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

ZHANG Zhe; SUN Na; CHEN Jianan; JI Hongwei; LANG Yuanlu; ZHANG Jindou; ZHAO Enhui; LIU Weibing; TIAN Jinjin

doi:10.13386/j.issn1002-0306.2021050131

Volume 43 Issue 4

Feb. 2022

Turn off MathJax

Article Contents

Abstract

References

Science and Technology of Food Industry > 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:

PDF (3142 KB)

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

School of Mechanical Engineering, Tianjin University of Commerce, Tianjin 300134, China

More Information

Received Date: May 16, 2021
Available Online: December 13, 2021

Graphical Abstract

Abstract

Abstract

The T_c (collapse temperature) and thermal history of the solution were studied using freeze-drying microscopy and differential scanning calorimetry (DSC), the T_g´ (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 T_g´ and T_c 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 T_g´ and T_c 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 T_c 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 T_c and T_g´, and T_c was 3~4 ℃ higher than T_g´. However, the higher the freezing rate, the more obvious the collapse phenomenon, with the increasing of heating rate , T_c and T_g´ increased and collapse phenomenon aggravates, T_c increased more obviously, the drying effect was better at 1 ℃/min. With the reduction of IMO/D-Mannitol ratio, T_g´ 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, T_c was 6~7 ℃ higher than T_g´. When a small amount of D-Mannitol was added, the dried structure was better preserved, T_c was higher than that of IMO solution at 9:1, and the drying layer maintained better.
- isomaltose (IMO),
- D-mannitol,
- collapse temperature,
- glass transition,
- low temperature transition,
- devitrification

FullText(HTML)

References (29)

