A kind of preparation method of pharmaceutical grade sodium cholesteryl sulfate

A cholesterol sulfate and cholesterol technology, which is applied in pharmaceutical formulations, medical preparations containing active ingredients, steroids, etc., can solve problems such as the accurate yield of sodium cholesteryl sulfate, achieve low toxicity, ensure safety, and reduce The effect of reaction cost

Active Publication Date: 2021-06-18
CSPC ZHONGQI PHARM TECH (SHIJIAZHUANG) CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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

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  • A kind of preparation method of pharmaceutical grade sodium cholesteryl sulfate
  • A kind of preparation method of pharmaceutical grade sodium cholesteryl sulfate
  • A kind of preparation method of pharmaceutical grade 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 respectively, accurately weigh them, 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 chol...

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...

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Abstract

The invention provides a pharmaceutical grade sodium cholesterol sulfate and a preparation method thereof. In the present invention, by controlling the addition ratio of cholesterol, sulfamic acid and sodium hydroxide, the sodium ion content in the product is within the range of 4.5%-4.9%, ensuring that the final product of the reaction is basically pure sodium cholesteryl sulfate, which hardly contains cholesterol sulfate Ester, to provide qualified raw materials for the safe and effective application of 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

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Application Information

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Patent Type & Authority Patents(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
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