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1.
Article in Chinese | WPRIM | ID: wpr-888031

ABSTRACT

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.


Subject(s)
China , Chromatography, High Pressure Liquid , Medicine, Chinese Traditional , Nonprescription Drugs , Quality Control
2.
Article in Chinese | WPRIM | ID: wpr-888029

ABSTRACT

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.


Subject(s)
Basidiomycota , Chromatography, High Pressure Liquid , Guanosine , Nucleosides , Tandem Mass Spectrometry
3.
Article in Chinese | WPRIM | ID: wpr-888028

ABSTRACT

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.


Subject(s)
Chromatography, High Pressure Liquid , Liliaceae , Melanthiaceae , Rhizome , Saponins , Tandem Mass Spectrometry
4.
Article in Chinese | WPRIM | ID: wpr-878986

ABSTRACT

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.


Subject(s)
Astragalus Plant , Chromatography, High Pressure Liquid , Drugs, Chinese Herbal , Saponins , Triterpenes/analysis
5.
Article in Chinese | WPRIM | ID: wpr-888062

ABSTRACT

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.


Subject(s)
Chromatography, High Pressure Liquid , Drugs, Chinese Herbal , Plant Extracts , Plant Leaves
6.
Article in Chinese | WPRIM | ID: wpr-888061

ABSTRACT

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.


Subject(s)
Drugs, Chinese Herbal , Medicine, Chinese Traditional , Plant Roots , Rhizome , Sophora
7.
Article in Chinese | WPRIM | ID: wpr-888060

ABSTRACT

As anti-aging ingredients, β-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.


Subject(s)
Chromatography, High Pressure Liquid , Chromatography, Liquid , Dendrobium , NAD , Nicotinamide Mononucleotide , Tandem Mass Spectrometry
8.
Article in Chinese | WPRIM | ID: wpr-888059

ABSTRACT

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.


Subject(s)
Liliaceae , Melanthiaceae , Plant Extracts , Rhizome , Saponins
9.
Article in Chinese | WPRIM | ID: wpr-888058

ABSTRACT

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.


Subject(s)
Animals , Flavonoids , Molecular Docking Simulation , Monophenol Monooxygenase , Plant Extracts/pharmacology , Plant Roots , Sophora
10.
Article in Chinese | WPRIM | ID: wpr-873166

ABSTRACT

Objective:To study the water soluble chemical constituents in rhizoma of Acorus tatarinowii and transformation pathway of nucleosides in the process of water extraction. Method:Compounds were isolated and purified by column chromatography on macroporous resin,Sephadex LH-20,ODS and preparative HPLC. Their structures were identified on the basis of physicochemical properties and spectral data. Nucleosides were identified from aqueous extract of A. tatarinowii,and their stability was investigated by HPLC. The possible transformation pathways of nucleosides in aqueous extract of A. tatarinowii were studied by nucleotide addition test. Result:Eleven compounds including four nucleosides,four phenylpropanoids,two alkaloids and a furfural were isolated,and identified as uridine(1),adenine(2),guanosine(3),adenosine(4),5-hydroxymethylfurfural(5),5-(hydroxymethyl)-1H-pyrrole-2-carboxaldehyde(6),(threo)1',2'-dihydroxyasarone(7),(erythro)1',2'-dihydroxyasarone(8),acoraminol A(9),acoraminol B(10),and tatarine A(11). The chromatographic peaks of compounds 1-4 and cytidine were identified from aqueous extract of A. tatarinowii by HPLC. After ultrasonic extraction for 0.5 h,the stability of nucleosides in water was poor. After ultrasonic extraction for 3 h or refluxing extraction for 0.5 h,the stability of nucleosides in water was good. Four transformation pathways including 5'-cytidylic acid→cytidine,uridine monophosphate→uridine,guanosine monophosphate,guanosine and adenosine-5'-monophosphate,adenosine 5'-diphosphate,adenosine 5'-triphosphorate,adenosine,adenine might exist in water extract of A. tatarinowii. Conclusion:Compounds 1-4 and 6 were isolated from the genus Acorus for the first time. These compounds further enriched the chemical constituents of A. tatarinowii. The stability and transformation pathway of nucleosides in A. tatarinowii provides reference data for the analysis of nucleosides in A. tatarinowii and other traditional Chinese medicine.

11.
Article in Chinese | WPRIM | ID: wpr-827975

ABSTRACT

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.


Subject(s)
Chromatography, High Pressure Liquid , Drugs, Chinese Herbal , Flowers , Lonicera , Quality Control
12.
Article in Chinese | WPRIM | ID: wpr-777501

ABSTRACT

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.


