离子液体辅助超声法提取工业大麻叶中大麻二酚的工艺优化

王崑仑; 管立军; 高扬; 严松; 李家磊; 李波; 周野

doi:10.13386/j.issn1002-0306.2022050272

离子液体辅助超声法提取工业大麻叶中大麻二酚的工艺优化

doi: 10.13386/j.issn1002-0306.2022050272

王崑仑^{1, 2,},
管立军^{1, 2, ,},
高扬^{1, 2},
严松^{1, 2},
李家磊^{1, 2},
李波^{1, 2},
周野^{1, 2}

1.
黑龙江省农业科学院食品加工研究所，黑龙江哈尔滨 150086
2.
黑龙江省食品加工重点实验室，黑龙江哈尔滨 150086

基金项目: 黑龙江省省属科研院所科研业务费（CZKYF2022-1-B021，CZKYF2021B001）；黑龙江省现代农业产业技术协同创新体系（YYM19STX-17）；黑龙江省农业科学院“农业科技创新跨越工程”专项（MLCX-22）。

详细信息

作者简介:
王崑仑（1982−），男，博士，助理研究员，研究方向：植物有效成分，食品工程与营养，E-mail：white19820708@163.com

通讯作者:
管立军（1983−），男，博士，副研究员，研究方向：植物有效成分，食品工程与营养，E-mail：qqaipphh@sina.com

中图分类号: TS255.1
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- 文章访问数: 45
- HTML全文浏览量: 26
- PDF下载量: 4
- 被引次数: 0
出版历程
- 收稿日期: 2022-05-25
- 网络出版日期: 2022-12-15
- 刊出日期: 2023-01-17

Process Optimization of the Method of Ionic Liquid Assisted Ultrasonic Extraction of Cannabidiol from Industrial Hemp Leaves

WANG Kunlun^{1, 2
,},
GUAN Lijun^{1, 2
, ,},
GAO Yang^{1, 2},
YAN Song^{1, 2},
LI Jialei^{1, 2},
LI Bo^{1, 2},
ZHOU Ye^{1, 2}

1.
Heilongjiang Province Academy of Agricultural Sciences Institute of Food Processing, Harbin 150086, China
2.
Heilongjiang Province Key Laboratory of Food Processing, Harbin 150086, China

