分溜法による天然アミノ酸混合物の分離の研究
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The concentrated hydrolysates of gelatin and casein were esterified with ethanol in the presence of benzene in a flask equipped with a dehydration column. After the neutralization of the product with gaseous ammonia, the free esters of amino acids were fractionally distilled under the pressure of 20〜5 mm Hg through a column of 20〜30 plates. Each fraction of distillate was hydrolysed to the acid by boiling it in water and analysed by paper chromatography. In this manner the following results were obtained. 1) The esters of glycine and alanine were distilled together in the first fraction. 2) or-Amino butyric acid was recognized in the next fraction. 3) The ester of valine was distilled in a fraction boiling at 69℃/9mmHg and was found satisfactorily pure from the result of paper chromatogram and the value of specific rotation. 4) The esters of proline, leucine and isoleucine were distilled together. The leucines fraction was separated in crystals free from proline after hydrolysis. Many attempts, however, to obtain pure proline free from leucines were unsuccessful. For that purpose, only a method of counter-current extraction by w-butanol-water solvent system was found to be satisfactory. By this method proline having [α]_D value of -81.6 was obtained. 5) Glycine-alanine mixture and leucine-isoleucine mixture obtained still retained optical activity, and hence almost no racemization was found to occur during the distillation procedure. 6) By the dislillation method, the yields of the esters from protein hydrolysats were considerably low and the esters of phenylalanine, methionine, aspartic and glutamic acids remained undistilled in the still pot. Although the method was thus found unsuitable for the component analysis, it was suitable for the preparative separation of glycine-alanine mixture, α-amino butyric acid, valine, proline and leucines. Further methods of more efficient dislillation of the esters and preparation of pure amino acids in better yield were discussed.
- 宇宙航空研究開発機構の論文
- 1957-03-15
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