Structural investigation of microbial poly(ε-L-lysine) derivatives with azo dyes by solid-state 13C and 15N NMR
Structural investigation of microbial poly(ε-L-lysine) derivatives with azo dyes by solid-state 13C and 15N NMR
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DOI：
10.1007/s00289-004-0330-9
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发表时间：
2005-02-01
期刊：
影响因子：
3.2
通讯作者：
Hanai, K
中科院分区：
文献类型：
--
作者：
Maeda, S;Mori, T;Hanai, K
测定了微生物聚赖氨酸偶氮衍生物的固态高分辨C-13和N-15核磁共振谱。分别与甲基橙子（MO）和丹磺酰氯（DC）反应制备了epsilon-PL、epsilon-PL/MO和epsilon-PL/DC的化学修饰衍生物。ε-PL/MO中ε-PL的侧链α-氨基与甲基橙子形成离子键，形成多离子复合物（ε-PL）-NH 3 + SO 3--（MO）。另一方面，允许epsilon-PL与epsilon-PL/DC中的丹磺酰氯反应以形成共价磺酰胺键，（epsilon-PL）-NH-SO2-（DC）。这些化学改性的epsilon-PL表现出在α-氨基处结合模式的N-15 NMR信号特征。光谱分析表明，epsilon-PL/DC样品中含有少量的MO离子络合物。结果表明，N-15固体NMR是测定ε-PL及其衍生物结构的有效工具。
Solid-state high-resolution C-13 and N-15 NMR spectra of microbial poly(epsilon-lysine) (epsilon-PL) derivatives with azo dyes have been measured. Chemically modified derivatives of epsilon-PL, epsilon-PL/MO and epsilon-PL/DC were prepared through reactions with methyl orange ( MO) and dabsyl chloride ( DC), respectively. Side chain alpha-amino groups of epsilon-PL in epsilon-PL/MO are involved in ionic bonds with methyl orange to form poly-ion complexes, (epsilon-PL)-NH3+SO3--(MO). On the other hand, epsilon-PL is allowed to react with dabsyl chloride in epsilon-PL/DC to form covalent sulfonamide bonds, (epsilon-PL)-NH-SO2-(DC). These chemically modified epsilon-PL's exhibit N-15 NMR signals characteristic of the binding mode at the alpha-amino groups. The spectral analysis reveals that the epsilon-PL/DC sample contains a small amount of ion complexes with MO. It has been shown that N-15 solid-state NMR is a useful tool for structural determination of epsilon-PL and its derivatives.