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Method for detecting six complex bufadienolide components in medicinal preparation containing toad skin

A technology of bufastenolide and detection method, which is applied in material separation, measurement device, analysis material and other directions, can solve the problems of not specifying certain components, short time of poisoning symptoms, uneven quality, etc. Excellent chromatographic peak shape, high sensitivity and good resolution

Pending Publication Date: 2021-01-12
GUANGZHOU PHARMACEUTICAL INDUSTRIAL RESEARCH INSTITUTE
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the quality of toad skin medicinal materials currently on the market is uneven, and the differences in harvesting and processing methods lead to large differences in the ingredients contained in the medicinal materials.
Studies have shown that the therapeutic dose of bufatenolactone is similar to the lethal dose, the symptoms of poisoning appear in a short time, and the safety factor is low. Therefore, it is urgent to establish a highly sensitive, specific, fast and efficient analysis for the components contained in toad skin Method, to provide basis for quality control and evaluation of toad skin medicinal materials, and to provide technical support for research on the activity of bufadenolactone
[0004] At present, there are patent reports on the quality control methods of toad skin medicinal materials or decoction pieces, all of which use HPLC to establish the fingerprints of characteristic peaks to indicate a certain type of compound, but not specific to certain components, and the method needs to be optimized

Method used

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  • Method for detecting six complex bufadienolide components in medicinal preparation containing toad skin
  • Method for detecting six complex bufadienolide components in medicinal preparation containing toad skin
  • Method for detecting six complex bufadienolide components in medicinal preparation containing toad skin

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preparation example Construction

[0062] (1) Preparation of stock solution:

[0063] Take the standard products Libufagenin, Bufalin, Cinobufagin, Cinobufalin, Cinobufagin, and Sandbufalin, respectively, and dissolve them in (50±5)% acetonitrile aqueous solution to prepare the standard product solution; six kinds of standard product solutions are mixed to obtain a mixed standard product stock solution;

[0064] (2) Preparation of standard curve solution:

[0065] Dilute the mixed standard stock solution with (50 ± 5)% acetonitrile aqueous solution respectively to prepare the mixed standard curve solution;

[0066] (3) Preparation of the sample solution to be tested:

[0067] Preparation of the sample solution to be tested: take toad skin medicinal materials, make powdery solid, add appropriate amount of 50±5% acetonitrile aqueous solution, ultrasonically extract for 30 minutes, then pass through a 0.22 μm microporous membrane, and filter the filtrate with 50±5% acetonitrile Dilute the aqueous solution to a ...

Embodiment 1

[0116] (1) Preparation of solution

[0117] Preparation of stock solutions:

[0118]Weigh an appropriate amount of standard products of the main components of toad skin medicinal materials, Libufagenin, Bufalin, Cinobufabufin, Cinobufafalin, Yuanhuabufajing and Sandbufatoxin, and dissolve them in an appropriate amount of 50% acetonitrile In the aqueous solution, standard solutions with a concentration of 1.00 mg / mL were prepared. Mix the three standard solutions with a concentration of 1.00 mg / mL in equal volumes, and add an appropriate amount of 50% acetonitrile aqueous solution to prepare a mixed standard stock solution with a concentration of 0.100 mg / mL for six complex bufacardenolactone components.

[0119] Preparation of standard curve solution:

[0120] Dilute the six kinds of complex bufacardenolactone components with 50% acetonitrile aqueous solution, the concentrations of which are all 0.100 mg / mL mixed standard stock solution, and the obtained concentrations are 0...

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Abstract

The invention provides a method for detecting six complex bufadienolide components in a medicinal material preparation containing toad skin. The method adopts high performance liquid chromatography tandem mass spectrometry detection, and comprises the following steps: (1) preparing a stock solution: respectively dissolving resibufogenin, bufalin, cinobufagin, cinobufotalin, telocinobufagin and arenobufagin in an acetonitrile aqueous solution to prepare a standard stock solution; (2) preparing a standard curve solution; (3) preparing a to-be-detected sample solution; (4) carrying out liquid chromatography separation on the to-be-detected sample solution obtained in the step (3); and carrying out mass spectrometric analysis on the sample subjected to liquid chromatography separation. In thedetection process of the method, the chromatographic peak shape is excellent, and a channel of each compound only has a unique target peak, so that interference of other effects such as solvent effects is avoided; and and the method is easy to operate, rapid in analysis, high in specificity and high in separation degree.

Description

technical field [0001] The invention relates to the technical field of traditional Chinese medicine analysis, in particular to a method for detecting six complex bufastenolactone components in medicinal material preparations. Background technique [0002] Toad skin is the dried viscera of toad, an animal belonging to the genus Toad of the amphibian class. It was first published in "Materia Medica Fengyuan". It is pungent, cool, and slightly toxic. Medicinal toad skin mostly comes from the animal Bufo bufo. Chansu Tablets (oral solution, injection), Hechan Tablets, Dabaidu Capsules, Jideshengshe Tablets and other Chinese patent medicines that are widely used in clinical practice all contain this medicinal material. In recent years, with the continuous deepening of research, the excellent anti-shock, anti-virus, and anti-tumor activities of the important active ingredient in toad skin—bufadenolactone has attracted extensive attention from scholars at home and abroad, and has ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/34G01N30/72G01N30/86
CPCG01N30/02G01N30/06G01N30/34G01N30/72G01N30/8675G01N2030/045
Inventor 倪庆纯孙晶晶殷玮周兰华胡钟芳
Owner GUANGZHOU PHARMACEUTICAL INDUSTRIAL RESEARCH INSTITUTE
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