Jaeger E, Thamm P, Schmidt I, Knof S, Moroder L, Wünsch E
Hoppe Seylers Z Physiol Chem. 1978 Feb;359(2):155-64.
The preparation of the pure 11-leucine analogue of human minigastrin I, a linear tridecapeptidaemide with full "gastrin activity", from the crude synthetic material obtained after deblocking of the overall protected tridecapeptide amide derivative by means of trifluoroacetic acid, is achieved by ion-exchange chromatography on DEAE-Sephadex A-25 and subsequent partition chromatography on Sephadex G-25. The isolation of a synthetic side-product and its identification as human [10-(Nin-tert-butyl-tryptophan),11-leucine]minigastrin I by means of spectroscopic (UV, fluorescence, 1H-NMR, MS), enzymatic and chromatographic methods is described. The pure tridecapeptide amides human [Leu11]minigastrin I and human [Trp(1'-But)10,Leu11]minigastrin I are isolated in overall yields of 37.4% and 4.6%, respectively (mol-% with regard to the overall protected tridecapeptide amide derivative).
从通过三氟乙酸脱保护的全保护十三肽酰胺衍生物得到的粗合成材料中制备具有完全“胃泌素活性”的人胃泌素 I 的纯 11-亮氨酸类似物(一种线性十三肽酰胺),是通过在 DEAE-葡聚糖 A-25 上进行离子交换色谱,随后在葡聚糖 G-25 上进行分配色谱来实现的。描述了通过光谱法(紫外、荧光、1H-核磁共振、质谱)、酶法和色谱法分离一种合成副产物并将其鉴定为人 [10-(N-叔丁基-色氨酸),11-亮氨酸]胃泌素 I 的过程。纯十三肽酰胺人 [Leu11]胃泌素 I 和人 [Trp(1'-But)10,Leu11]胃泌素 I 的总产率分别为 37.4% 和 4.6%(相对于全保护十三肽酰胺衍生物的摩尔百分比)。