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中国精品科技期刊2020
张哲,孙娜,陈佳楠,等. IMO/D-甘露醇水溶液玻璃化转变温度的确定及冻干过程塌陷现象分析[J]. 食品工业科技,2022,43(4):33−40. doi: 10.13386/j.issn1002-0306.2021050131.
引用本文: 张哲,孙娜,陈佳楠,等. IMO/D-甘露醇水溶液玻璃化转变温度的确定及冻干过程塌陷现象分析[J]. 食品工业科技,2022,43(4):33−40. doi: 10.13386/j.issn1002-0306.2021050131.
ZHANG Zhe, SUN Na, CHEN Jianan, et al. Determination of Glass Transition Temperature of IMO/D-Mannitol Aqueous Solution and Analysis of Collapse Phenomenon during Freeze-drying Process of Solution[J]. Science and Technology of Food Industry, 2022, 43(4): 33−40. (in Chinese with English abstract). doi: 10.13386/j.issn1002-0306.2021050131.
Citation: ZHANG Zhe, SUN Na, CHEN Jianan, et al. Determination of Glass Transition Temperature of IMO/D-Mannitol Aqueous Solution and Analysis of Collapse Phenomenon during Freeze-drying Process of Solution[J]. Science and Technology of Food Industry, 2022, 43(4): 33−40. (in Chinese with English abstract). doi: 10.13386/j.issn1002-0306.2021050131.

IMO/D-甘露醇水溶液玻璃化转变温度的确定及冻干过程塌陷现象分析

Determination of Glass Transition Temperature of IMO/D-Mannitol Aqueous Solution and Analysis of Collapse Phenomenon during Freeze-drying Process of Solution

  • 摘要: 采用冻干显微镜和差示扫描量热法(DSC)研究了溶液的塌陷温度Tc和热历史特性,将两种测量结果相结合确定冷冻浓缩状态下的玻璃化转化温度Tg´,分析不同升降温速率对低聚异麦芽糖(IMO)溶液Tg´及Tc的影响,根据D-甘露醇反玻璃化和强化冰晶结构的特性,研究其对IMO溶液Tg´和Tc的影响。结果表明:溶液的热历史存在低温和高温转变,测定的Tc在低温转变结束和高温转变开始之间,根据冷冻浓缩液转变特性,确定低温转变为玻璃化转变;降温速率对Tc和Tg´无显著影响,且Tc均比Tg´高3~4 ℃,但降温速率越大塌陷越严重;Tc和Tg´随升温速率的增大而增大,Tc升高较明显,塌陷随升温速率升高而加剧,1 ℃/min升温时干燥效果较好;Tg´随着IMO:D-甘露醇比值的降低而减小,反玻璃化越明显,5:5时最为明显,9:1和5:5较IMO溶液干燥效果好,8:2时塌陷最严重,Tc均比Tg´高6~7 ℃,添加少量D-甘露醇时干燥结构完整,9:1时Tc高于IMO溶液的值且干燥层保持较好。

     

    Abstract: The Tc (collapse temperature) and thermal history of the solution were studied using freeze-drying microscopy and differential scanning calorimetry (DSC), the Tg´ (glass transition temperature of the maximally freeze-concentrated state) was determined according to the two results obtained. The effects of different heating and freezing rated on Tg´ and Tc of isomaltose (IMO) solution were analyzed. The effect of D-Mannitol solution, according to its characteristics reverse glass transition and enhancement of ice crystal structure, on Tg´ and Tc of IMO solution was investigated. It could be concluded that the low and high temperature transitions presented in the thermal history of sample solutions. The measured Tc existed between the end of low temperature transition and the beginning of high temperature transition, and the low temperature transition was identified to be glass transition according to the freeze-concentrated state of solutions. The freezing rates had no significant effect on Tc and Tg´, and Tc was 3~4 ℃ higher than Tg´. However, the higher the freezing rate, the more obvious the collapse phenomenon, with the increasing of heating rate , Tc and Tg´ increased and collapse phenomenon aggravates, Tc increased more obviously, the drying effect was better at 1 ℃/min. With the reduction of IMO/D-Mannitol ratio, Tg´ decreased and the devitrification phenomenon became more obvious, the most was 5:5, the drying effect of 9:1 and 5:5 was better than that of IMO solution, the collapse was worst at 8:2, Tc was 6~7 ℃ higher than Tg´. When a small amount of D-Mannitol was added, the dried structure was better preserved, Tc was higher than that of IMO solution at 9:1, and the drying layer maintained better.

     

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