Gross H J, Bünsch A, Paulson J C, Brossmer R
Institut für Biochemie II der Universität Heidelberg, Federal Republic of Germany.
Eur J Biochem. 1987 Nov 2;168(3):595-602. doi: 10.1111/j.1432-1033.1987.tb13458.x.
In this report several NeuAc analogues differently modified at position C-9 were tested as substrates for CMP sialic acid synthase from bovine brain: the hydroxy group at C-9 was replaced by an amino, acetamido, benzamido, hexanoylamido and azido group. The synthase was partially purified by chromatography on CDP-hexanolamine--Sepharose. CMP-glycosides synthesized were measured by analytical HPLC at 275 nm. Each NeuAc analogue was activated to the respective CMP-glycoside: Km-values varied from 0.8 mM to 4.6 mM, the Km for NeuAc was 1.4 mM. Thus affinity of the enzyme was influenced only moderately by chemical modification at C-9. CMP-glycosides were synthesized on a preparative scale with good yield and characterized by analytical HPLC. In addition, 500-MHz 1H-NMR data of CMP-9-amino-NeuAc and CMP-9-acetamido-NeuAc were obtained. Each CMP-activated NeuAc analogue was a suitable donor substrate for Gal beta 1-4GlcNAc alpha 2,6-sialyltransferase from rat liver. Transfer was determined by the thiobarbituric acid method and by analytical HPLC at 200 nm. The results demonstrate that synthetic, not naturally occurring, non-labelled NeuAc analogues can be incorporated into glycoprotein with high yield.
在本报告中,测试了几种在C-9位有不同修饰的NeuAc类似物作为牛脑CMP唾液酸合成酶的底物:C-9位的羟基被氨基、乙酰氨基、苯甲酰胺基、己酰氨基和叠氮基取代。通过在CDP-己醇胺-琼脂糖上进行色谱法对合成酶进行了部分纯化。通过在275nm处的分析型高效液相色谱法测定合成的CMP-糖苷。每种NeuAc类似物都被激活生成相应的CMP-糖苷:Km值在0.8mM至4.6mM之间变化,NeuAc的Km值为1.4mM。因此,C-9位的化学修饰对该酶的亲和力仅有适度影响。以良好的产率制备规模合成了CMP-糖苷,并通过分析型高效液相色谱法进行了表征。此外,还获得了CMP-9-氨基-NeuAc和CMP-9-乙酰氨基-NeuAc的500MHz 1H-NMR数据。每种CMP激活的NeuAc类似物都是大鼠肝脏Galβ1-4GlcNAcα2,6-唾液酸转移酶的合适供体底物。通过硫代巴比妥酸法和在200nm处的分析型高效液相色谱法测定转移情况。结果表明,合成的而非天然存在的未标记NeuAc类似物可以高产率地掺入糖蛋白中。