CH201760A - Process for the preparation of k-strophanthin-B. - Google Patents

Description

  

  Process for the production of k-strophanthin-p- It is known that in the seeds of Strophanthus kombö the crystallized glucosides cymarin (strophanthidin + cymarose) and k-strophantithin-p (strophanthidin, which have been produced in pure form for a long time) rubbed <B> + </B> Cymarose <B> + 1 </B> Mol glucose) there are other cardiac active glucosides,

    which contain several molecules of glucose (cf. the comprehensive paper by W. <B> A. </B> Jacobs, Physiologieal Reviews <B> 13, </B> <B> S. </B> 22 [1933]) .



  It has now been found that k-strophanthin-p can be produced by allowing α-glucosidase to act on k-strophanthin-p. The k-strophanthoside consists of strophanthidin, cymarose and 2 moles of glucose and can be obtained in pure form, for example, according to the process described in patent specification no. 199908 </B>.

   To carry out the present process, one can start from the pure, crystallized k-sti-ophanthoside or use crude glucoside mixtures, such as those produced by extraction of Strophanthus komb6 Sameii. When the method according to the invention is carried out, the temperature and pH value of the egg enzyme material used are appropriately adapted.



  The new process enables the k-strophanthin-p to be obtained from Strophanthus komb6 seeds in a yield which is several times that of the previous one. Correspondingly, according to this procedure, the main amount of the cardiac active glucosides present is obtained in the form of k-strophanthin-p, which is to be used in therapy.

      <I>Example<B>1:</B> </I> <B> <I> 1 </I> g </B> pure crystallized k-stropbarithoside (see patent no. <B> 199908 ) </B> is dissolved in <B> 30 </B> cm 'water with <B> 10 </B> cm8 yeast solution and <B> 10 </B> cm3' / 8 molar phosphate buffer from pE < B> = 6.8 </B> and the mixture kept in thermostats at <B> 30 '</B>.

   The yeast solution was obtained by neutral autolysis of common brewer's yeast, <B> 10 </B> cm8 of this corresponds to <B> 1 g </B> dry yeast substance and is capable of a 5% maltose solution in <B> 135 </B> minutes split to 50 '/ o. After <B> 65 </B> hours, the batch is shaken out three times with such amounts of chloroform-alcohol that the ratio of water: chloroform <B> - Al- </B> alcohol <B> = </B> 2 < B>: <B> 2: <B> 1 </B>.

   The chloroform fractions are evaporated to dryness and the residue is rubbed with a little water. Immediately 0.4 g of pure k-strophanthine-p crystallized out. Thus 50% of the glucose-rich glucoside was converted into k-strophanthin-p during this time.



  <I> Example 2: </I> 2 <B> g </B> crude, non-crystallized k-strophanthoside, which, as stated in patent no. <B> 199908 </B>, is obtained by extraction of the defatted Strophantus seeds combined with Ohloroform alcohol or aqueous alcohol and the subsequent separation of the tannins with lead hydroxide and fractionation of the glucosides with chloroform-alcohol-water or alcohol and ether

    are treated with <B> 30 </B> one yeast solution according to example <B> 1 </B> at pH # <B> 6.8 </B> and processed further as indicated there. In this case <B> 1.1 g </B> k-stropharithiii- # can be isolated.



  <I> Example<B>3:</B> </I> <B> 1 kg </B> Strophanthus komb6-Sameii w, earth extracted with chloroform alcohol or aqueous <B> Al </B> alcohol and the evaporated extract is exhaustively treated with ether. After separating the tannins with lead hydroxide, the crude orlucoside mixture is taken up in 2 liters of water and poured with <B> 600 </B> eni3 feed solution from <B> 60 g </B> (dry weight) according to example <B> 1 </ B> treated at pH == <B> 6.8 </B>.

   After 120 hours the cloudy solution is clarified with talc and the filtrate is shaken out after adding saturated sodium chloride solution with chloroform to remove the cymariis and yellow-colored greasy impurities. Half the volume of alcohol is added to the clear, yellow-colored aqueous solution and the k-strophantine-p is extracted by shaking it out with chloroform.

   The treatment with chloroform alcohol is repeated twice more on the aqueous solution, each time so that the ratio of water: chloroform <B>: </B> alcohol == 2: 2 <B>: 1 </B>. The separated chloroform solutions are concentrated in vacuo. The k-strophaiithin-p looks crystallized from the residue after rubbing with a little water. The yield of raw k-strophanthin-A amounts to <B> 1 kg </B> drug to <B> 25 </B> and more grams.

    The k-strophanthin-p can be obtained in pure form by recrystallization from alcohol-water or hot water.

 

Claims (1)

<B> PATENT CLAIM: </B> Process for the production of k-strophanthoside, 8, characterized in that a-glucosidase is allowed to act on k-strophanthoside. SUBSTANTIAL CLAIM: A method according to Pallent claim, characterized in that a yeast solution containing α-glucosidase is used at a pH of 6-7.