Method for detecting concentration of six bufadienolide components in toad skin-containing medicinal material preparation in blood plasma or tissue

A technology of bufastenolide and detection method, which is applied in material separation, measurement device, analysis material and other directions, can solve problems such as unloaded dried toad skin and the like, achieves simplified sample pretreatment process, excellent chromatographic peak shape, Simple to use effects

Active Publication Date: 2021-01-08
GUANGZHOU PHARMACEUTICAL INDUSTRIAL RESEARCH INSTITUTE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The 2015 edition of "Chinese Pharmacopoeia" uses the total poisonous base amount of bufagenin and cinobufacin as the quality control index of toad venom, but it has not included the dried toad skin

Method used

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  • Method for detecting concentration of six bufadienolide components in toad skin-containing medicinal material preparation in blood plasma or tissue
  • Method for detecting concentration of six bufadienolide components in toad skin-containing medicinal material preparation in blood plasma or tissue
  • Method for detecting concentration of six bufadienolide components in toad skin-containing medicinal material preparation in blood plasma or tissue

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preparation example Construction

[0065] (1) Preparation of stock solution:

[0066] 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 stock solution; the standard stock solution is mixed to obtain a mixed standard stock solution;

[0067] Dissolve reserpine in (50±5)% acetonitrile aqueous solution to prepare reserpine stock solution;

[0068] (2) Preparation of working solution:

[0069] Dilute the mixed standard stock solution with (50 ± 5)% acetonitrile aqueous solution respectively to prepare a mixed standard curve sample working solution and a mixed quality control sample working solution;

[0070] Dilute the reserpine stock solution with (50 ± 5)% acetonitrile aqueous solution to prepare an internal standard working solution;

[0071] (3) Preparation of the sample solution to be tested:

[0072] Preparation of the plasma sample solution to be tested: ...

Embodiment 1

[0133] (1) Preparation of solution

[0134] Preparation of stock solutions:

[0135] Weigh an appropriate amount of standard products of the main components of toad skin medicinal materials, Bufagenin, Bufalin, Cinobufabufin, Cinobufafalin, Yuanhuabufajing, and Shabubufajing, and dissolve them in an appropriate amount of 50% acetonitrile In the aqueous solution, standard stock solutions with a concentration of 1.00 mg / mL were prepared. Three standard stock solutions with a concentration of 1.00 mg / mL were mixed in equal volumes, and an appropriate amount of 50% acetonitrile aqueous solution was added to prepare a mixed standard stock solution with a concentration of 0.100 mg / mL for the six bufacardenolactone components.

[0136] Take an appropriate amount of reserpine standard substance and dissolve it in 50% acetonitrile aqueous solution to prepare a reserpine stock solution with a concentration of 1.00 mg / mL.

[0137] Preparation of standard curve working solution:

[013...

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Abstract

The invention relates to a method for detecting the concentration of six bufadienolide components in a medicinal preparation containing toad skin in blood plasma or tissue. The method comprises the following steps: (1) preparing a stock solution, namely respectively dissolving resibufogenin, bufalin, cinobufagin, cinobufotalin, telocinobufagin and arenobufagin in a (50+/-5)% acetonitrile aqueous solution to prepare a standard stock solution; dissolving reserpine in a (50+/-5)% acetonitrile aqueous solution to prepare a reserpine stock solution; (2) preparing a working solution; (3) preparing ato-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 the detection process of the method, the chromatographic peak shape is excellent, a channel of each compound only has a unique target peak, theinterference of other effects such as solvent effects is avoided, 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 drug analysis, in particular to a method for detecting the concentration of six bufacardenolactone components in a medicinal preparation containing toad skin in blood plasma or tissue. 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. With the research progress of chemical composition and pharmacological activity, in addition to the traditional cardiotonic effect, the significant anti-tumor activity of toad skin medicinal materials and their active ingredients 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 孙晶晶殷玮戚园梅凌珊彭佳裕蔡文镇
Owner GUANGZHOU PHARMACEUTICAL INDUSTRIAL RESEARCH INSTITUTE
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