Your browser doesn't support javascript.
loading
Show: 20 | 50 | 100
Results 1 - 3 de 3
Filter
Add filters








Language
Year range
1.
Article in Chinese | WPRIM | ID: wpr-940599

ABSTRACT

ObjectiveTo develop a quantitative analysis of multi-components by single marker (QAMS) for determination of bufalin, cinobufagin and resibufogenin in Shexiang Baoxin pills, and to provide a method for improving the national standard of the pills. MethodHigh performance liquid chromatography (HPLC) was developed for simultaneous determination of bufalin, cinobufagin and resibufogenin in Shexiang Baoxin pills and the methodology validation was carried out. The chromatographic separation was performed on a Nucleosil 100-5 C18 column (4.6 mm×250 mm, 5 μm) with the mobile phase of acetonitrile -0.1% potassium dihydrogen phosphate aqueous solution (pH adjusted to 3.2 with phosphoric acid) (48∶52), and the flow rate was 0.6 mL·min-1, the detection wavelength was set at 296 nm and the column temperature was 35 ℃. Taking cinobufagin as the internal standard, the relative correction factors (RCFs) of bufalin and resibufogenin were calculated, and the key influencing factors of RCFs were investigated. Relative retention time was used for the chromatographic peak location of the analyte, combining with the on-line ultraviolet spectroscopy and accurate relative molecular weight obtained by ultra-performance liquid chromatography-quadrupole time-of-flight mass spectrometry (UPLC-QTOF/MS). The external standard method was used to verify the contents of three components obtained by QAMS. ResultQAMS was established for the determination of bufalin, cinobufagin and resibufogenin in the samples, and RCFs of cinobufagin to bufalin and resibufogenin were 0.922 and 1.01, respectively. The total content of the three marker compounds in 11 batches of Shexiang Baoxin pills was 33.7-36.0 µg per pill. There was no significant difference between the quantitative results of QAMS and external standard method. ConclusionThe established method can be used for the quality control of bufalin, cinobufagin and resibufogenin in Shexiang Baoxin pills. It is suggested that bufalin should be considered as one of three marker compounds, and the sum of bufalin, cinobufagin and resibufogenin should be used for the content limit of this preparation.

2.
Article in Chinese | WPRIM | ID: wpr-949007

ABSTRACT

Based on standard sampling for Bufonis Venenum, this study analyzed the effect of the origin, and body weight and gender of Bufo bufo gargarizans on the quality of Bufonis Venenum. To be specific, mass spectrometry(MS) and the content determination methods in Chinese Pharmacopoeia(2020) were adopted. First, MS was performed on 76 Bufonis Venenum samples collected from 40 cities/counties in 17 provinces/autonomous regions which were derived from B. bufo gargarizans and B. melanostictus. Based on content determination, the body weight and gender of B. bufo gargarizans, which influenced the quality of Bufonis Venenum, were evaluated. Multivariate statistical analysis suggested huge difference in the material basis of the medicinal material derived from B. bufo gargarizans and B. melanostictus, and 9 differential compounds were identified. The content of components specified in Chinese Pharmacopoeia was higher in the medicinal material derived from B. bufo gargarizans than in the medicinal material derived from B. melanostictus. The content of the components specified in Chinese Pharmacopoeia was low in Bufonis Venenum derived from heavy B. bufo gargarizans, and higher in the Bufonis Venenum produced by male B. bufo gargarizans than in that produced by female B. bufo gargarizans irrespective of time and geographic location. In summary, this study provide new ideas and reference for the quality control of Bufonis Venenum, collection and processing of Bufonis Venenum, artificial breeding of B. bufo gargarizans, and biosynthesis mechanism of Bufonis Venenum.


Subject(s)
Animals , Male , Female , Bufanolides/analysis , Bufonidae , Mass Spectrometry , Quality Control , Body Weight
3.
Acta Pharmaceutica Sinica ; (12): 1120-1126, 2021.
Article in Chinese | WPRIM | ID: wpr-886994

ABSTRACT

Qualitative and quantitative methods were used to establish the quality of different medicinal parts of Poria cocos (Poriae Cutis, rubra Poria, white Poria, Poria cum Radix Pini) by using ultra-performance convergence chromatography coupled with photo-diode array and quadrupole time-of-flight mass spectrometry (UPC2-PDA-Q-TOF/MSE). A total of 18 chromatographic peaks were detected from Poria cocos by UPC2-PDA. Principal component analysis (PCA) and partial least squares discriminant analysis (PLS-DA) were used to compare the four medicinal parts. The results showed that there were significant differences in the components of different medicinal parts, and the main triterpenoic acids were poricoic acid A, poricoic acid B, dehydroeburicoic acid, and dehydrotrametenolic acid. When combined with the common active component polyporenic acid C, a method for determination of five triterpenoic acids in different parts of Poria cocos was established. These components could be separated within 15 min, and the amount of methanol was 3.63% of that of HPLC method. Taking the five triterpenoid acids as an index, the content of triterpenoid acids in different parts of Poria cocos from high to low were Poriae Cutis, rubra Poria, white Poria and Poria cum Radix Pini. The method is simple, rapid, and uses minimal solvent. The mobile phase of environment-friendly gas carbon dioxide has unique advantages in reducing environmental pollution, which can provide a basis for the development and standard formulation of Poria cocos and its related products.

SELECTION OF CITATIONS
SEARCH DETAIL