13c Cp Mas Nmr Pectin Chitosan
Table 1 shows the chemical shifts of chitosan protons in d 2 o dcl at 70 c.
13c cp mas nmr pectin chitosan. Cp mas 13 c nmr heux et al. The conditions of acid extraction of tobacco samples and. 100 mg is dissolved in a known volume of aqueous hcl 0 010 mol l 1 and the solution is then ti trated with 0 1 mol l 1 naoh while the ph of the solution is measured at constant ionic strength 0 1 mol l 1 nacl. 94 biotechnology of biopolymers 3 2 potentiometric titration chitosan ca.
The graph with the variation of ph versus the. Cp mas 13 c nmr spectra of sclerotized insect cuticle and of chitin. Nishioka sulfated derivatives of chitosan and their characterization with respect to biological activity chitin in nature and technology 10 1007 978 1 4613 2167 5 461 468 1986. Chitin and chitosan were analyzed by x ray 13c cp mas nmr 13c ft chitin samples in a alpha form structure were isolated from beetle larva cuticle and silkworm bombyx mori pupa exuvia by treatment with 1 n hcl and 1 n naoh.
One could not expect to detect the da less than 10 in 15 n nmr and 13 c nmr techniques due to line broadening effects their high coefficient of variation 10. The solvent hod proton resonates at 4 67 ppm. New chemical hydrogels potentially suitable for biomedical applications have been synthesized and characterized by 13c cp mas nmr spectroscopy. A double air bearing probe and a zirconium oxide rotor were used.
Cp mas 13 c nmr and cp mas 15 n nmr are appropriate methods for insoluble chitin chitosan samples even the samples are associated with impurities and humidity ottøy et al 1996. Acquisition was performed with a standard cp pulse sequence using a 3 5 μs proton 90 pulse a 800 μs contact pulse and a 2 5 s. A new method utilizing 13c cp mas nmr spectra was developed for the simultaneous quantitative and structure analysis of pectin in tobacco. In this study the relaxation delay and contact time leading to quantitative chitin and deacetylated chitin 13 c cp mas nmr spectra have been determined.
1h and 13c nmr spectra of chitosan allow a good characterization of the starting materials. The polysaccharidic component of these hydrogels is chitosan while the novel cross linking agent is diethyl squarate des. 2 presents the 400 mhz 1 h nmr spectrum of chitosan pcch00005 dda 87 at 70 c. Chitosan was prepared by treating them in 40 naoh containing nabh 4.
5 4 solid state 13 c nuclear magnetic resonance. The mas rate was in the 4 5 khz range. The assignment of chitosan peaks have already been reported in the literature. The structures of acetylated and deacetylated monomers of chitosan are presented in fig.
The degree of acetylation of chitin and deacetylated chitin samples determined from the 13 c cp mas nmr spectra acquired with the optimised relaxation delay 5 s and contact time 1 ms is 0 68 and 0 16 respectively.