromatography(UPLC) method integrating characteristic chromatogram and eight terpenoids determination has been established for comparing the differences of Alismatis Rhizoma(Zexie) from different product areas. Thirty-seven batches of crude drugs and thirty batches of prepared slices of Alismatis Rhizoma were analyzed. The obtained data were analyzed by similarity evaluation, principal components analysis(PCA) and partial least squares discriminant analysis(PLS-DA). There were three main characteristic peaks in the characteristic chromatograms, and alisol B 23-acetate(S) was selected as the reference. Compared with the S peak, the relative retention times of the other two characteristic peaks were 0.55(alisol) and 0.77(alisol B), respectively. Peak areas and the ratio of alisol B to alisol B 23-acetate could be used to distinguish Alismatis Rhizoma from different geographical origins. The samples were divided into three groups by PCA and PLS-DA based on the content determination results, and they were "Jian Zexie"(Fujian and Jiangxi provinces), "Chuan Zexie"(Sichuan and Hubei provinces), and "Guang Zexie"(Guangxi province). The contents of chemical components in samples from different producing areas were notably different. For example, the contents of alisol A and alisol A 24-acetate were significantly higher in "Guang Zexie" compared with "Jian Zexie" and "Chuan Zexie"(P<0.000 1). The contents of alisol B and alisol C were significantly higher in "Chuan Zexie" compared with "Jian Zexie"(P<0.000 1). Combining the characteristic chromatograms and quantitative analysis of eight terpenoids, this study showed that the relative contents of components and their ratios were notable different in samples from different regions, but types and numbers of chemical compositions were basically similar. The results of this study illustrated the regional differences of Alismatis Rhizoma and their components characteristics, and provided references for authentication and quality control of Alismatis Rhizoma.


Assuntos
Rizoma , China , Cromatografia Líquida de Alta Pressão , Medicamentos de Ervas Chinesas , Terpenos
13.
Zhongguo Zhong Yao Za Zhi ; 45(8): 1717-1725, 2020 Apr.
Artigo em Chinês | MEDLINE | ID: mdl-32489054

RESUMO

The effects of the growing periods, processing methods, nutritive organs and cut parts of the herbs on the quality of Andrographis Herba have been studied, which could provide scientific basis for producing high-quality crude materials of Andrographis Herba. A quantitative analysis of multi-components by single-marker(QAMS) method was used to simultaneously determine 4 diterpene lactones of andrographolide(AD), neoandrographolide(NAD), 14-deoxyandrographolide(14-DAD), and dehydroandrographolide(DHAD) in 78 batches of Andrographis Herba samples. Visual analysis, clustering analysis and partial least squares discrimination analysis(PLS-DA) were used for data processing and mining. The growing periods of Andrographis Herba were divide into the rapid growing stage(Ⅰ), the luxuriant foliage stage(Ⅱ), the bud stage(Ⅲ), the flower stage(Ⅳ), the fruiting stage(Ⅴ) and the later fruiting stage(Ⅵ), six ones in total. The results showed that the total contents of 4 diterpene lactones(TC) kept almost constant in growing periods of Ⅰ-Ⅲ, began to fall off in growing period Ⅳ, decreased rapidly in growing period Ⅴ and reduced to minimum in growing period Ⅵ. Therefore, the best harvesting period for Andrographis Herba was the bud stage. For the processing methods, none significant difference occurred for TC between drying by the sun and drying in the shade. However, in comparison of the samples dried by the sun, the samples dried in the shade exhibited lower content of AD, nonetheless, the higher contents of DHAD and NAD, indicating that the process of drying in the shade may lead to the decomposition and transformation of AD. Therefore, when the weather conditions permitted, the method drying by the sun should be used. The distributions of AD, DHAD and TC in the different cut parts and nutritive organs were determined as follows: upper cut parts > middle cut parts ≈ entire herbs > lower cut parts, leaves > entire herbs > stems. Furthermore, the contents of 4 diterpene lactones in leaves and herbs were much higher than those in stems. Therefore, it was suggested that the upper and middle cut parts of the herbs or the parts containing leaves should be preferred for harvesting to ensure the proportion of the leaves in Andrographis Herba.


