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首页> 外文会议>NMR spectroscopy of polymers: Innovative strategies for complex macromolecules >Characterization of Microbial Poly(ε-L-lysine) and Its Derivatives by Solid-State NMR
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Characterization of Microbial Poly(ε-L-lysine) and Its Derivatives by Solid-State NMR

机译：固态NMR表征微生物聚（ε-L-赖氨酸）及其衍生物

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The molecular structure and conformation of microbial poly(ε-L-lysine) (ε-PL) and its derivatives in aqueous solution and in the solid-state have been studied with liquid-state ~1H and ~(13)C NMR, and solid-state ~(13)C and ~(15)N NMR, together with FT-IR, FT-Raman, and circular dichroism (CD) techniques. CD and vibrational spectroscopic results indicate that ε-PL assumes a p-sheet conformation in aqueous solution and in the solid state. Solid-state ~(13)C NMR spectra of the crystalline and the amorphous components were obtained separately by utilizing difference in ~(13)C spin-lattice relaxation times between the two components. The degree of crystallinity was estimated to be 63%. Conformation models of the crystalline component were also discussed. Chemically modified derivatives of ε-PL, ε-PL/MO and ε-PL/DC were prepared through reactions with methyl orange (MO) and dabsyl chloride (DC), respectively. Characterization of these derivatives was carried out by solid-state ~(13)C and ~(15)N NMR. In ε-PL/MO side chain a-amino groups of ε-PL are involved in ionic bonds with methyl orange (MO) to form poly-ionic complexes, (ε-PL)-NH_3~+ SO_3 -(MO). In contrast, the a-amino groups react with DC in c-PL/DC to form covalent sulfonamide bonds, (ε-PL)-NH-SO_2-(DC). The ~(15)N NMR data are consistent with these structures.
机译：用液相〜1H和〜（13）C NMR研究了微生物聚（ε-L-赖氨酸）（ε-PL）及其衍生物在水溶液和固态中的分子结构和构象，固态〜（13）C和〜（15）N NMR，以及FT-IR，FT-Raman和圆二色性（CD）技术。 CD和振动光谱结果表明，ε-PL在水溶液和固态下呈p-片状构象。利用两种组分之间〜（13）C自旋晶格弛豫时间的差异，分别获得了晶体和非晶态组分的固态〜（13）C NMR光谱。结晶度估计为63％。还讨论了结晶成分的构象模型。分别通过与甲基橙（MO）和dabsyl chloride（DC）反应制备了ε-PL，ε-PL/ MO和ε-PL/ DC的化学改性衍生物。这些衍生物的表征通过固态〜（13）C和〜（15）N NMR进行。在ε-PL/ MO的侧链中，ε-PL的α-氨基与甲基橙（MO）形成离子键，形成聚离子配合物（ε-PL）-NH_3〜+ SO_3-（MO）。相反，α-氨基与c-PL / DC中的DC反应形成共价磺酰胺键（ε-PL）-NH-SO_2-（DC）。 〜（15）N NMR数据与这些结构一致。

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