摘要

摘要: 为提高工业大麻的经济价值，本研究以工业大麻叶为原料，利用离子液体辅助超声法提取具有药用价值的活性成分大麻二酚（CBD），并对提取工艺进行优化。本研究以CBD得率为指标，先从16种咪唑类离子液体中筛选出[C₈mim]NTF₂为最佳提取溶剂，再对影响离子液体辅助超声法提取CBD得率的6个因素（超声功率、超声温度、超声时间、乙醇溶液浓度、离子液体摩尔浓度和液料比）进行单因素实验，并确定乙醇浓度为65%，离子液体摩尔浓度为0.3 mol/L（65%乙醇溶液配制）。在此结果基础上，利用Plackett-Burman试验设计筛选出4个显著因素（超声功率、超声温度、超声时间和液料比）。并利用响应面Box-Behnken试验设计进一步优化提取工艺。确定CBD显著因素的最佳提取工艺条件为：超声功率280 W，超声温度50 ℃，超声时间62.5 min，液料比25 mL/g。在上述条件下，离子液体[C₈mim]NTF₂提取CBD得率为7.66%±0.2%、甲醇的CBD得率为6.42%±0.3%，65%乙醇溶液的CBD得率为5.81%±0.2%。即CBD的提取能力，离子液体[C₈mim]NTF₂>甲醇>65%乙醇溶液。通过CBD降解实验，表明离子液体[C₈mim]NTF₂的CBD降解率为16.40%±0.3%，小于甲醇的24.65%±0.6%和65%乙醇溶液的32.88%±0.5%，结果表明65%乙醇溶液加入离子液体[C₈mim]NTF₂后，既可以降低CBD的降解率，又可提高CBD的得率。本研究证明了离子液体既是 CBD的保护剂，也是CBD的优良提取溶剂，研发了离子液体辅助超声法提取CBD工艺，为工业大麻的开发利用提供数据支持。
- 工业大麻叶 /
- 大麻二酚（CBD） /
- 离子液体 /
- 超声提取 /
- Plackett-Burman设计 /
- 响应面
Abstract: In order to improve the economic value of industrial hemp, an active ingredient cannabinoid (CBD) with medicinal value from industrial hemp leaves was extracted by ionic liquid assisted ultrasonic method and the extraction process was optimized. In this study, [C₈mim]NTF₂ was selected as the best extraction solvent from 16 kinds of imidazole ionic liquids based on the yield of CBD. Then single factor experiment was conducted on six factors affecting the yield of CBD extraction by ionic liquid assisted ultrasonic method. The six factors included: Ultrasonic power, ultrasonic temperature, ultrasonic time, ethanol concentration, molar concentration of ionic liquid and liquid material ratio. And the ethanol concentration was 65%. The ionic liquid molar concentration was 0.3 mol/L (65% ethanol solution preparation). On the basis of these results, four significant factors (ultrasonic power, ultrasonic temperature, ultrasonic time and liquid material ratio) were screened out by Plackett-Burman experimental design. The extraction process was further optimized by response surface Box-Behnken experimental design. The optimum extraction process conditions of CBD significant factors were as follows: Ultrasonic power 280 W, ultrasonic temperature 50 ℃, ultrasonic time 62.5 min, liquid material ratio 25 mL/g. Under the above conditions, the yield of CBD extracted by ionic liquid [C₈mim]NTF₂ was 7.66%±0.2%, the yield of CBD extracted by methanol was 6.42%±0.3%, and the yield of CBD extracted by 65% ethanol solution was 5.81%±0.2%. The extraction ability of CBD was ionic liquid [C₈mim]NTF₂>methanol>65% ethanol solution. The CBD degradation experiment showed that the CBD degradation rate of ionic liquid [C₈mim]NTF₂ was 16.40%±0.3%, which was smaller than that of methanol (24.65%±0.6%) and 65% ethanol solution (32.88%±0.5%). The results showed that adding 65% ethanol solution into ionic liquid [C₈mim]NTF₂ could not only reduce the degradation rate of CBD, but also increase the yield of CBD. This study proved that ionic liquid was not only a protective agent for CBD, but also an excellent solvent for CBD extraction. The technology of extracting CBD by ionic liquid assisted ultrasonic method was developed, which provided data support for the development and utilization of industrial hemp CBD.
- industrial hemp leafs /
- cannabidiol (CBD) /
- ionic liquid /
- ultrasonic extraction /
- Plackett-Burman design /
- response surface

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图 1 各单因素对CBD得率的影响

Figure 1. Effect of each single factor on CBD yield

注：同一指标不同小写字母表示差异显著（P<0.05），图7、图8同。

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图 2 6因素对CBD得率影响的帕累托图

Figure 2. Pareto chart of the effects of six variables on CBD yield

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图 3 超声功率与超声温度交互作用对CBD得率的影响

Figure 3. Effect of interaction of ultrasonic power and ultrasonic temperature on CBD yield

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图 4 超声功率和超声时间交互作用对CBD得率的影响

Figure 4. Effect of interaction of ultrasonic power and ultrasonic time on CBD yield

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图 5 超声温度和超声时间交互作用对CBD得率的影响

Figure 5. Effect of interaction of ultrasonic temperature and ultrasonic time on CBD yield

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图 6 超声时间和液料比交互作用对CBD得率的影响

Figure 6. Effect of interaction of ultrasonic time and liquid material ratio on CBD yield

