Method for the determination of plasma or tissue concentrations of six bufastenolide components in bufa skin-containing medicinal preparations

A technology of bufastenolactone and detection method, which is applied in the direction of material separation, measuring device, and analysis of materials, can solve the problem of unloaded toad skin, etc., and achieve simplified sample pretreatment process, simple operation, and high resolution Effect

Active Publication Date: 2022-07-29
GUANGZHOU PHARMACEUTICAL INDUSTRIAL RESEARCH INSTITUTE
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  • 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 the determination of plasma or tissue concentrations of six bufastenolide components in bufa skin-containing medicinal preparations
  • Method for the determination of plasma or tissue concentrations of six bufastenolide components in bufa skin-containing medicinal preparations
  • Method for the determination of plasma or tissue concentrations of six bufastenolide components in bufa skin-containing medicinal preparations

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preparation example Construction

[0065] (1) Preparation of stock solution:

[0066] Take the standard products lipobufaxin, bufalin, cinobufogen, cinobufalin, celinobufagin, xenobufalin, and dissolve them in (50±5)% acetonitrile aqueous solution respectively to prepare the standard product stock solution; mix the standard stock solution 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 sample solution to be tested:

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

Embodiment 1

[0133] (1) Preparation of solution

[0134] Preparation of stock solutions:

[0135] Weigh an appropriate amount of the standard products of the main components of bufaxin, bufalin, cinobufogen, cinobufogen, celinobufosin, and xenobufalin, respectively, and dissolve them in an appropriate amount of 50% acetonitrile. In aqueous solution, standard stock solutions with concentrations 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 the concentration of six bufastenolide components of 0.100 mg / mL.

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

[0137] Preparation of standard curve working solutions:

[0138] Dilute the stock solutions of the six b...

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Abstract

The present invention relates to a method for detecting the concentration of six bufastenolide components in plasma or tissue in preparations containing bufa skin. The method comprises the following steps: (1) preparation of a stock solution: lipobufaxin, bufalin, cinobufogen, cinobufulin, celinobufagin and xenobufalin are respectively dissolved in (50 ±5)% acetonitrile aqueous solution to prepare standard stock solution; dissolving reserpine in (50 ± 5)% acetonitrile aqueous solution to prepare reserpine stock solution; (2) preparation of working solution; (3) Preparation of the sample solution to be tested; (4) subjecting the sample solution to be tested obtained in step (3) to liquid chromatography separation; subjecting the sample separated by liquid chromatography to mass spectrometry analysis. In the detection process of the method of the invention, the chromatographic peak shape is excellent, and the channel of each compound has only a unique target peak, which avoids other interferences such as solvent effects, and has the advantages of simple operation, rapid analysis, high specificity and high resolution.

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 bufastenolide components in plasma or tissue in preparations containing bufa skin. Background technique [0002] The toad skin is the dry body of the amphibian toad with its internal organs removed. It was first published in "Ben Cao Feng Yuan". It is acrid, cool and slightly toxic. The medicinal toad skin mostly comes from the animal Chinese toad. This medicinal material is contained in widely used Chinese patent medicines such as Chansu Tablets (oral liquid, injection), Hechan Tablets, Dabaidu Capsules, and Ji Desheng She Tablets. Along with the research progress of chemical constituents and pharmacological activities, in addition to the traditional cardiotonic effect, the significant antitumor activity of toad skin and its active ingredients has attracted more and more attention of researchers. So far, the chemical compon...

Claims

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Application Information

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Patent Type & Authority Patents(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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