초록
1. 오징어 연골과 chitin, chitosan의 질소함량은 각각 $12.1\%,\;8.1\%,\;5.8\%$이며 회분함량은 각각 $0.8\%,\;9.4\%,\;0.2\%$로 나타났으며 오징어 연골로부터 최종적으로 만들어지는 chitosan의 수율은 $25\pm3\%$ 이었다. 2. 재탈아세틸화 하여 얻어진 chitosan의 탈아세틸화도는 $92\%$로 이는 NMR을 분석한 결과 chitin의 NMR 분석에서 보여지는 $CH_3$와 C=O기의 peak가 거의 나타나지 않았으며 또한 $C_3, C_5$가 $\beta-chitin$에서는 역평행 구조로서 2개의 signal로 나타나는데 본 실험에서는 $\beta-chitin$에서 보여지는 단일의 signal로 나타났다. 3. Chitosan을 0.2M AcOH-0.1 M AcONa 용액에 녹여 $30^{\circ}C$에서 점도를 측정한 결과 Mark-Houwink 식과 Rinaudo의 상수로부터 $[\eta]=1.424\times10^{-5}M^{0.96}$이었으며 분자량은 $1.15\times10^6$이었다. 4. I.R spectrum을 측정한 결과 chitin은 $1,653 cm^{-1}$에서amide I bend가 $1,558 cm^{-1}$에서 amide II bend가 나타났으며 chitosan은 $1,601 cm^{-1}$에서 1개의 넓은 bend가 생겼다. N-acetylchitosan의 경우 chitin과 마찬가지로 $1,655cm^{-1}$에서 amide I bend가 $1,560 cm^{-1}$에서 amide II bend가 나타났다. 5. 아세틸 함량은 N-acetylchitosan 분말이 $5.9\%$, acetylchitosan bead가 $63.2\%$ , N-ACF-1이 $56\%$ , N-ACF-2가 $58.7\%$ 이었다. 6. Chitin, chitosan 및 N-acetylchitosan을 formic acid에 용해하여 실온에서 시간에 따른 고유점도 변화를 관찰한 결과 chitosan이 chitin, N-acetylchitosan 보다 비교적 점도가 높았지만 3개 모두 시간이 지남에 따라 점도가 현저히 저하되어 25일째에는 chitosan이 14.39 dL/g, chitin이 1.31 dL/g, N-acetylchitosan이 1.06 dL/g이었다.
In order to utilize the processing wastes of squid, chitosan was prepared by intermittent deacetylation treaoent of $\beta-chitin$ contained richly in the pen of squid. Acetylchitosan also was synthesized from squid pen chitosan with anhydrous acetic acid and their characteristics were investigated. The amounts of nitrogen and ash of squid pen chitosan were $5.80.2\% and 0.2\pm0.03\%$ respectively, the yield of squid pen chitosan was $25\pm3\%$, the degree of deacetylation was $92\%$, and the molecular weight was $1.15\times10^6$, Acetyl contents of N-acetylchitosan powder, acetylchitosan bead, N-ACF-1 (N-acetylchitosan film-1) and N-ACF-2 (N-acetylchitosan film-2) were $55.9\%, 63.2\%, 56\% and 58.7\%$ respectively. Two major peaks, amide I ($1,653 cm^{-1}$) and II ($1,558 cm^{-1}$) bent, on FT-IR spectra of the N-acetylchitosan from squid pen were almost similar to these of $\beta-chitin$, While there was a broad single peak at $1,601 cm^{-1}$assigned to be an amide I bend in squid pen chitosan. The CP/MAS NMR spectra of $\beta-chitin$, squid pen chitosan and N-acetylchitosan from squid pen showed a relative broad and single peak at 74 ppm assigned to fifth carbon (C-5) and third carbon (C-3). In case of $\beta-chitin$ and N-acetylchitosan from squid pen, single peak at 74 ppm was showed as the same of $\beta-chitin$ type.
(Department of Food Science and Technology, Pukyong National University)