Box-Behnken响应面法优化丁香挥发油包合物制备工艺

马英; 刘语柔; 刘晓会

doi:10.12299/jsues.24-0085

Box-Behnken响应面法优化丁香挥发油包合物制备工艺

doi: 10.12299/jsues.24-0085

上海工程技术大学化学化工学院, 上海 201620

基金项目: 上海工程技术大学大学生创新训练项目（CX2204001）

详细信息

作者简介:
刘语柔：马　英（1996 − ），女，硕士生，研究方向为天然抗菌药物。E-mail：my13310102107@163.com

通讯作者:
刘晓会（1978 − ），女，讲师，博士，研究方向为天然抗感染药物。E-mail：xhui1113@sues.edu.cn

中图分类号: R944
计量
- 文章访问数: 14
- HTML全文浏览量: 10
- PDF下载量: 1
- 被引次数: 0
出版历程
- 收稿日期: 2023-03-23
- 网络出版日期: 2025-09-30
- 刊出日期: 2025-06-30

Optimization of preparation process of clove volatile oil inclusion complex by Box-Behnken response surface methodology

School of Chemistry and Chemical Engineering, Shanghai University of Engineering Science, Shanghai 201620, China

摘要

摘要: 采用饱和水溶液法制备丁香挥发油羟丙基-β-环糊精包合物。在单因素实验的基础上，选择羟丙基-β-环糊精与挥发油比例、包合温度、包合时间作为自变量，以综合评分为响应值，采用Box-Behnken响应面法优化包合工艺，得到最佳包合工艺为：羟丙基-β-环糊精与挥发油的混合比例为14.5∶1，包合温度59 ℃，包合时间2.4 h。3组验证实验的综合评分为92.21%±0.50%，与预测值接近，表明该模型的预测准确可靠。该包合物经显微镜观察，薄层色谱法(TLC)分析，红外光谱鉴别，证明已形成稳定的包合物，为进一步开发利用丁香挥发油提供数据支持。
- 丁香挥发油 /
- 羟丙基-β-环糊精 /
- 工艺优化 /
- Box-Behnken响应面法
Abstract: To prepare the hydroxypropyl-β-cyclodextrin inclusion complex from clove essential oil using saturated aqueous solution method. Based on the single factor experiments, the ratio of hydroxypropyl-β-cyclodextrin to volatile oil, encapsulation temperature, and encapsulation time were used as influencing factors, and the comprehensive score was used as the response value. The encapsulation process was optimized by Box-Behnken response surface methodology. The optimal condition was obtained as the ratio of hydroxypropyl-β-cyclodextrin to volatile oil was 14.5∶1, with an inclusion temperature of 59 ℃ and an inclusion time of 2.4 h. The comprehensive score of the three validation experiments is 92.21%±0.50%, which is close to the predicted value, indicating that the prediction of the model is accurate and reliable. The inclusion complex was observed under microscope, analyzed by thin layer chromatography (TLC), and identified by infrared spectroscopy, proving the formation of a stable inclusion complex. These results can provide data support for further development and utilization of clove volatile oil.
- clove volatile oil /
- hydroxypropyl-β-cyclodextrin /
- process optimization /
- Box-Behnken response surface methodology

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图 1 包合比例对综合评分的影响

Figure 1. Effect of encapsulation ratio on composite score

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图 3 包合时间对综合评分的影响

Figure 3. Effect of encapsulation time on composite score

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图 2 包合温度对综合评分的影响

Figure 2. Effect of encapsulation temperature on composite score

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图 4 3D响应面图与等高线图

Figure 4. 3D response surface and contour plot

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图 5 样品表面形貌显微图

Figure 5. Microscopic images of sample surface morphology

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图 6 薄层色谱图

Figure 6. Thin-layer chromatography (TLC) Chart

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图 7 样品红外光谱图

Figure 7. Infrared spectrum chart of samples

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表 1 因素水平表

Table 1. Factor levels table

水平	包合比例	包合温度/℃	包合时间/h
−1	12∶1	50	2.0
0	15∶1	60	2.5
1	18∶1	70	3.0

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表 2 响应面实验设计与结果

Table 2. Experimental design and results of response surface

实验号	A	B	C	含油率/%	包合率/%	收率/%	综合评分
1	−1	−1	0	27.60	17.36	69.63	79.86
2	1	−1	0	33.71	14.47	69.06	77.88
3	0	−1	1	28.59	15.97	53.05	72.84
4	−1	0	−1	39.06	19.82	69.65	94.21
5	0	0	0	29.71	14.22	61.94	72.24
6	1	0	1	21.82	13.9	68.75	67.39
7	1	0	−1	28.26	15.79	63.29	75.05
8	−1	1	0	29.64	15.28	57.50	73.33
9	0	−1	−1	33.84	16.84	71.06	83.37
10	0	1	−1	29.29	16.55	62.58	77.34
11	−1	0	1	29.31	19.16	67.00	84.50
12	0	0	0	37.31	22.21	59.40	95.36
13	0	0	0	23.31	13.40	61.52	65.37
14	1	1	0	35.92	19.31	65.76	89.55
15	0	0	0	28.3	17.91	69.19	81.52
16	0	0	0	34.42	18.71	65.05	84.84
17	0	1	1	35.4	20.70	60.46	90.79

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表 3 方差分析结果

Table 3. Analysis of variance results

方差来源	平方和	自由度υ	均方	F值	P值
模型	1192.56	9	132.51	9.43	0.0037
A	36.04	1	36.04	2.57	0.1532
B	36.99	1	36.99	2.63	0.1487
C	156.78	1	156.78	11.16	0.0124
AB	26.42	1	26.42	1.88	0.2126
AC	46.52	1	46.52	3.31	0.1116
BC	2.48	1	2.48	0.18	0.6872
A²	217.31	1	217.31	15.47	0.0057
B²	129.52	1	129.52	9.22	0.0189
C²	454.78	1	454.78	32.38	0.0007
残差	98.32	7	14.05	—	—
失拟项	50.19	3	16.73	1.39	0.3675
纯误差	48.13	4	12.03	—	—
总计	1290.88	16	—	—	—

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