糯小麦辛烯基琥珀酸淀粉酯的制备及其特性研究
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摘要
本课题以糯小麦淀粉为原料,对辛烯基琥珀酸淀粉酯的湿法制备工艺进行了研究。同时以糯小麦淀粉为对照,比较研究了该淀粉酯的基本性质,即淀粉糊的性质,包括粘度、透明度、凝沉性、冻融稳定性和乳化性能。并研究了该淀粉酯对速冻饺子皮冻裂率的影响。
首先研究了淀粉乳浓度、pH值、反应时间和反应温度四个因素对该淀粉酯取代度的影响。在单因素试验基础上采用Design-Expert软件作响应面分析,得出湿法制备糯小麦辛烯基琥珀酸淀粉酯最佳工艺条件为:淀粉乳浓度31.3%,pH值8.6,反应时间3h,反应温度30.6℃。在最佳工艺条件下制得的产品取代度为0.0144。
然后研究了该淀粉酯的结构特性。红外光谱图证明原淀粉和辛烯基琥珀酸酐发生了酯化反应,淀粉分子上存在酯羰基。X-射线衍射分析表明淀粉的酯化反应主要发生在分子的无定形区,并未使其晶型发生改变,仍保持为糯小麦原淀粉的A型。DSC分析证明改性之后淀粉颗粒虽然保持原有的晶体结构,但是颗粒有所膨胀,结晶结构的致密程度有所下降,结果使SSOS更易于发生糊化。同步辐射X光束线分析得出,糯小麦辛烯基琥珀酸淀粉酯在反应中主要晶格排列不改变,由于淀粉链的柔性,聚集结构对化学反应具有响应性。
之后又对该淀粉酯的性质进行了研究。研究表明:经过OSA改性之后,辛烯基琥珀酸淀粉酯的峰值粘度、低谷粘度和冷胶粘度均比原淀粉的高。并且随着取代度(DS)的增加,该淀粉酯糊的峰值粘度,低谷粘度和冷胶粘度也不断增加,而峰值时间却在减少;淀粉酯糊的透明度、凝沉性和冻融稳定性也得到很大的提高,并且随着取代度的增加,淀粉酯糊的透明度、凝沉性也随之增强;蔗糖与SSOS相互作用,使淀粉糊的透明度和凝沉性增加,抗老化稳定性增强;NaCl使淀粉糊的透光率降低,凝沉性下降,淀粉糊不稳定,易于老化;糯小麦SSOS随着取代度的提高,乳化能力提高。
最后研究了该淀粉酯对速冻饺子皮冻裂率的影响。糯小麦辛烯基琥珀酸淀粉酯的取代度逐渐增加时,速冻饺子皮的冻裂率随之降低;并且在同一取代度下,添加量增加时,速冻饺子皮的冻裂率也随之降低。
This thesis studied preparation of Octenyl succinic anhydride (OSA) modified starches from raw material waxy wheat starch in aqueous slurry system. Some properties of the OSA starch were also investigated in this thesis, including the viscosity, clarity, retrogradation, freeze-thawing stability of the starch paste, and emulsification property of the OSA starch. Then the effect of the OSA starch on the cracking rate of deep-frozen dumpling peel was investigated in this thesis.
At first, study the effect of different reaction conditions on the degree of substitution (DS) of the OSA starch, such as the concentration of starch slurry, pH range, reaction temperature, reaction time. On the base of single factor analysis result, response surface analysis was done with design expert software and the optimistic condition of synthesizing was obtained. The optimistic condition of synthesizing was that: the concentration of starch slurry 31.3%, pH 8.6, reaction time 3h, reaction temperature 30.6℃. At this condition, the degree of substitution (DS) is 0.0144.
Secondly, research the structure of the OSA starch. FT-IR spectroscopy verified that native starch reacted with OSA and the ester carbonyl is in the OSA starch. X-ray analysis showed that the OSA starch occurred mainly in amorphous molecular areas and still maintained the same crystalline pattern as native starch. DSC analysis revealed that though the OSA starch maintained the same crystalline pattern as native starch, the starch granule swelled at a certain extent and the compact degree of crystalline pattern descended, so SSOS gelatinize more easily. Synchrotron radiation X-ray diffraction analysis showed that the main crystal-lattice tactic of SSOS didn’t change in reaction and this aggregate structure had responsiveness to chemical reaction.
After, investigate the properties of the OSA starch. The results showed that the OSA starch paste had higher peak viscosities, HPV and CPV than native waxy wheat starch. Moreover, the degree of substitution(DS) is increased, the PV, HPV and CPV of OSA starch paste increased, but the peak time decreased; Comparing with native waxy wheat starch, the paste clarity, retrogradation and freeze-thaw stability of OSA starch had enhanced, and more, as the DS was getting higher, the paste clarity, retrogradation and freeze-thaw stability of OSA starch was better; The paste clarity and retrogradation of OSA starch greatly decreased by the presence of sodium chloride, but only increased slightly in the presence of sucrose; Emulsification property of the OSA starch increased with DS increasing.