Assuntos
Andrographis , Diterpenos , Lactonas , Folhas de Planta
14.
Zhongguo Zhong Yao Za Zhi ; 45(8): 1726-1733, 2020 Apr.
Artigo em Chinês | MEDLINE | ID: mdl-32489055

RESUMO

Bufonis Venenum(toad venom) is prepared from the dried secretion of Bufo bufo gargarizans or B. melanostictus. Toad venom powder is one of the processed slices of crude material toad venom. In the present study, the global quality control method and standard of toad venom and its processed slice, toad venom powder were established, including TLC identification, characteristic chromatogram and QAMS by HPLC. The relative correction factor(RCF) was re-calculated and validated. The average RCFs of cinobufagin to gamabufotalin, bufotalin, bufalin and resibufogenin were considered for the determination of five bufadienolides in the samples. The total amount in the different batches of the dried samples varied from 4.06% to 17.0%. Referring to the revised methods for crude materials, the quality standard of toad venom powder was drafted including appearance description, TLC examination, characteristic chromatogram, water content and the total amount of five bufadienolides. The present investigation provided scientific evidences for the quality standard improvement of toad venom to be described in the next edition of Chinese pharmacopoeia(2020 edition).


Assuntos
Venenos de Anfíbios , Bufanolídeos , Animais , Bufonidae , Cromatografia Líquida de Alta Pressão , Pós , Controle de Qualidade
15.
Zhongguo Zhong Yao Za Zhi ; 45(8): 1734-1744, 2020 Apr.
Artigo em Chinês | MEDLINE | ID: mdl-32489056

RESUMO

In order to provide scientific recommendations for the revision of the quality standards of Poria in Chinese Pharmacopoeia(Ch. P) 2020 edition, a series of experiments were carried out to improve the quality standards of Poria. TLC methods were established to identify Poria by using pachymic acid, dehydrotumulosic acid and reference herbs as reference substances. The contents of water, total ash, pesticide residues, heavy metals and deleterious element, mycotoxins, sulfur dioxide residues and ethanol-soluble extract of herbal materials and decoction pieces of Poria were determined according to the methods recorded in the volume Ⅳ of Ch. P 2015 edition. An HPLC method was developed for the determination of pachymic acid and dehydropachymic acid. The contents of polysaccharide were determined by spectrophotometry using D-glucose as reference substance. The quality standards were established on the basis of the research results, in which the [assay] were added, and the [identification] and [tests] were revised when compared with Ch. P 2015 edition. The established methods are simple, specific, repeatable, and suitable for the quality evaluation of Poria.


Assuntos
Medicamentos de Ervas Chinesas , Poria , Cromatografia Líquida de Alta Pressão , Padrões de Referência
16.
Zhongguo Zhong Yao Za Zhi ; 45(8): 1745-1755, 2020 Apr.
Artigo em Chinês | MEDLINE | ID: mdl-32489057

RESUMO

Paridis Rhizoma is prepared from the dried rhizoma of Paris polyphylla var. yunnanensis or P. polyphylla var. chinensis. For the improvement of the quality standard of Paridis Rhizoma described in Chinese Pharmacopoeia(2015 edition), it is proposed that the quality marker no longer contains polyphyllin Ⅵ, and instead, polyphyllin H is an alternative for the quantitative analysis. To determine polyphyllin Ⅰ, Ⅱ, H and Ⅶ in the Paridis Rhizoma samples collected from the different growing area in China, HPLC method was established using the same chromatographic conditions as those for simultaneous determination of polyphyllin Ⅰ, Ⅱ, Ⅵ and Ⅶ described in Chinese Pharmacopoeia(2015 edition). The methodology validation indicated that there was a good linearity among the ranges of 0.006 48-0.828, 0.006 52-0.834, 0.006 17-0.790, 0.006 31-0.808 g·L~(-1) for polyphyllin Ⅰ, Ⅱ, H and Ⅶ, respectively. The average recoveries of four components were 100.2%-101.4%, with RSD less than 3.5%. The total amount of polyphyllin Ⅰ, Ⅱ, H and Ⅶ in the analyzed samples of P. polyphylla var. chinensis and P. polyphylla var. yunnanensis ranged from 0.050 9% to 3.99% and from 0.115% to 3.23%, respectively. In the tested samples collected from other Paris plants, there are high content of steroidal saponins in the samples of P. fargesii and P. forrestii, low content in the samples of P. polyphylla var. stenophylla, P. delavayi and P. thibetica, and almost not occurrence in the sample of P. mairei. As a representative adulterant of Paridis Rhizoma processed slices, 7 batches of Trillium samples contained high amount of polyphyllin Ⅵ and did not have polyphyllin H. Based on the present investigation, it is recommended that polyphyllin H together with polyphyllin Ⅰ, Ⅱ and Ⅶ are suitable for the improvement of quality standard of Paridis Rhizoma and the total amount of four components are not less than 0.80%.