References

[1]	MAITE H, DAVIDE F. On the effects of freeze-drying processes on the nutritional properties of foodstuff: A review[J]. Drying Technology,2020,38(7):846−868. doi: 10.1080/07373937.2019.1599905
[2]	U VETRÁKOVÁ, V NEDĚLA, RUNTUK J, et al. Dynamical in-situ observation of the lyophilization and vacuum-drying processes of a model biopharmaceutical system by an environmental scanning electron microscope[J]. International Journal of Pharmaceutics,2020,585:119448. doi: 10.1016/j.ijpharm.2020.119448
[3]	金敬红, 孙晓明, 陈文华. 真空冷冻干燥过程中微生物数量变化规律的初步研究[J]. 中国野生植物资源,2019,38(4):48−52. [JIN Jinghong, SUN Xiaoming, CHEN Wenhua. Preliminary study on the variation of microorganism quantity during vacuum freeze drying[J]. Chinese Wild Plant Resources,2019,38(4):48−52. doi: 10.3969/j.issn.1006-9690.2019.04.010
[4]	左建国, 李维仲, 翁林岽. 冷冻干燥参数对塌陷温度的影响分析[J]. 农业机械学报,2011,42(2):126−129. [ZUO Jianguo, LI Weizhong, WENG Lindong. Analysis of influence of freeze drying parameters on collapse temperature[J]. Transactions of the Chinese Society for Agricultural Machinery,2011,42(2):126−129.
[5]	王海鸥, 王前菊, 姜英, 等. 葡萄糖-柠檬酸溶液浸渍处理对冻干苹果片品质的影响[J]. 江苏农业学报,2020,36(2):477−486. [WANG Haiou, WANG Qianju, JIANG Ying, et al. Effect of glucose-citric acid solution impregnation on the quality of lyophilized apple slices[J]. Journal of Jiangsu Agricultural Sciences,2020,36(2):477−486. doi: 10.3969/j.issn.1000-4440.2020.02.031
[6]	李维杰, 周新丽, 刘宝林, 等. 升降温速率对低温保护剂溶液结晶性质的影响[J]. 化工学报,2013,64(8):2969−2974. [LI Weijie, ZHOU Xinli, LIU Baolin, et al. Effect of cooling rate on crystallization properties of cryoprotectant solution[J]. Journal of Chemical Industry and Technology,2013,64(8):2969−2974.
[7]	刘占杰, 华泽钊, 陶乐仁, 等. 不同保护剂浓度和不同降温速率对脂质体玻璃化转变温度的影响[J]. 低温工程,2000(6):1−5. [LIU Zhanjie, HUA Zezhao, TAO Leren, et al. Effect of different concentration of protective agent and different cooling rate on glass transition temperature of liposome[J]. Cryogenic Engineering,2000(6):1−5. doi: 10.3969/j.issn.1000-6516.2000.06.001
[8]	SABLANI S S, RAHMAN M S, AL BUSAIDI S, et al. Thermal transitions of king fish whole muscle, fat and fat-free muscle by differential scanning calorimetry[J]. Thermochimica Acta,2007,462(1):56−63.
[9]	张昊阳, 乔春艳, 党高平, 等. 基于真空冷冻干燥的羊乳及其分离产物的差示扫描量热学分析[J/OL]. 食品科学技术学报: 1−14[2020-09-08]. http://kns.cnki.net/kcms/detail/10.1151.TS. 20200814.1721.002. ZHANG Haoyang, QIAO Chunyan, DANG Gaoping, et al. Differ html ential scanning calorimetry analysis of vacuum freeze-drying sheep milk and its separation products [J/OL]. Journal of Food Science and Technology: 1−14 [2020-09-08]. http://kns.cnki.net/kcms/detail/10.1151TS.20200814.1721.002.html.
[10]	赵学伟, 毛多斌. 玻璃化转变对食品稳定性的影响[J]. 食品科学,2007(12):539−546. [ZHAO Xuewei, MAO Duobin. Effect of glass transition on food stability[J]. Food Science,2007(12):539−546. doi: 10.3321/j.issn:1002-6630.2007.12.129
[11]	SWATI M, ZHU Z Q, SUN D W. Glass transitions as affected by food compositions and by conventional and novel freezing technologies: A review[J]. Trends in Food Science & Technology,2019,94:1−11.
[12]	赵凯, 李君, 刘宁, 等. 小麦淀粉老化动力学及玻璃化转变温度[J]. 食品科学,2017,38(23):100−105. [ZHAO Kai, LI Jun, LIU Ning, et al. Aging kinetics and glass transition temperature of wheat starch[J]. Food Science,2017,38(23):100−105. doi: 10.7506/spkx1002-6630-201723017
[13]	KNOPP S A, CHONGPRASERT S, NAIL S L. The relationship between the TMDSC curve of frozen sucrose solutions and collapse during freeze-drying[J]. Journal of Thermal Analysis and Calorimetry,1998,54(2):659−672. doi: 10.1023/A:1010115230736
[14]	KALICHEVSKV M T, JAROSZKIEWICZ E M, ABLETT S, et al. The glass transition of amylopectin measured by DSC, DMTA and NMR[J]. Carbohydrate Polymers,1992,18(2):77−88. doi: 10.1016/0144-8617(92)90129-E
[15]	BLOND G, SIMATOS D, CATTÉ M, et al. Modeling of the water-sucrose state diagram below 0 °C[J]. Carbohydrate Research,1997,298(3):139−145. doi: 10.1016/S0008-6215(96)00313-8
[16]	SHALAEV E Y, FRANKS F. Equilibrium phase diagram of the water-sucrose-NaCl system[J]. Thermochimica Acta,1995,255(5):49−61.
[17]	BALASUBRAMANIAN S, APRAMITA DEVI, SINGH K K, et al. Application of glass transition in food processing[J]. Critical Reviews in Food Science and Nutrition,2016,56(6):919−936. doi: 10.1080/10408398.2012.734343
[18]	吕福扣, 刘宝林, 李维杰. HA纳米微粒对PEG-600低温保护剂反玻璃化结晶的影响[J]. 低温物理学报,2012,34(4):315−320. [LV Fukou, LIU Baolin, LI Weijie. Effect of HA nanoparticles on reverse vitrification of PEG-600 cryoprotectant[J]. Chinese Journal of Low Temperature Physics,2012,34(4):315−320.
[19]	JEERARUANGRATTANA Y, SMITH G, POLYGALOV E, et al. Determination of ice interface temperature, sublimation rate and the dried product resistance, and its application in the assessment of microcollapse using through-vial impedance spectroscopy[J]. European Journal of Pharmaceutics and Biopharmaceutics, 2020, 152: 144−163.
[20]	SABINE U, STEFAN S, GEOFFREY L. Measurement of shrinkage and cracking in lyophilized amorphous cakes, Part 3: Hydrophobic vials and the question of adhesion[J]. Journal of Pharmaceutical Sciences,2015,104(6):2040−2046. doi: 10.1002/jps.24441
[21]	刘代春, 于颖, 卢存义. 冻干显微镜研究进展[J]. 机电信息,2017(32):1−15. [LIU Daichun, YV Ying, LU Cunyi. Research progress of lyophilization microscope[J]. Mechanical and Electrical Information,2017(32):1−15. doi: 10.3969/j.issn.1671-0797.2017.32.001
[22]	OHORI R, AKITA T, YAMASHITA C. Effect of temperature ramp rate during the primary drying process on the properties of amorphous-based lyophilized cake, Part 2: Successful lyophilization by adopting a fast ramp rate during primary drying in protein formulations[J]. Eur J Pharm Biopharm,2018,130:83−95. doi: 10.1016/j.ejpb.2018.06.010
[23]	ULLRICH S, SEYFERTH S, LEE G. Measurement of shrinkage and cracking in lyophilized amorphous cakes. Part II: Kinetics [J]. Pharmaceutical Research, 2015, 32(8).
[24]	HERTEL N, BIRK G, SCHERLIEß R. Performance tuning of particle engineered mannitol in dry powder inhalation formulations[J]. International Journal of Pharmaceutics,2020:586.
[25]	CHEN Ming, ZHANG Wenli, WU Hao, et al. Mannitol: Physiological functionalities, determination methods, biotechnological production, and applications[J]. Applied Microbiology and Biotechnology,2020,104(16):6941−6951. doi: 10.1007/s00253-020-10757-y
[26]	THAKRAL S, SONJE J, SURYANARAYANAN R. Anomalous behavior of mannitol hemihydrate: Implications on sucrose crystallization in colyophilized systems[J]. International Journal of Pharmaceutics, 2020, 587: 119629-119629.
[27]	张雪芹, 王超先, 郝伟萍. 差示扫描量热法对PET热性能的研究[J]. 塑料工业,2001(5):41−42,48. [ZHANG Xueqin, WANG Chaoxian, HAO Weiping. Study on thermal properties of PET by differential scanning calorimetry[J]. Plastics Industry,2001(5):41−42,48. doi: 10.3321/j.issn:1005-5770.2001.05.017
[28]	吴唯, 毕丽颖, 陈玉, 等. PET/PEN共混物的结晶与冷结晶性能及其机理[J]. 高分子材料科学与工程, 2013, 29(1): 67-70. WU Wei, BI Liying, CHEN Yv, et al. Crystallization and cold crystallization properties and mechanism of PET/PEN blends[J]. Polymer Materials Science and Engineering, 2013, 29(1): 67-70.
[29]	杨智, 李代禧, 张燕, 等. 冷冻干燥过程中重要参数塌陷温度的研究[J]. 应用化工,2014,43(5):962−965. [YANG Zhi, LI Daixi, ZHANG Yan, et al. Study on collapse temperature of important parameter in freeze drying process[J]. Applied Chemical Industry,2014,43(5):962−965.