Subject(s)
Andrographis , Chromatography, High Pressure Liquid , Diterpenes , Drugs, Chinese Herbal , Quality Control
13.
Article in Chinese | WPRIM | ID: wpr-801905

ABSTRACT

Objective:To study the appearance description,TLC examination and content determination was carried out, in order to improve the quality standard of processed slices of Paridis Rhizoma in the 2020 edition of Chinese Pharmacopoeia. Method:Based on the literature review and observation on the samples,the appearance description was described. TLC examination was used for the qualitative analysis. HPLC was used for the determination of polyphyllin Ⅰ,Ⅱ,Ⅵ and Ⅶ in the commercial and processed samples. UPLC was employed for the determination of 10 steroidal saponins,namely pseudoprotodioscin,polyphyllin Ⅶ,17-hydroxygracillin,polyphyllin H,polyphyllin Ⅵ,polyphyllin Ⅱ,dioscin,gracilin,polyphyllin Ⅰ and polyphyllin Ⅴ. Result:For the appearance description,color and luster,texture,odor and taste as well as the diameter of 1.0-4.5 cm were recorded. polyphyllin Ⅵ was not detected in the thin layer chromatograms of most of the tested samples derived from high-quality species but obviously detected in those of Trillium Rhizoma. Five of 13 commercial samples met the requirements that the total amounts of polyphyllin Ⅶ,Ⅵ,Ⅱ,and Ⅰ should be no less than 0.6%according to the current Chinese Pharmacopoeia. Because softening and drying had the obvious influence on the contents of steroidal saponins in the samples,soaking and sun-drying were preferred. Conclusion:Appearance description should be supplemented. Polyphyllin Ⅵ is not considered as one of quality markers for the TLC identification and HPLC determination of Paridis Rhizoma. Polyphyllin H was considered as a new marker for the quality control. It is recommended that the total amounts of polyphyllin Ⅶ,H,Ⅱ,and Ⅰ should be no less than 1.0%.

14.
Article in Chinese | WPRIM | ID: wpr-771709

ABSTRACT

To investigate the differences of chemical compositions in Gynostemma pentaphyllum leaves prepared by different processing methods. Ultra performance liquid chromatography-quadrupole time-of-flight mass spectrometry(UPLC-Q-TOF-MS) was used to compare the chemical compositions between shade-dried processing and drum-dried processing. Forty six gypenosides were identified by control comparison, liquid chromatography-mass spectrometry(LC-MSn) fragmentation information, and literature data. The mass spectral peak area statistics was combined with principal component analysis(PCA), and the results showed that eight batches of Gynostemma pentaphyllum leaves samples were divided into two groups according to the two different processing methods; ten chemical compositions with significant differences were screened according to mass spectrum information combined with partial least-squares discriminant analysis(PLS-DA). The result showed that most parent nucleus of the gypenosides contained three to four glycosides in drum-dried samples, and one to two glycosides in the shade-dried samples. It was inferred from further MS analysis that desugarization of gypenosides was present to produce secondary glycosides with the effect of glucosidase in the shade-drying, thus resulting in difference in compositions. This study provided data support for harvesting, processing and quality control of Gynostemma pentaphyllum leaves.


Subject(s)
Chromatography, High Pressure Liquid , Gynostemma , Chemistry , Mass Spectrometry , Plant Leaves , Chemistry , Saponins , Chemistry
15.
Article in Chinese | WPRIM | ID: wpr-687373

ABSTRACT

Toad venom (Chansu) is prepared from the dried secretion of parotid gland and skin gland from Bufo bufo gargarizans or B. melanostictus. Up to now, much attention shall be paid to the poor quality of commercial toad venom because of the adulteration. So, it is urgent to establish a scientific and perfect quality control method to improve the quality of toad venom and guarantee its safety and effectiveness in clinical application. The different batches of toad venom samples were assayed by high performance liquid chromatography (HPLC) and the quantitative analysis of multi-components by single marker (QAMS) was used to detect the contents of five bufagenins. As a result, the reference characteristic chromatogram was established, displaying serotonin, gamabufotalin, arenobufagin, hellebrigenin, telocinobufagin, bufotalin, cinobufotalin, bufalin, cinobufagin and resibufogenin as characteristic peaks. Taking cinobufagin as an internal reference substance, QAMS was verified for the determination of five bufagenins (gamabufotalin, bufotalin, bufalin, cinobufagin, resibufogenin) in toad venom samples. The durability and applicability of the relative correction factor (RCF) were also studied systematically. RCFs of cinobufagin to gamabufotalin, bufotalin, bufalin and resibufogenin were determined as 1.05, 0.895, 1.09 and 0.913, respectively. The characteristic chromatogram and QAMS established in this study could effectively control the quality of toad venom and provide scientific evidence for the improvement of the quality standard of the toad venom to be described in Chinese Pharmacopoeia (2020 edition).