At last, work over the effect of the OSA starch on the cracking rate of deep-frozen dumpling peel. When the degree of substitution of the OSA starch increased, the cracking rate of deep-frozen dumpling peel decreased. Moreover, the cracking rate of deep-frozen dumpling peel decreased with the addition of the same DS starch increasing.
首先研究了淀粉乳浓度、pH值、反应时间和反应温度四个因素对该淀粉酯取代度的影响。在单因素试验基础上采用Design-Expert软件作响应面分析,得出湿法制备糯小麦辛烯基琥珀酸淀粉酯最佳工艺条件为:淀粉乳浓度31.3%,pH值8.6,反应时间3h,反应温度30.6℃。在最佳工艺条件下制得的产品取代度为0.0144。
然后研究了该淀粉酯的结构特性。红外光谱图证明原淀粉和辛烯基琥珀酸酐发生了酯化反应,淀粉分子上存在酯羰基。X-射线衍射分析表明淀粉的酯化反应主要发生在分子的无定形区,并未使其晶型发生改变,仍保持为糯小麦原淀粉的A型。DSC分析证明改性之后淀粉颗粒虽然保持原有的晶体结构,但是颗粒有所膨胀,结晶结构的致密程度有所下降,结果使SSOS更易于发生糊化。同步辐射X光束线分析得出,糯小麦辛烯基琥珀酸淀粉酯在反应中主要晶格排列不改变,由于淀粉链的柔性,聚集结构对化学反应具有响应性。
之后又对该淀粉酯的性质进行了研究。研究表明:经过OSA改性之后,辛烯基琥珀酸淀粉酯的峰值粘度、低谷粘度和冷胶粘度均比原淀粉的高。并且随着取代度(DS)的增加,该淀粉酯糊的峰值粘度,低谷粘度和冷胶粘度也不断增加,而峰值时间却在减少;淀粉酯糊的透明度、凝沉性和冻融稳定性也得到很大的提高,并且随着取代度的增加,淀粉酯糊的透明度、凝沉性也随之增强;蔗糖与SSOS相互作用,使淀粉糊的透明度和凝沉性增加,抗老化稳定性增强;NaCl使淀粉糊的透光率降低,凝沉性下降,淀粉糊不稳定,易于老化;糯小麦SSOS随着取代度的提高,乳化能力提高。
最后研究了该淀粉酯对速冻饺子皮冻裂率的影响。糯小麦辛烯基琥珀酸淀粉酯的取代度逐渐增加时,速冻饺子皮的冻裂率随之降低;并且在同一取代度下,添加量增加时,速冻饺子皮的冻裂率也随之降低。
This thesis studied preparation of Octenyl succinic anhydride (OSA) modified starches from raw material waxy wheat starch in aqueous slurry system. Some properties of the OSA starch were also investigated in this thesis, including the viscosity, clarity, retrogradation, freeze-thawing stability of the starch paste, and emulsification property of the OSA starch. Then the effect of the OSA starch on the cracking rate of deep-frozen dumpling peel was investigated in this thesis.
At first, study the effect of different reaction conditions on the degree of substitution (DS) of the OSA starch, such as the concentration of starch slurry, pH range, reaction temperature, reaction time. On the base of single factor analysis result, response surface analysis was done with design expert software and the optimistic condition of synthesizing was obtained. The optimistic condition of synthesizing was that: the concentration of starch slurry 31.3%, pH 8.6, reaction time 3h, reaction temperature 30.6℃. At this condition, the degree of substitution (DS) is 0.0144.
Secondly, research the structure of the OSA starch. FT-IR spectroscopy verified that native starch reacted with OSA and the ester carbonyl is in the OSA starch. X-ray analysis showed that the OSA starch occurred mainly in amorphous molecular areas and still maintained the same crystalline pattern as native starch. DSC analysis revealed that though the OSA starch maintained the same crystalline pattern as native starch, the starch granule swelled at a certain extent and the compact degree of crystalline pattern descended, so SSOS gelatinize more easily. Synchrotron radiation X-ray diffraction analysis showed that the main crystal-lattice tactic of SSOS didn’t change in reaction and this aggregate structure had responsiveness to chemical reaction.
After, investigate the properties of the OSA starch. The results showed that the OSA starch paste had higher peak viscosities, HPV and CPV than native waxy wheat starch. Moreover, the degree of substitution(DS) is increased, the PV, HPV and CPV of OSA starch paste increased, but the peak time decreased; Comparing with native waxy wheat starch, the paste clarity, retrogradation and freeze-thaw stability of OSA starch had enhanced, and more, as the DS was getting higher, the paste clarity, retrogradation and freeze-thaw stability of OSA starch was better; The paste clarity and retrogradation of OSA starch greatly decreased by the presence of sodium chloride, but only increased slightly in the presence of sucrose; Emulsification property of the OSA starch increased with DS increasing.
At last, work over the effect of the OSA starch on the cracking rate of deep-frozen dumpling peel. When the degree of substitution of the OSA starch increased, the cracking rate of deep-frozen dumpling peel decreased. Moreover, the cracking rate of deep-frozen dumpling peel decreased with the addition of the same DS starch increasing.
引文
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