Assuntos
Liliaceae , Melanthiaceae , Saponinas , China , Rizoma
17.
Zhongguo Zhong Yao Za Zhi ; 45(8): 1756-1763, 2020 Apr.
Artigo em Chinês | MEDLINE | ID: mdl-32489058

RESUMO

Sophorae Flavescentis Radix is prepared from the root of Sophora flavescens. The comprehensive knowledge of the effective components in S. flavescens makes its quality standard improvement more possible. TLC identification method for main flavonoids and alkaloids in one test was established using GF_(254) thin layer plate and the lower solution of chloroform-methanol-water-formic acid(4∶2∶1∶0.6) as developing solvent. The quantitative method of marker alkaloids was revised including the simplified sample preparation procedure and the chromatographic conditions. The determination of four alkaloids in the samples indicated that 32 batches of tested samples were qualified ones. The total oxymatrine and matrine, total oxysophocarpine and sophocarpine, as well as total amount of four tested components in the different samples were 1.08%-2.55%, 0.369%-0.860%, 1.67%-3.40%, respectively. There was a significantly positive correlation between oxymatrine and oxysophocarpine. Total oxymatrine and matrine had same correlation with total oxysophocarpine and sophocarpine. The moisture content and extractive in 32 batches of samples fulfilled the require of not more than 11.0% and not less than 20.0%, respectively. Thirteen tested pesticides were not detected in 12 batches of samples. The present study provided the evidence for the revision of quality standard of Sophora Flavescentis Radix.


Assuntos
Medicamentos de Ervas Chinesas , Sophora , Flavonoides , Quinolizinas
18.
Zhongguo Zhong Yao Za Zhi ; 45(9): 2091-2102, 2020 May.
Artigo em Chinês | MEDLINE | ID: mdl-32495558

RESUMO

Taking Lonicerae Japonicae Flos as an example, the method of "expert consensus of different regions" was used to screen the representative samples and evaluate their commodity grades. The correlation analysis, hierarchical cluster analysis and partial least squares discriminant analysis(PLS-DA) of "commodity grade-appearance characteristic-component content" were carried out to reveal the scientificity of traditional commodity grade of Chinese medicinal material. By referring to the existing literature and the grade investigation from the sample collection regions, 78 "initial grade" samples were screened out from 118 collected samples. Authoritative experts from four regions(n=4) including Linyi(Shangdong province), Bozhou(Anhui province), Anguo(Hebei province) and Beijing were organized to evaluate their commodity grades, separately. Based on the grade consistency rate(R_i≥70%), 69 "local grade" samples were screened out from the "initial grade" samples. Based on the average grade consistency rate ■ "authoritative grade" samples were screened out from the "local grade" samples, including15 first-grade samples, 9 second-grade samples, 11 third-grade samples and 17 fourth-grade samples. For these "authoritative grade" samples, the main appea-rance characteristics were quantified and the contents of 13 components were determined by ultra performance liquid chromatography(UPLC). Furthermore, the total contents of 6 phenolic acids, 4 flavonoids and 3 iridoids were calculated, respectively. The results of correlation analysis showed that 4 appearance characteristics indices were correlated with the commodity grades: color, rate of yellow bars(including blooming flowers), rate of black heads(including black bars), and rate of stems and leaves(including bud debris). Five component content indices were correlated with the commodity grades: chlorogenic acid, isochlorogenic acid C, sweroside, loganin and the total contents of six phenolic acids. Furthermore, chlorogenic acid, loganin and the total contents of six phenolic acids showed significantly negative correlation with the main appearance characteristics, indicating that the appearance characteristics of Lonicerae Japonicae Flos can reflect its internal quality, and these 3 indices can be used as quality markers(Q-markers). The results of hierarchical cluster analysis showed that the samples of four grades were classified into four categories, and the samples with the same grades and the same categories accounted for 80.8% of the total samples, while the samples with the different grades were obviously classified into different categories. The results of PLS-DA analysis showed that the samples of different grades showed obvious intragroup aggregation and intergroup dispersion. The above results indicated that it was feasible to evaluate the traditional commodity grade of Lonicerae Japonicae Flos by the method of "expert consensus of different regions". For the evaluation of traditional commodity grade of Chinese medicinal material, the samples should be representative, expert conclusions should have enough consensuses, and grade determination should be authoritative. As the crystallization of clinical experience, traditional commodity grade can scientifically reflect the internal quality of Chinese medicinal material.


