橘皮油微胶囊制备及其产品质量评价

doi:10.16085/j.issn.1000-6613.2022-1347

摘要/Abstract

摘要：

橘皮油的易挥发、易氧化等特点使其难以长期保存。为了延长橘皮油的保质期并丰富其应用范围，本文利用微胶囊技术，以麦芽糊精和阿拉伯胶为复配壁材，分别采用喷雾干燥法和冷冻干燥法对橘皮油进行包埋，并对所得产品进行质量评价。喷雾干燥的最佳工艺参数为：进风温度194℃、进料速度90.2mL/min和料液固含量34.7%。冷冻干燥的工艺参数为冷冻温度-30℃、干燥室压力30Pa和干燥室温度30℃。在此工艺条件下，喷雾干燥法和冷冻干燥法制备的橘皮油微胶囊包埋率分别为90.17%和82.48%。喷雾干燥产品呈规则球形、质感细腻并且囊壁致密，而冷冻干燥产品呈不规则的薄片状，但水分含量较低并且流动性好。2种干燥产品都具有一定的耐热能力，可以减少芯材在贮存和使用过程中的受热损失。综合比较，喷雾干燥法比冷冻干燥法更适合应用于制备橘皮油微胶囊产品。

关键词: 喷雾干燥, 冷冻干燥, 橘皮油, 微胶囊, 质量评价

Abstract:

Mandarin oil is characterized by easy volatilization and oxidization, which is difficult for long-term storage. Spray drying and freeze-drying methods were adopted in this work to encapsulate the mandarin oil in order to prolong its shelf life and enrich its application scope. Microcapsules qualities, such as encapsulation efficiency and product microstructure, were evaluated. Optimal operating conditions of spray drying were air inlet temperature 194˚C, feed flow rate 90.2mL/min, and feed solid content 34.7%. Operating conditions of freeze-drying were freezing temperature -30˚C, chamber pressure 30Pa, and radiation temperature 30˚C. Encapsulation efficiencies of products prepared by spray drying and freeze-drying were 90.17% and 82.48%, respectively, under the present conditions. The products by spray drying were fine and sphere-like with dense microcapsule walls, while the products by freeze-drying were irregular and platelet-shaped but with lower moisture content and better fluidity. Both products exhibited certain heat resistances, which could reduce the heat-induced loss of core materials in storage and application. In general, the spray drying method was more suitable than the freeze-drying method for the preparation of mandarin oil microcapsules.

Key words: spray drying, freeze-drying, mandarin oil, microcapsule, quality evaluation

中图分类号:

TQ028.5

孙闫晨昊, 王维, 李一喆, 祝妍妮, 刘学武, 张大为. 橘皮油微胶囊制备及其产品质量评价[J]. 化工进展, 2023, 42(5): 2626-2637.

SUN Yanchenhao, WANG Wei, LI Yizhe, ZHU Yanni, LIU Xuewu, ZHANG Dawei. Preparation of mandarin oil microcapsules and its product quality evaluation[J]. Chemical Industry and Engineering Progress, 2023, 42(5): 2626-2637.

图/表 12

图1 喷雾干燥系统流程图1—输料泵；2—雾化器；3—电加热器；4—鼓风机；5—空气过滤器；6—引风机；7—旋风分离器；8—干燥塔；9—冷风鼓风机；10—控制电源

图2 冷冻干燥系统流程图1—干燥室；2—干燥样品；3—搁板；4—共晶点传感器；5—乳化液；6—冷阱；7—压力控制阀；8—通气阀；9—冷凝水排除阀；10—真空泵；11—冰柜；12—计算机

图3 不同芯壁比、进风温度、进料速度和固含量下橘皮油微胶囊的包埋率

表1 响应面因素水平表

因素	-1	0	1
A：进风温度/℃	180	190	200
B：进料速度/mL·min^–1	80	90	100
C：固含量质量分数/%	30	35	40

表2 响应面实验设计及结果

编号	进风温度 /℃	进料速度 /mL·min^–1	固含量（质量分数） /%	包埋率 /%
1	180	80	35	88.17
2	200	80	35	86.76
3	180	100	35	85.37
4	200	100	35	87.55
5	180	90	30	81.98
6	200	90	30	87.43
7	180	90	40	86.46
8	200	90	40	84.80
9	190	80	30	85.03
10	190	100	30	83.49
11	190	80	40	85.08
12	190	100	40	84.83
13	190	90	35	89.51
14	190	90	35	89.34
15	190	90	35	88.97
16	190	90	35	90.00
17	190	90	35	90.30

表3 响应面模型方差分析

方差分析	平方和	自由度	均方	F值	p值
模型	100.01	9	11.11	59.23	< 0.0001
A	5.54	1	5.54	29.55	0.0010
B	2.29	1	2.29	12.21	0.0101
C	1.31	1	1.31	6.99	0.0332
AB	8.09	1	8.09	43.14	0.0003
AC	12.64	1	12.64	67.37	< 0.0001
BC	0.4160	1	0.4160	2.22	0.1801
A²	5.19	1	5.19	27.69	0.0012
B²	11.75	1	11.75	62.65	< 0.0001
C²	47.13	1	47.13	251.24	< 0.0001
残差	1.31	7	0.1876	—	—
失拟项	0.1935	3	0.0645	0.2304	0.8711
纯误差	1.12	4	0.2799	—	—
总和	101.32	16	—	—	—

图4 交互项对包埋率交互影响的响应面和等高线图

图5 共晶点测试系统记录数据

图6 喷雾干燥法和冷冻干燥法制备的产品外观形貌

图7 喷雾干燥法和冷冻干燥法所得产品的SEM图

图8 喷雾干燥法和冷冻干燥法制备产品的差示扫描量热曲线

图9 喷雾干燥法和冷冻干燥法制备产品的热重曲线

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