16.
Article in Chinese | WPRIM | ID: wpr-687372

ABSTRACT

To systematically identify the related substances in the original materials of breviscapine injection, 18 batches of samples collected from different pharmaceutical companies, its ethanol extract and breviscapine mother liquor concentrate were analyzed by high performance liquid chromatography (HPLC), and their structures were identified by ultra performance liquid chromatography and quadruple/time-of-flight mass spectrometry (UPLC-QTOF-MS). Under the selected chromatographic conditions, scutellarin and related substances have good resolution and 13 related substances were observed. Based on the molecular weight and fragmentation patterns obtained by UPLC-QTOF-MS as well as reference substances, their structures were elucidated as 6-hydroxyapigenin-6--glucosyl-7--glucuronide (1), 5,7,8,3',4',5'-hexahydroxyflavone-7--glucuronide (2), 5,6,7,3',4'-pentahydroxyflavone-7--glucuronide(3)and its isomer (4), patuletin-3--glucuronide (5), methoxylscutellarin (6), apigenin 7--glucuronide (7), isorhamnetin 7--glucuronide (8), diosmetin 7--glucuronide (9), scutellarein (10), scutellarin methyl ester (11), scutellarin ethyl ester (12), and apigenin (13). This study has clarified related substances in the original materials of breviscapine injection, providing references for the improvement of quality control for breviscapine drug material and its preparations.

17.
Article in Chinese | WPRIM | ID: wpr-350181

ABSTRACT

To optimize the purification process of gynostemma pentaphyllum saponins (GPS) based on "adjoint marker" online control technology with GPS as the testing index. UPLC-QTOF-MS technology was used for qualitative analysis. "Adjoint marker" online control results showed that the end point of load sample was that the UV absorbance of effluent liquid was equal to half of that of load sample solution, and the absorbance was basically stable when the end point was stable. In UPLC-QTOF-MS qualitative analysis, 16 saponins were identified from GPS, including 13 known gynostemma saponins and 3 new saponins. This optimized method was proved to be simple, scientific, reasonable, easy for online determination, real-time record, and can be better applied to the mass production and automation of production. The results of qualitative analysis indicated that the "adjoint marker" online control technology can well retain main efficacy components of medicinal materials, and provide analysis tools for the process control and quality traceability.

18.
Article in Chinese | WPRIM | ID: wpr-350178

ABSTRACT

To observe the protective effect of scutellarin ethyl ester on focal cerebral ischemia injury induced by middle cerebral artery occlusion in rats(MCAOR), and explore its mechanism. Totally 84 male SD rats were randomly divided into seven groups: sham-operated group, model group,positive drug group(niomdipine,12 mg•kg⁻¹), Brevisapin tablets group(48 mg•kg⁻¹), and high, middle and low-dose scutellarin ethyl ester groups(100, 50, 25 mg•kg⁻¹). The MCAOR model was prepared by using thread embolism method to observe the neurological function of rats, the area of cerebral infarction was measured with TTC, and the levels of MDA, SOD and NO in serum were detected with semiautomatic biochemistry analyzer.Ox-LDL and TNF-α cell injury models was established by treating HUVECs with 200 mg•L⁻¹ ox-LDL and 100 μg•L⁻¹ TNF-α,and the levels of MDA, SOD, NO, ET, 6-keto-PGF1α,TXB2, IL-1, IL-6, IL-8, ICAM-1 and PECAM-1 in the cell supernatant were determined. The results showed that scutellarin ethyl ester could effectively improve the neurological function of MCAOR rats, and significantly reduce the area of cerebral infarction. Compared with the model group, activities of SOD and NO in serum increased, while content of MDA decreased. In the cell supernatant, activities of SOD, 6-keto-PGF1α and NO increased, content of IL-1, IL-6, IL-8, ICAM-1, PECAM-1, TXB2, ET and MDA decreased, which indicated that scutellarin ethyl ester has a certain protective effect on focal cerebral ischemia injury induced by middle cerebral artery occlusion in rats, and its mechanism may be related to antioxidative stress, improvement of endothelial function and reduction in inflammatory reaction.

19.
Article in Chinese | WPRIM | ID: wpr-258498

ABSTRACT

Sophorae Tonkinensis Radix et Rhizoma, which has been commonly used in clinic, shows activities in antitumor, antivirus, antibacteria, analgesia, anti-inflammation, anti-liver injury, anti-oxidation and immune enhancement, but can cause liver toxicity, neurotoxicity, gastrointestinal toxicity and respiratory toxicity. Its pharmacological effect and toxicity are related to extraction process, dosage and administration time. Therefore, exploration of appropriate extraction process, toxicity-effect dosage range, toxic substance basis provides guarantee for attenuation and safe clinical medication.

20.
Article in Chinese | WPRIM | ID: wpr-275448

ABSTRACT

Toad venom (Chansu) is prepared from the dried secretion of Bufo bufo gargarizans or B. melanostictus. It is not only one of the famous and expensive traditional Chinese medicines(TCMs) from animal origin, but also one of 28 kinds of toxic TCMs to be required for special management issued by the State Council of the People's Republic of China. Chansu contains the rich bufadienolides and indole alkaloids, and displays various bioactivity including cardiotonic, anti-tumor, analgesia, and local anesthesia. Based on the published references in the recent years, the advance on the identification of adulterants and quality evaluation as well as the influence factors on the quality of toad venom was summarized to improve the quality standards and promote the level of quality control of toad venom and its preparations.

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