Assuntos
Medicamentos de Ervas Chinesas , Lonicera , Cromatografia Líquida de Alta Pressão , Flores , Controle de Qualidade
19.
Zhongguo Zhong Yao Za Zhi ; 45(6): 1350-1356, 2020 Mar.
Artigo em Chinês | MEDLINE | ID: mdl-32281347

RESUMO

To define the composition of relevant substances in Breviscapine for Injection, in order to improve the quality control of impurity, and ensure the clinical safety. The analysis and structural identification of relevant substances in different specifications and batches of Breviscapine for Injection powders were carried out by HPLC and UPLC-QTOF-MS. Three primary relevant substances, namely 5,6,7,3',4'-pentahydroxyflavone-7-O-glucuronide(3), 3,5,6,7,4'-pentahydroxyflavone-3-O-glucuronide(4) and scutellarein(10), as well as three minor impurities, namely 6-hydroxyapigenin-6-O-glucosyl-7-O-glucuronide(1), methoxylscutellarin(6) and apigenin-7-O-glucuronide(7) were structurally identified by matching retention time, UV spectra, and mass spectra with authentic compounds and MS fragmentation rules. The main relevant substances(3) and(4) were separated and purified by semi-preparative HPLC, and their structures were further confirmed by NMR data. The study defined relevant substances of Breviscapine for Injection, and provided reference for improving the quality control level of single impurity in breviscapine preparation.


Assuntos
Apigenina/análise , Medicamentos de Ervas Chinesas/normas , Flavonoides/química , Glucuronídeos/análise , Cromatografia Líquida de Alta Pressão , Injeções , Espectroscopia de Ressonância Magnética , Espectrometria de Massas , Controle de Qualidade
20.
Zhongguo Zhong Yao Za Zhi ; 44(4): 730-739, 2019 Feb.
Artigo em Chinês | MEDLINE | ID: mdl-30989886

RESUMO

To solve the problems of the poor resolution of chromatographic separation,the weak durability of the relative correction factors,and the low accuracy of content determination results in the quantitative analysis of multi-components by single-marker( QAMS) method with andrographolide as the internal reference substance in the existing research of Andrographis Herba,a new QAMS method using dehydroandrographolide as the internal reference substance was established for the first time in this study. This new method can be used to simultaneously determine four diterpene lactones,including andrographolide( A),neoandrographolide( B),14-deoxyandrographolide( C),and dehydroandrographolide( S) through the optimization of chromatographic conditions and systematic investigation of methodology. At the present HPLC chromatographic conditions,four components could be well separated( R > 1. 5),and the methodology validations could satisfy the requirement of quantitative analysis. The relative correction factors( RCFs) of fA/S,fB/S,fC/S were determined as 0. 65,0. 54,0. 78,respectively. The relative standard deviations( RSDs) of their RCFs ranged between 1. 3%-5. 1%,0. 25%-0. 33%,0. 070%-0. 15%,0. 070%-0. 22%,respectively with three brands of HPLC instruments,five brands of C18 column,different flow rates( 0. 9,1. 0,1. 1 m L·min~(-1)),and different column temperatures( 25,30,35 ℃),indicating good durability of the RCFs. The relative retention value( RRV) method was used to locate the chromatographic peak of the components to be determined.The RRVs of rA/S,rB/S,and rC/Swere 0. 44,0. 86,0. 97,respectively. The RSDs of the RRVs ranged between 0. 030%-1. 6% with different HPLC instruments and columns,showing accurate peak location. The present QAMS method and the external standard method( ESM)were both used to determine the contents of four diterpene lactones from Andrographis Herba( 6 batches of medicinal materials and 18 batches of cut crude drugs). The relative errors of the determined content results between two methods were less than 2. 0%. It demonstrated that there was no significant difference in content results between these two methods,indicating good accuracy of the present QAMS method. Therefore,in this study,an accurate and highly durable QAMS method using dehydroandrographolide as the internal reference substance was established for simultaneous determination of four diterpene lactones. This method could be used to effectively control the quality of Andrographis Herba and provide technical basis for the formulation of traditional Chinese medicine industry standard and improvement of the Chinese Pharmacopoeia standard of Andrographis Herba.


Assuntos
Andrographis , Medicamentos de Ervas Chinesas , Cromatografia Líquida de Alta Pressão , Diterpenos , Controle de Qualidade
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