Selective separation and purification method of bufadienolide compounds

A technology for the separation and purification of bufadienolactones, which is applied in the fields of steroids and organic chemistry, can solve the problems of time-consuming separation and purification methods, complex structures, large quantities, etc., and achieve the effect of efficient preparation

Inactive Publication Date: 2015-07-15
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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Problems solved by technology

Due to the large number and complex structure of bufadienolides, conventional separation and purification methods are time-consuming and inefficient (L.Krenn, B.Kopp, Bufadienolides from animal and plant sources, P

Method used

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  • Selective separation and purification method of bufadienolide compounds

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Embodiment

[0023] 1) The 95% (volume concentration) ethanol extract of toad skin was separated by preparative RPLC. Chromatographic conditions: chromatographic column is a carbon-octave column (C18TDE column); water (A) and methanol (B) mobile phase system; elution The gradient is 0-7min, volume concentration 25%→40%B; 7-60min, volume concentration 40%→65%B; 60-65min, volume concentration 65%→100%B; 65-75min, 100%B; flow rate It is 330mL / min; in the separation process, it is detected by an ultraviolet detector, and the detection wavelength is 300nm; it is dissolved in methanol-water with a volume concentration of 65%, and the concentration of the sample solution is 440mg / mL; the injection volume is 40mL; according to the retention of each chromatographic peak Each fraction was collected separately at different times, and a total of 22 components were collected, and each component was concentrated to dryness for later use; for the component F13 rich in bufadienolactone (the volume of metha...

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Abstract

The invention provides a selective separation and purification method of bufadienolide compounds. Positively charged XCharge C18 column is used for developing a novel high-performance liquid chromatographic separation method with high selectivity based on that at a low pH value, ionic properties of amino acid modified bufadienolides are different from ionic properties of bufadienolides which are not modified with amino acid. According to the selective separation and purification method, a mobile phase contains no buffer salt, so that it is convenient for sample preparation postprocessing; a toad skin 98% ethanol extract product is subjected to reversion phase chromatography preparation separation so as to obtain a fraction; and two kinds of compounds, including eight compounds, are obtained via reversed phase chromatography preparation. The selective separation and purification method is capable of realizing high efficiency preparation of amino acid modified bufadienolides and bufadienolides which are not modified with amino acid; and the selective separation and purification method is capable of solving a problem of trailing in separation process of amino acid modified bufadienolides; and excellent peaks are observed, and excellent separation effect is achieved. The selective separation and purification method is used for high efficiency systematic separation of bufadienolides, and is capable of providing substance base and technical support for anticancer active research of bufadienolides and signal-component new drug development.

Description

technical field [0001] The present invention relates to the separation and purification of bufadiene lactones, in particular to a reverse phase chromatography using a positively charged XCharge C18 column to separate and purify bufadienes with high selectivity under low pH conditions. new method. The method showed better separation effect on amino acid modified bufadienolactone compounds and non-amino acid modified bufadienolactone compounds. Background technique [0002] Bufadienolides are a class of C24 steroids, and there is a β six-membered unsaturated lactone ring at the C17 position of the steroid core. This type of compound is also often called bufadienolides. Liselotte.Krenn, Pieter S.Steyn and Gao Huimin respectively reviewed the biological activities of bufadiene lactones. These activities mainly include local anesthesia, cardiotonic, pressor, Na + / K + -ATPase inhibitory activity and anti-tumor effects (L.Krenn, B.Kopp, Bufadienolides from animal and plant sou...

Claims

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Application Information

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IPC IPC(8): C07J41/00C07J71/00C07J19/00
CPCC07J19/00C07J41/0055C07J71/0021
Inventor 李晓龙梁鑫淼刘艳芳张云张秀莉薛兴亚
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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