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Preparation and detection method of high-purity high-melting-point sodium pantothenate

A detection method, the technology of sodium pantothenate, which is applied in the field of preparation and detection of high-purity and high-melting-point sodium pantothenate, can solve the problems of residual raw materials, low melting point, unstable purity, etc.

Active Publication Date: 2020-04-28
HEFEI HUAFANG PHARMA SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The main disadvantage of this method is still that the operation process is cumbersome, and the starting material remains
[0008] After investigation, it is found that sodium pantothenate currently available in the market generally has problems such as hygroscopicity, unstable purity, unstable crystal form, and low melting point, which cannot meet the quality standards for raw materials of sodium pantothenate

Method used

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  • Preparation and detection method of high-purity high-melting-point sodium pantothenate
  • Preparation and detection method of high-purity high-melting-point sodium pantothenate
  • Preparation and detection method of high-purity high-melting-point sodium pantothenate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] Take calcium pantothenate (50.0 g, 104.92 mmol) and dissolve it in 100 mL of purified water. Sodium carbonate (12.34g, 116.41mmol) was dissolved in 40mL of purified water. At 25°C, add the sodium carbonate aqueous solution dropwise to the calcium pantothenate aqueous solution, and after 20 minutes, the dropwise addition is completed, and then stir at the same temperature for 30 minutes. Filter and wash the filter cake with 10 mL of purified water. The filtrate was collected and tested with a pH meter. The pH value of the filtrate was between 9.0 and 10.0, and concentrated under reduced pressure at 75° C. (vacuum degree 0.090 MPa) until the moisture content of the oil was about 18%.

[0043] Add 100mL absolute ethanol to the oily substance and dissolve at 60°C. Then add 0.50 g (1%, m / m) of sodium pantothenate seed crystals, stir and disperse evenly, and stir and crystallize at 25° C. for 2 h. After more white particles were precipitated, 90 mL of acetonitrile was adde...

Embodiment 2

[0048] Take calcium pantothenate (50.20g, 105.34mmol) and dissolve it in 100mL of purified water. Sodium carbonate (12.34g, 116.41mmol) was dissolved in 40mL of purified water. Add the sodium carbonate aqueous solution dropwise to the calcium pantothenate aqueous solution at 28°C. After 30 minutes, the dropwise addition is completed, and then stir at the same temperature for 40 minutes. Filter and wash the filter cake with 10 mL of purified water. The filtrate was collected and tested with a pH meter. The pH value of the filtrate was between 9.0 and 10.0, and concentrated under reduced pressure at 75° C. (vacuum degree 0.090 MPa) until the moisture content of the oil was about 16%.

[0049] Add 100mL absolute ethanol to the oily substance and dissolve at 60°C. Add 0.51 g (1%, m / m) of sodium pantothenate seed crystals and stir to disperse evenly. Stir and crystallize at 26° C. for 3 h. After more white particles were precipitated, 90 mL of methyl ethyl ketone was added dropw...

Embodiment 3

[0054] Take calcium pantothenate (49.80g, 104.51mmol) and dissolve it in 100mL of purified water. Sodium carbonate (12.34g, 116.41mmol) was dissolved in 40mL of purified water. At 34°C, add the sodium carbonate aqueous solution dropwise to the calcium pantothenate aqueous solution, and the dropwise addition is completed in 15 minutes, and then stir at the same temperature for 20 minutes. Filter and wash the filter cake with 10 mL of purified water. The filtrate was collected and tested with a pH meter. The pH value of the filtrate was between 9.0 and 10.0, and concentrated under reduced pressure at 75° C. (vacuum degree 0.090 MPa) until the moisture content of the oil was about 19%.

[0055] Add 200mL of absolute ethanol to the oil and dissolve at 60°C. Then add 0.50 g (1%, m / m) of sodium pantothenate seed crystals, stir and disperse evenly, stir and crystallize at 18° C. for 3 h. After more white particles were precipitated, 90 mL of methyl ethyl ketone was added dropwise,...

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Abstract

The invention discloses a preparation and detection method of high-purity high-melting-point sodium pantothenate, and relates to the technical field of organic synthesis. The preparation and detectionmethod comprises the steps that calcium pantothenate and anhydrous sodium carbonate are used for preparing sodium pantothenate, and then the impurity beta-aminopropionic acid in the sodium pantothenate is detected; according to the invention, a method for rapidly detecting amino acids is used, and strong chromophoric group fluorenylmethoxycarbonyl or benzyloxycarbonyl is introduced, so that the content of the sodium pantothenate hydrolysis impurity beta-aminopropionic acid can be rapidly detected through a liquid phase; meanwhile, the high-purity and high-melting-point sodium pantothenate isprepared by controlling the concentration temperature, the water consumption and the pH value of the filtrate, so that the sodium pantothenate reaches the medicinal level.

Description

Technical field: [0001] The invention relates to the technical field of organic synthesis, in particular to a preparation and detection method of high-purity and high-melting-point sodium pantothenate. Background technique: [0002] Pantothenic acid is a kind of vitamin B group, common DL-configuration, only D-configuration pantothenic acid has biological activity. D-pantothenic acid is an indispensable substance when fat and sugar are converted into energy, and it can maintain the function of the adrenal gland and the development of the central system of the human body. The calcium and sodium salts of pantothenic acid are commonly used clinically. Calcium pantothenate raw materials and tablets are recorded in the Chinese Pharmacopoeia 2000 edition. Since pantothenic acid often needs to be used in combination with other B vitamins such as riboflavin sodium phosphate or other phosphate drugs, calcium pantothenic acid will reduce the potency due to the formation of calcium p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C231/12C07C231/24C07C235/08G01N30/02G01N30/06G01N30/14G01N30/74
CPCC07C231/12C07C231/24G01N30/02G01N30/06G01N30/14G01N30/74C07B2200/07G01N2030/067G01N2030/146C07C235/08
Inventor 杨士伟夏伦洋何勇高永好任何于艳英方宗华
Owner HEFEI HUAFANG PHARMA SCI & TECH
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