Optimization of carboxymethyl chitosan synthesis using response surface methodology and desirability function

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• 作者：Andrea L. Bukzem^a ; ^{andrea_bukzem@hotmail.com" class="auth_mail" title="E-mail the corresponding author} ; Roberta Signini^a ; ^{roberta.signini@ueg.br" class="auth_mail" title="E-mail the corresponding author} ; Danilo M. dos Santos^a ; ^{danilomartins_1@hotmail.com" class="auth_mail" title="E-mail the corresponding author} ; Luciano M. Liã ; o^b ; ^{luciano@quimica.ufg.br" class="auth_mail" title="E-mail the corresponding author} ; Diego Palmiro R. Ascheri^a ; ^{ascheridpr@gmail.com" class="auth_mail" title="E-mail the corresponding author}
• 关键词：Carboxymethylation of chitosan ; Response surface methodology ; Desirability function
• 刊名：International Journal of Biological Macromolecules
• 出版年：2016
• 出版时间：April 2016
• 年：2016
• 卷：85
• 期：Complete
• 页码：615-624
• 全文大小：2153 K

文摘

In this paper, chitosan was reacted with monochloroacetic acid under alkaline conditions to prepare carboxymethyl chitosan. A 2³ full-factorial central composite design was applied to evaluate the effect of molar ratio sodium hydroxide (NaOH)/Chitosan (Ch), time and molar ratio monochloroacetic acid (MCA)/Chitosan (Ch) on the reaction yield and on the characteristics of carboxymethyl chitosan such as average degree of substitution (class="mathmlsrc">title="View the MathML source" class="mathImg" data-mathURL="/science?_ob=MathURL&_method=retrieve&_eid=1-s2.0-S0141813016300174&_mathId=si2.gif&_user=111111111&_pii=S0141813016300174&_rdoc=1&_issn=01418130&md5=944b79d59ff3d0c7d8592b46de9dda7b">class="imgLazyJSB inlineImage" height="14" width="20" alt="View the MathML source" style="margin-top: -5px; vertical-align: middle" title="View the MathML source" src="/sd/grey_pxl.gif" data-inlimgeid="1-s2.0-S0141813016300174-si2.gif">class="mathContainer hidden">class="mathCode">$\overline{DS}$) and solubility. An optimization strategy based on response surface methodology was used together with the desirability function approach to optimize this process. The occurrence of carboxymethylation was evidenced by FTIR and ¹H NMR spectroscopy. The optimum conditions for carboxymethylation process were found to be 12.4, 10.6 h and 5 for molar ratio sodium hydroxide (NaOH)/Chitosan (Ch), time and molar ratio monochloroacetic acid (MCA)/Chitosan (Ch), respectively. Under these optimal conditions, it was possible to obtain carboxymethyl chitosan with class="mathmlsrc">title="View the MathML source" class="mathImg" data-mathURL="/science?_ob=MathURL&_method=retrieve&_eid=1-s2.0-S0141813016300174&_mathId=si1.gif&_user=111111111&_pii=S0141813016300174&_rdoc=1&_issn=01418130&md5=f00acff5815602af6a88fbe7b4e9ff33">class="imgLazyJSB inlineImage" height="14" width="21" alt="View the MathML source" style="margin-top: -5px; vertical-align: middle" title="View the MathML source" src="/sd/grey_pxl.gif" data-inlimgeid="1-s2.0-S0141813016300174-si1.gif">class="mathContainer hidden">class="mathCode">${\displaystyle \overline{DS}}$ of 1.86 and solubility of 99.6%. X-ray diffraction and thermogravimetry analysis showed that crystallinity and thermal stability of derivatives was lower than chitosan and decreased with increase of class="mathmlsrc">title="View the MathML source" class="mathImg" data-mathURL="/science?_ob=MathURL&_method=retrieve&_eid=1-s2.0-S0141813016300174&_mathId=si1.gif&_user=111111111&_pii=S0141813016300174&_rdoc=1&_issn=01418130&md5=f00acff5815602af6a88fbe7b4e9ff33">class="imgLazyJSB inlineImage" height="14" width="21" alt="View the MathML source" style="margin-top: -5px; vertical-align: middle" title="View the MathML source" src="/sd/grey_pxl.gif" data-inlimgeid="1-s2.0-S0141813016300174-si1.gif">class="mathContainer hidden">class="mathCode">${\displaystyle \overline{DS}}$.