高取代度磷酸魔芋葡甘聚糖酯的制备
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摘要
以魔芋葡甘聚糖(konjac glucomannan,KGM)、Na H_2PO_4与Na_2HPO_4混合盐为原料,采用真空辅助微波半干法制备高取代度磷酸魔芋葡甘聚糖酯(konjac glucomannan phosphate ester,KGMP),通过单因素试验研究了微波时间、微波温度、酯化剂与KGM摩尔比、真空处理时间、p H值、尿素用量对取代度的影响,并通过响应面试验确定最佳工艺参数并研究所得产物的基本性质。结果表明,真空辅助微波半干法制备高取代度KGMP的最佳工艺条件:微波时间7 min、微波温度100℃、磷酸盐与KGM摩尔比为0.72∶1、真空处理时间29 s、p H值5.0、尿素用量(质量分数)6%,KGMP的取代度为0.199;随着取代度的增加,产品的黏度适度降低,透光率增加;红外光谱表明,KGM上引入了磷酸基团,得到KGMP。
Using microwave irradiation with vacuum-assisted method,konjac glucomannan phosphate ester(KGMP)with high degree of substitution was produced by semi-drying konjac glucomannan(KGM)and the mixture of NaH_2PO_4and Na_2HPO_4.Based on single-factor experiments,effects of microwave time,microwave temperature,molar ratio of esterifying agent to KGM,vacuum treatment time,pH value,and urea dosage on the degree of substitution of KGMP were studied.The results showed that the optimal conditions were as follows:at pH=5.0,microwaving at 100℃for 7 min,with 0.72∶1 as the molar ratio of esterifying agent to KGM,vacuum treating for 29 s,and with6%urea.The substitution degree of KGMP was 0.199.With increasing substitution degree,the product viscosity decreased,and the light transmittance significantly increased.Infrared spectroscopy indicated that phosphate groups were introduced to KGM,confirming the formation of KGMP.
Using microwave irradiation with vacuum-assisted method,konjac glucomannan phosphate ester(KGMP)with high degree of substitution was produced by semi-drying konjac glucomannan(KGM)and the mixture of NaH_2PO_4and Na_2HPO_4.Based on single-factor experiments,effects of microwave time,microwave temperature,molar ratio of esterifying agent to KGM,vacuum treatment time,pH value,and urea dosage on the degree of substitution of KGMP were studied.The results showed that the optimal conditions were as follows:at pH=5.0,microwaving at 100℃for 7 min,with 0.72∶1 as the molar ratio of esterifying agent to KGM,vacuum treating for 29 s,and with6%urea.The substitution degree of KGMP was 0.199.With increasing substitution degree,the product viscosity decreased,and the light transmittance significantly increased.Infrared spectroscopy indicated that phosphate groups were introduced to KGM,confirming the formation of KGMP.
引文
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[3]ZHU F. Modifications of konjac glucomannan for diverse applications[J]. Food Chemistry,2018,256:419-426.
[4]LI Shijie,XIONG Qingping,LAI Xiaoping,et al. Molecular modification of polysaccharides and resulting bioactivities[J]. Comprehensive Reviews in Food Science&Food Safety,2016,15(2):237-250.
[5]XIE Chenxin,FENG Yujun,CAO Weiping,et al. Novel biodegradable flocculating agents prepared by phosphate modification of Konjac[J]. Carbohydrate Polymers,2007,67(4):566-571.
[6]李坚斌,陈小云,张帆,等.葡甘露聚糖微波法磷酸酯化改性研究[J].食品科学,2015,36(8):19-23.
[7]王洋.魔芋阳离子交换树脂新法制备、结构及吸附特性研究[D].武汉:华中农业大学,2009.
[8]王福强.磷酸酯淀粉微波干法低温制备技术及性质研究[D].重庆:西南大学,2011.
[9]张晓宇.半干法制备两性淀粉研究[D].无锡:江南大学,2005.
[10]邓利玲,钟耕,刘倍毓,等.半干法酶解制备的魔芋葡甘低聚糖性质[J].食品科学,2013,34(15):115-119.
[11]梁叶星,熊家艳,王永红,等.辛烯基琥珀酸魔芋葡甘聚糖酯的微波半干法制备工艺及性能[J].食品科学,2013,34(14):163-168.
[12]黎斌,彭桂兰,吴绍峰,等.魔芋真空干燥特性及动力学模型的建立[J].食品与发酵工业,2017,43(8):115-122.
[13]ZHANG Qing,ZHANG Shuai,DENG Liling, et al.Effect of vacuum treatment on the characteristics of oxidized starches prepared using a green method[J]. StarchStrke,2017,70(3-4):1 700 216.
[14]PASSAUER L,LIEBNER F,FISCHER K. Synthesis and properties of novel hydrogels from cross-linked starch phosphates[J]. Macromolecular Symposia,2006,244(1):180-193.
[15]国家食品药品监督管理总局. GB 5009. 87—2016食品安全国家标准食品中磷的测定[S].北京:中国标准出版社,2016.
[16]王建,钱丽.半干法制备磷酸酯化纤维的工艺研究[J].陕西科技大学学报,2017,35(6):20-24.
[17]李巧云.淀粉磷酸单酯的微波合成研究[J].上海化工,2003,17(11):52-54.
[18]赵伟,李振花,冯芳.磷酸单酯淀粉制备工艺优化[J].食品科学,2010,31(20):89-92.
[19]安鸿雁,佟毅,刘馨远,等.半干法磷酸酯淀粉的制备[J].食品工业科技,2018(5).
[20]YANG Liping,WANG Haisong,ZHANG Haiwei,et al.Preparation and physicochemical properties of three types of modified glutinous rice starches.[J]. Carbohydrate Polymers,2016,137:305-313.
[21]SITOHY M Z,EL-SAADANY S S,LABIB S M,et al.Physicochemical properties of different types of starch phosphate monoesters[J]. Starch-Strke,2015,52(4):101-105.
[22]YANG Liping,ZHOU Yibin,ZHENG Xiangyu,et al.Determination of optimum experimental conditions for preparation and functional properties of hydroxypropylated,phosphorylated and hydroxypropyl-phosphorylated glutinous rice starch[J]. International Journal of Biological Macromolecules,2017,105(1):317-327.
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