Supplements (0)

Cited By

Cited by

Periodical cited type(12)

1.	黄靖，胡利利，何婉莺，王鹏，张润光，田洪磊，詹萍，耿敬章. 九蒸九制对滇黄精呈香品质及抗氧化活性的影响. 食品研究与开发. 2025(01): 70-79 .
2.	马永强，张一鹏，王鑫，张丝瑶. 九蒸九制对黄精中AGEs含量、多糖结构及体外活性的影响. 食品工业科技. 2024(03): 226-234 . 本站查看
3.	许梦粤，丁泽宇，李锦鹏，王灿，王铭阳，刘琴，曾长立，王红波. 大豆多糖与纳豆多糖结构特征和主要生物活性比较. 食品科学. 2024(07): 78-86 .
4.	李得天，封亮，贾晓斌，杨冰. 黄精炮制原理解析及工艺优化策略. 中草药. 2024(20): 7110-7121 .
5.	杨庆雄，李欣. 林下经济作物黄精的研究进展. 贵州师范大学学报(自然科学版). 2024(06): 1-34+140 .
6.	毛子俊，王金兰，张树军，赵英楠，王丹，孙立秋，赵明，时志春，李军. 干鲜2种马齿苋多糖的提取及其抗氧化活性与吸湿保湿性能研究. 中国野生植物资源. 2024(11): 1-10 .
7.	刘心洁，周安，刘亚鹏，陈文迪，陈雪莉，俞年军，吴振东，梁娟. “九蒸九制”对黄精滋味品质及多糖结构变化的影响. 中医药导报. 2023(04): 46-52 .
8.	吴兰兰，吴钢，谭强来，林锦峰，甘淑娇，熊梅惠，吴伟菁. 煮制对多花黄精多糖结构及其体外免疫刺激活性的影响. 中国食物与营养. 2023(06): 28-34 .
9.	程亚楠，张金华，田胜兰，杨超然，司靖宇，黄丽莉，胡晓波，余强. 不同来源多花黄精多糖的结构特性及抗氧化活性比较. 现代食品科技. 2023(07): 145-153 .
10.	屈雅宁，许梦粤，唐双庆，刘琴，陈禅友，王亚珍，王红波. 枯草芽孢杆菌发酵对豆类粗多糖结构与抗氧化活性的影响. 食品工业科技. 2023(17): 129-138 . 本站查看
11.	唐军，杨欣，杨鑫，胡琦，高继海，杨明，贺亚男，张定堃. 附子多糖的结构、构效关系与生物活性研究进展. 中国中药杂志. 2023(20): 5410-5418 .
12.	王超，孙浩然，苏为耿，阚欢，刘云. 响应面法优化低糖滇黄精果脯制备工艺. 山东农业科学. 2022(12): 129-135 .