Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Preparation method of medicinal sodium cholesteryl sulfate

A cholesteryl sulfate, pharmaceutical grade technology, applied in the direction of pharmaceutical formulations, medical preparations containing active ingredients, steroids, etc., can solve problems such as the exact yield of cholesteryl sulfate sodium, achieve low toxicity and ensure safety Effect

Active Publication Date: 2020-05-05
CSPC ZHONGQI PHARM TECH (SHIJIAZHUANG) CO LTD
View PDF2 Cites 4 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Therefore, the final product reported in this paper is also a mixture of cholesteryl sulfate sodium and cholesteryl sulfate, and the reported yield is not the accurate yield of cholesteryl sulfate sodium

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Preparation method of medicinal sodium cholesteryl sulfate
  • Preparation method of medicinal sodium cholesteryl sulfate
  • Preparation method of medicinal sodium cholesteryl sulfate

Examples

Experimental program
Comparison scheme
Effect test

experiment example 1

[0066] Experimental Example 1: HPLC Determination of Cholesterol Sulfate and Sodium Cholesterol Sulfate

[0067] Cholesterol sulfate and cholesterol are detected respectively by the HPLC method of Yang Zhimin et al. Sodium Sulfate:

[0068] Chromatographic conditions: liquid chromatography, UV detector, Kromasil C8 column (250mm×4.6mm, 5μm), 0.01mol / L ammonium acetate solution-acetonitrile (7:33) as mobile phase, detection wavelength 210nm.

[0069] Take 50mg of cholesteryl sulfate and sodium cholesteryl sulfate, weigh them accurately, place them in different 100mL measuring bottles, add mobile phase to dissolve and dilute to the mark, shake well, and use it as the test solution. Accurately measure 20 μL respectively and inject them into the liquid chromatograph, and record the chromatograms. in figure 1 for cholesterol sulfate, figure 2 Sodium Cholesterol Sulfate.

[0070] As can be seen from the figure, the peak times of cholesteryl sulfate and sodium cholesteryl sulfa...

Embodiment 1

[0080] Embodiment 1: the preparation of cholesterol sulfate

[0081]Put cholesterol and dimethylformamide (80mL) into a three-neck flask, heat and stir. After the cholesterol is completely dissolved, add sulfamic acid, heat to the reaction temperature, and stir vigorously for about 2 hours. After the reaction is complete, lower the temperature to 25°C and stir to crystallize until the crystallization is complete, filter, add anhydrous methanol to wash the filter cake, drain to obtain the intermediate product, and calculate the molar yield and residual cholesterol. When the above other conditions were the same, the amount of raw materials added and the reaction temperature were changed to observe their influence on the molar yield and residual cholesterol. The results are shown in Table 1.

[0082] Table 1. The impact of raw material addition and reaction temperature on the preparation of cholesteryl sulfate

[0083]

[0084] The results in Table 1 show that when the feed r...

Embodiment 2

[0100] Embodiment 2: the preparation of sodium cholesteryl sulfate

[0101] The intermediate product cholesterol sulfate (10 g cholesterol, 25.86 mmol) was prepared according to the method of Example 1-4.

[0102] The intermediate product cholesterol sulfate prepared in Examples 1-4 was added into anhydrous methanol, stirred and heated to the reaction temperature, and refluxed for 1 h. Add a solution of sodium hydroxide in anhydrous methanol (sodium hydroxide is dissolved in 30 mL of anhydrous methanol), control the temperature and continue to reflux for 3 hours, stir and cool down to 25°C, then stir and crystallize at 25°C, filter until no liquid flows out. Add purified water to wash the filter cake, suction filter until no liquid flows out, then wash the filter cake with anhydrous methanol, suction filter until no liquid flows out, and dry the filter cake to obtain the final product. Based on the amount of cholesterol fed, calculate the total molar yield . When above-menti...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention provides medicinal sodium cholesteryl sulfate and a preparation method thereof. By controlling the addition proportion of cholesterol, sulfamic acid and sodium hydroxide, the content ofsodium ions in the product is within the range of 4.5%-4.9%, it is guaranteed that the final reaction product is basically pure sodium cholesteryl sulfate and hardly contains cholesterol sulfate, anda qualified raw material is provided for safely and effectively applying sodium cholesteryl sulfate.

Description

technical field [0001] This patent relates to the field of drug synthesis, in particular to a preparation method of pharmaceutical grade sodium cholesterol sulfate. Background technique [0002] Cholesteryl sulfate sodium, the chemical name is 5-cholesten-3β alcohol sodium sulfate, the CAS number is 2864-50-8, and the structure is as follows: [0003] [0004] Sodium cholesteryl sulfate is a relatively polar lipid compound with a polarity close to that of the skin. It is a negatively charged lipid and is suitable for use as a membrane material for preparing liposomes from positively charged drugs. The liposomes it participates in, because they have the same lipids as the stratum corneum, are easy to fuse with each other, which can make the drug have greater skin permeability and stability. Sodium cholesteryl sulfate is a pharmaceutical excipient for preparing amphotericin B. Since the amphotericin B currently on the market is an injection, the finished product of sodium...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Applications(China)
IPC IPC(8): C07J31/00A61K31/575
CPCC07J31/006
Inventor 米斌李海霞刘晓鹏赵永璐刘静媛韩培培
Owner CSPC ZHONGQI PHARM TECH (SHIJIAZHUANG) CO LTD
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com