Dutta Joydeep
Department of Chemistry, Amity School of Applied Sciences, Amity University Haryana, Gurgaon 122413, Haryana, India.
Heliyon. 2022 Jul 11;8(7):e09924. doi: 10.1016/j.heliyon.2022.e09924. eCollection 2022 Jul.
Several spectroscopic techniques such as nuclear magnetic resonance (NMR), UV-visible, Fourier transform infrared (FT-IR), etc. have been already used for the determination of degree of deacetylation (DD) of chitosan. These techniques involve the interpretation of spectral data apart from sample preparation for obtaining DD of chitosan. In addition, inaccurate interpretation of data sometimes misleads researchers to get an exact value of DD of chitosan. Among them, NMR is an excellent technique for the estimation of DD of chitosan but expensive and not found easily in every research laboratory. On the other hand, titrimetric methods have been employed by many researchers for determining the DD of chitosan but these existing methods involve many complex calculations, which do not always give accurate results. Moreover, few of the acid-base titration methods are little complicated for execution. Therefore, in this present study, we adopted a very handy and simple acid-base titration method with a new approach and proposed a new equation facilitating the ease of calculation that is not reported elsewhere for the determination of DD value by observing the net volume of NaOH consumed for the complete neutralization of protonated amino groups (-NH ) of chitosan describing the novelty of the work. All the DD values (77.04 ± 1.36; 81.71 ± 1.73; 91.68 ± 1.42 for CS1, CS2, and CS3 respectively) obtained for various chitosan samples were in good agreement with the reported DD values (>75%, >80%, and >85% for CS1, CS2, and CS3 respectively) mentioned in the specifications of chitosan samples supplied by the manufacturer. Finally, the experimental DD values were further validated with the DD values (77.39%, 81.64%, and 90.5% for CS1, CS2, and CS3 respectively) obtained from the interpretation of C-NMR spectral data and all the experimental DD values were consistent with the DD values as calculated based on NMR spectra.
几种光谱技术,如核磁共振(NMR)、紫外可见光谱、傅里叶变换红外光谱(FT-IR)等,已被用于测定壳聚糖的脱乙酰度(DD)。这些技术除了进行用于获取壳聚糖DD值的样品制备外,还涉及光谱数据的解读。此外,数据的不准确解读有时会误导研究人员获得壳聚糖DD的准确值。其中,NMR是估算壳聚糖DD的优秀技术,但价格昂贵,并非每个研究实验室都能轻易获得。另一方面,许多研究人员采用滴定法测定壳聚糖的DD,但这些现有方法涉及许多复杂计算,并不总能给出准确结果。此外,一些酸碱滴定法在操作上有点复杂。因此,在本研究中,我们采用了一种非常简便的酸碱滴定法,并提出了一种新的方法和新的方程式,通过观察用于完全中和壳聚糖质子化氨基(-NH)所消耗的NaOH净体积来简化计算,从而测定DD值,这在其他地方尚未见报道,体现了这项工作的新颖性。所获得的各种壳聚糖样品的所有DD值(CS1、CS2和CS3分别为77.04±1.36;81.71±1.73;91.68±1.42)与制造商提供的壳聚糖样品规格中提到的报告DD值(CS1、CS2和CS3分别>75%、>80%和>85%)高度一致。最后,通过对C-NMR光谱数据解读获得的DD值(CS1、CS2和CS3分别为77.39%、81.64%和90.5%)进一步验证了实验DD值,所有实验DD值与基于NMR光谱计算的DD值一致。