Method for measuring contents of indole alkaloids in cinobufagin alcohol precipitation liquid

A technology of cinobufacinol and indole, which is applied in the field of determination of indole alkaloid content in cinobufacinol precipitation solution, to achieve the effect of reducing the difference between batches and saving manpower and material resources

Inactive Publication Date: 2011-04-27
ZHEJIANG UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, in the current reports, there are very few applications of near-infrared spectroscopy to the rapid analysis of active ingredients in the alcohol precipitation process.

Method used

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  • Method for measuring contents of indole alkaloids in cinobufagin alcohol precipitation liquid
  • Method for measuring contents of indole alkaloids in cinobufagin alcohol precipitation liquid
  • Method for measuring contents of indole alkaloids in cinobufagin alcohol precipitation liquid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] 1 Calibration collection of alcohol sediment samples

[0029] Concentrate the extract obtained from the water extraction of toad skin to a density of 1.12g / mL, take 1L of the water extraction concentrate and place it in an alcohol sink, keep the mechanical stirring speed at 300rpm at a temperature of 40°C, and use 60mL / min Add 95% (v / v) ethanol at a flow rate until the end point ethanol concentration of the medicinal solution is 70% (v / v). The alcohol precipitation process continued for 50 minutes, and while adding ethanol, samples were taken regularly. A total of 55 samples from 4 batches of alcohol precipitation process of cinobufacin were collected and used as calibration set samples for model establishment.

[0030] 2 Determination of the reference value of the indole alkaloid content in the sample of calibration alcohol precipitation

[0031] (1) Preparation of reference substance solution: Accurately weigh 15 mg of 5-hydroxytryptamine reference substance, place ...

Embodiment 2

[0056] 1 Collection of alcohol precipitation liquid samples under different alcohol precipitation processes

[0057] Concentrate the extract obtained by water extraction of toad skin to a density of 1.15g / mL, take 1L of the water extraction concentrate and place it in an alcohol sink, keep the mechanical stirring speed at 500rpm at a temperature of 60°C, and use 60mL / min Add 95% (v / v) ethanol at a flow rate until the end point ethanol concentration of the medicinal solution is 75% (v / v). While adding ethanol, samples were taken at regular intervals. 16 cinobufacin alcohol-precipitated samples were obtained.

[0058] 2. Determination of reference value of indole alkaloid content in alcohol precipitation solution sample

[0059] The content of indole alkaloids in the sample in the above process was measured by ultraviolet spectrophotometry in step 2 of Example 1, and this content value was used as a reference value.

[0060] 3. Collection of near-infrared transmission spectru...

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Abstract

The invention provides a method for measuring the contents of indole alkaloids in cinobufagin alcohol precipitation liquid. The alcohol precipitation method is a key unit operation in the production process of cinobufagin injection and a quick and effective content analysis method aiming at the alcohol precipitation process is especially important. The method comprises the following steps of: collecting a representative alcohol precipitation liquid sample as a correction set; measuring the contents of the indole alkaloids by adopting ultraviolet visible spectrophotometry and scanning a near-infrared original spectrum chart of the bisindole alkaloids at the same time; selecting a proper spectrum preprocessing method, a modeling spectrum section and a main factor number; and constructing a near-infrared quantitative correction model of the indole alkaloid of the alcohol precipitation liquid sample and quickly measuring the content of the cinobufagin alcohol precipitation liquid sample with the unknown content by using a chemometric method. The invention has the advantages of quickness, no damage and accuracy, can effectively solve the problems of lacking of quality monitoring and batch difference in the alcohol precipitation process and provides a new idea and means for quality control of the traditional Chinese medicine process.

Description

technical field [0001] The invention belongs to a quality detection method in the production process of traditional Chinese medicines, and relates to a detection method for rapidly measuring the content of indole alkaloids in the alcohol precipitation process of cinobufacin injection by using near-infrared spectroscopy. Background technique [0002] Cinobufacin injection is a sterilized aqueous solution made from dried toad skin. It has the effects of reducing swelling, relieving pain and detoxifying. It is mainly used for treating middle and advanced tumors, chronic hepatitis B and other diseases. contagious tuberculosis, epidemic hemorrhagic fever, intractable hiccups and mumps complicated by meningitis in children. Due to its good anti-cancer effect, Cinobufacin Injection is currently listed as a Class A drug in the national basic medical insurance and a national protected traditional Chinese medicine. [0003] The production process of cinobufacin injection consists of ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): A61K35/56G01N21/33G01N21/35A61P35/00A61P1/16A61P31/20A61P31/06A61P31/12A61P1/00A61P31/14A61P25/00A61K35/65G01N21/359
Inventor 刘雪松孙笛王龙虎陈勇吴永江袁佳胡小雁高波张效蓬
Owner ZHEJIANG UNIV
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