响应面法优化微波辅助水蒸气蒸馏法提取油樟精油工艺

doi:10.16085/j.issn.1000-6613.2020-0593

摘要/Abstract

摘要：

为了解决油樟精油传统提取工艺时间长、效率低、耗能高和成本高等问题，本文遵循绿色提取理念，采用微波辅助水蒸气蒸馏法提取油樟精油并优化最佳提取工艺。根据单因素试验并结合响应面法建立二次回归模型进行方差分析和诊断，考察物料粒度、微波提取时间和微波提取功率对油樟精油得率的影响，确定最佳提取工艺并对理论结果进行实验验证。结果表明，在油樟精油得率相似的情况下，与传统的水蒸气蒸馏法（2h）相比，微波辅助水蒸气蒸馏法（10min）具有提取时间更短、效率更高和更节约能源的优势。通过二次多项式回归模型极显著（P<0.01），失拟项不显著（P>0.05），决定系数为R²=0.989等分析结合诊断图表明该模型对数据拟合良好。微波辅助水蒸气蒸馏法提取油樟精油最佳提取工艺为：物料粒度10目，微波提取时间11min，微波提取功率630W，此条件下油樟精油得率为4.479%，与实验验证结果（4.442%±0.16%）基本一致，验证了二次回归模型的可靠性。该技术较传统工艺提取时间短、效率高、耗能少、成本低，更加绿色安全且容易实现产业化，有望提高油樟精油在日化、美容、医药等各个领域的应用价值。

关键词: 油樟精油, 微波, 提取, 响应面法, 优化, 实验验证

Abstract:

In order to solve the problems of long time, low efficiency, high energy consumption and high cost of traditional extraction process of Cinnamomum longepaniculatum essential oil, following the concept of green extraction, the microwave-assisted steam distillation method was adopted to extract the essential oil of C. longepaniculatum and the optimal extraction process was optimized. A quadratic regression model was established, variance analysis and diagnosis were carried out based on single factor test and response surface methodology. The effect of particle size, microwave extraction time and microwave extraction power on the yield of C. longepaniculatum essential oil was investigated to determine the optimal extraction process, and the theoretical results were verified by experiments. The results showed that microwave-assisted steam distillation method (10min) had the advantages of shorter extraction time, higher efficiency and more energy saving than the traditional steam distillation method (2h) when the yield of essential oil was similar. The quadratic polynomial regression model was very significant (P<0.01). Lack of fit was not significant (P>0.05), and the coefficient of determination was R²=0.989, and the analysis indicate that the model fits the data well combined with the diagnosis chart. The optimal extraction process of C. longepaniculatum essential oil by the microwave-assisted steam distillation method was as follows: particle size of material was 10 meshes, microwave extraction time was 11 min, microwave extraction power was 630W. Under this condition, the yield of essential oil was 4.479%, which was basically consistent with the experimental verification results (4.442%+0.16%), and the reliability of the quadratic regression model was verified. Compared with the traditional process, this technology has the advantages of shorter extraction time, higher efficiency, low energy consumption, lower cost, it is more green, safe and easy to realize industrialization, it is expected to improve the application value of C. longepaniculatum essential oil in various fields such as daily chemistry, beauty, medicine and so on.

Key words: Cinnamomum longepaniculatum essential oil, microwave, extraction, response surface method, optimization, experimental validation

中图分类号:

张圆圆, 孟永斌, 张琳, 祖元刚. 响应面法优化微波辅助水蒸气蒸馏法提取油樟精油工艺[J]. 化工进展, 2020, 39(S2): 291-299.

Yuanyuan ZHANG, Yongbin MENG, Lin ZHANG, Yuangang ZU. Optimization of microwave-assisted steam distillation extraction of Cinnamomum longepaniculatum essential oil by response surface methodology[J]. Chemical Industry and Engineering Progress, 2020, 39(S2): 291-299.

图/表 11

参考文献 44

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实验号	因素			响应值Y
实验号	A/目	B/min	C/W	实际值	预测值
1	-1	-1	0	2.86	2.99
2	1	-1	0	2.09	2.08
3	-1	1	0	4.30	4.30
4	1	1	0	3.66	3.52
5	-1	0	-1	3.26	3.22
6	1	0	-1	2.04	2.14
7	-1	0	1	3.91	3.81
8	1	0	1	3.15	3.19
9	0	-1	-1	1.51	1.42
10	0	1	-1	2.88	2.92
11	0	-1	1	2.40	2.36
12	0	1	1	3.52	3.62
13	0	0	0	4.15	3.99
14	0	0	0	3.97	3.99
15	0	0	0	3.89	3.99
16	0	0	0	3.91	3.99
17	0	0	0	4.05	3.99

实验号	因素			响应值Y
实验号	A/目	B/min	C/W	实际值	预测值
1	-1	-1	0	2.86	2.99
2	1	-1	0	2.09	2.08
3	-1	1	0	4.30	4.30
4	1	1	0	3.66	3.52
5	-1	0	-1	3.26	3.22
6	1	0	-1	2.04	2.14
7	-1	0	1	3.91	3.81
8	1	0	1	3.15	3.19
9	0	-1	-1	1.51	1.42
10	0	1	-1	2.88	2.92
11	0	-1	1	2.40	2.36
12	0	1	1	3.52	3.62
13	0	0	0	4.15	3.99
14	0	0	0	3.97	3.99
15	0	0	0	3.89	3.99
16	0	0	0	3.91	3.99
17	0	0	0	4.05	3.99

来源	平方和	自由度	均方	F值	P值
模型	11.294	9	1.255	69.101	<0.0001
A	1.435	1	1.435	79.008	<0.0001
B	3.772	1	3.772	207.685	<0.0001
C	1.347	1	1.347	74.187	<0.0001
AB	0.004	1	0.004	0.212	0.659
AC	0.052	1	0.052	2.863	0.135
BC	0.015	1	0.015	0.813	0.397
A2	0.070	1	0.070	3.851	0.091
B2	1.725	1	1.725	95.004	<0.0001
C2	2.530	1	2.530	139.302	<0.0001
残差	0.127	7	0.018	—	—
失拟项	0.081	3	0.027	2.358	0.213
纯误差	0.046	4	0.011	—	—
总离差	11.421	16	—	—	—

来源	平方和	自由度	均方	F值	P值
模型	11.294	9	1.255	69.101	<0.0001
A	1.435	1	1.435	79.008	<0.0001
B	3.772	1	3.772	207.685	<0.0001
C	1.347	1	1.347	74.187	<0.0001
AB	0.004	1	0.004	0.212	0.659
AC	0.052	1	0.052	2.863	0.135
BC	0.015	1	0.015	0.813	0.397
A2	0.070	1	0.070	3.851	0.091
B2	1.725	1	1.725	95.004	<0.0001
C2	2.530	1	2.530	139.302	<0.0001
残差	0.127	7	0.018	—	—
失拟项	0.081	3	0.027	2.358	0.213
纯误差	0.046	4	0.011	—	—
总离差	11.421	16	—	—	—

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