Preparation method of standard digoxin substance

A standard substance and technology of digoxin, which is applied in the field of preparation of digoxin standard substances, can solve the problem of decreased impurity content, long delivery period, impurity digoxigenin and digoxin tetradigoxin saccharide. The problem of limited separation effect, etc., to achieve the effect of improving product purity and simple preparation method

Active Publication Date: 2019-03-19
TIANJIN UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] (1) Preparative chromatographic method: use preparative chromatographic technology to separate and purify digoxin and impurities, and collect fractions that meet the purity requirements, but this method is not suitable for large-scale preparation of digoxin;
[0007] (2) Fractional dissolution method: Utilize the difference in the dissolving ability of solvents to digoxin and impurities, and separate impurities from digoxin products through multiple fractional dissolution processes, but this method is not effective for impurities digoxigenin and digoxigenin. The separation effect of digoxin four digitoxin glycosides is limited, resulting in the purity of digoxin products not meeting the purity requirements of standard substances;
[0008] (3) Liquid-liquid extraction method: the purpose of purifying digoxin is achieved by utilizing the difference in dissolving ability of immiscible solvent systems for digoxin and impurities. However, due to the variety of impurities in digoxin products, the liquid The result of liquid extraction will lead to a decrease in the content of some impurities in the product, and a corresponding increase in the content of some impurities
At present, there is no research institution in China that can provide digoxin reference materials, and importing foreign digoxin reference materials has problems such as high cost, long delivery cycle, and lack of traceability of test results. Therefore, it is urgent to develop high-purity digoxin reference materials. Purification and preparation technology

Method used

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  • Preparation method of standard digoxin substance

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] A preparation method of digoxin standard substance, comprising the following steps:

[0036] (1) Weigh 2g of commercially available digoxin crude product (raw material) and add it to a 250ml round bottom flask, add 150mL of chloroform, install a reflux condenser, use an electric heating mantle to heat and boil to make all the solids dissolve, and then When the temperature of the solution drops to 55°C, add 0.1 g of activated carbon, then reflux at the boiling point for decolorization for 45 minutes, filter off the activated carbon with a heat preservation funnel, and rotate the obtained filter body to obtain 1.9 g of crude digoxin white crystals;

[0037] After detection by liquid chromatography, the content of digoxin was 97.9%, the content of dihydroxydigoxigenin was 1.0%, the content of digitalis was 0.3%, the content of hydroxydigoxigenin was 0.3%, and the content of digoxigenin was 0.3%. Other impurities are unknown components.

[0038](2) The 1.9g digoxin crystal...

Embodiment 2-6

[0055] The starting materials were 2 g of commercially available crude digoxin, and the preparation steps were the same as in Example 1, and the specific parameters were shown in Table 1.

[0056] Table 1

[0057]

[0058]

[0059]

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PUM

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Abstract

The invention discloses a preparation method of a standard digoxin substance. The preparation method includes: subjecting crude digoxin to activated carbon fading, liquid-liquid extraction and solventcrystallization. The preparation method of the standard digoxin substance has the advantages that micro impurities having influence on color of a digoxin product can be removed, the digoxin product can be whiter in color; digoxin can be effectively separated from impurities including digitalis, hydroxy digitoxin and the like, purity of the digoxin product can be improved effectively; impurities structurally similar to dihydroxy digitoxin can be separated out from the digoxin product, and the purity of the digoxin product can be over 99.5%; an obtained crystal digoxin product with content higher than 99.5% (measured by an HPLC-high performance liquid chromatography method) can be applied to crude digoxin drug monitoring and blood concentration monitoring and is simple in preparation method.

Description

technical field [0001] The invention relates to a preparation method of a standard substance, in particular to a preparation method of a digoxin standard substance. Background technique [0002] Digoxin, also known as digoxigenin, is a cardiac glycoside drug used to treat various acute and chronic cardiac insufficiency, as well as supraventricular tachycardia, atrial fibrillation and flutter. Its chemical name is: 3β-O-2,O-dideoxy-β-D-nucleo-hexapyranosyl-(1→4)-O-2,6-dideoxy-β-D-nucleo-hexapyranosyl- (1→4)-2,6-dideoxy-β-D-nucleo-hexapyranosyloxy-12β,14β-dihydroxy-5β-centro-20(22)enolactone. The molecular formula is: C 41 h 64 o 14 ; The molecular weight is 780.94. Pure digoxin is white crystal or crystalline powder with a melting point of 248°C (decomposition). Digoxin is insoluble in water, ethanol, ether, acetone, slightly soluble in chloroform, diethyl alcohol, soluble in pyridine, chloroform-ethanol, dichloro Organic solvents such as methane-methanol. Its structur...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/04
CPCG01N30/04G01N2030/042
Inventor 李国兵全灿刘兰云张旭斌蔡旺锋
Owner TIANJIN UNIV
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