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图 7 不同溶剂提取对CBD得率的影响

Figure 7. Effect of different solvent extraction on CBD yield

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图 8 不同溶剂提取对CBD降解率的影响

Figure 8. Effect of different solvent extraction on CBD degradation rate

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表 1 因素与水平编码表

Table 1. Code of factors and levels

水平	因素
水平	A（W）	B（℃）	C（min）	D（%）	E（mol/L）	F（mL/g）
−1	200	30	40	55	0.1	15
+1	280	50	60	65	0.3	25

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表 2 因素与水平编码表

Table 2. Code of factors and levels

水平	因素
水平	X₁（W）	X₂（℃）	X₃（min）	X₄（mL/g）
−1	240	40	50	20
0	280	50	60	25
+1	320	60	70	30

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表 3 离子液体的筛选

Table 3. Screening of ionic liquids

序号	名称	CBD得率（%）	误差
1	[C₄mim]NTF₂	3.15	±0.11
2	[C₆mim]NTF₂	4.63	±0.13
3	[C₈mim]NTF₂	5.15	±0.14
4	[C₁₀mim]NTF₂	3.89	±0.10
5	[C₄mim]PF₆	4.31	±0.09
6	[C₆mim]PF₆	2.99	±0.05
7	[C₈mim]PF₆	3.23	±0.08
8	[C₁₀mim]PF₆	2.91	±0.05
9	[C₄mim]BF₄	4.43	±0.13
10	[C₆mim]BF₄	4.30	±0.10
11	[C₈mim]BF₄	3.90	±0.09
12	[C₁₀mim]BF₄	3.58	±0.07
13	[C₄mim]Br	3.19	±0.07
14	[C₆mim]Br	2.83	±0.04
15	[C₈mim]Br	3.62	±0.08
16	[C₁₀mim]Br	3.24	±0.08

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表 4 Plackett-Burman试验设计及响应值

Table 4. Plackett-Burman test design and results

试验号	A	B	C	D	E	F	Y₁（%）
1	−1	+1	+1	+1	−1	−1	5.65±0.17
2	−1	+1	−1	+1	+1	−1	4.53±0.19
3	+1	−1	+1	+1	−1	+1	6.76±0.22
4	−1	−1	+1	−1	+1	+1	6.00±0.11
5	+1	−1	−1	−1	+1	−1	4.40±0.15
6	+1	+1	+1	−1	−1	−1	7.26±0.16
7	−1	+1	+1	−1	+1	+1	7.26±0.15
8	+1	−1	+1	+1	+1	−1	7.08±0.14
9	−1	−1	−1	+1	−1	+1	4.38±0.05
10	−1	−1	−1	−1	−1	−1	3.21±0.06
11	+1	+1	−1	−1	−1	+1	6.96±0.14
12	+1	+1	−1	+1	+1	+1	6.81±0.13

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表 5 Plackett-Burman试验设计方差分析

Table 5. ANOVA of Plackett-Burman test design

变量	平方和	自由度	均方	F值	P 值	显著性
模型	20.54	6	3.42	17.59	0.0032	**
A	5.66	1	5.66	29.08	0.0030	**
B	3.67	1	3.67	18.88	0.0074	*
C	7.87	1	7.87	40.46	0.0014	**
D	1.2×10⁻³	1	1.2×10⁻³	6.167×10⁻³	0.9405
E	0.29	1	0.29	1.48	0.2778
F	3.04	1	3.04	15.62	0.0108	*
残差	0.97	5	0.19
总差	21.51	11
R²	0.9548
R²_Adj	0.9005
注：表示差异显著（P<0.05）；*表示差异极显著（P<0.01）；表7同。

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表 6 Box-Behnken设计方案及结果

Table 6. Design and results of Box-Behnken

试验号	水平编码				Y₁（%）
试验号	X₁	X₂	X₃	X₄	Y₁（%）
1	+1	0	−1	0	6.57±0.22
2	0	0	−1	−1	5.69±0.18
3	0	0	0	0	7.66±0.15
4	0	0	+1	+1	6.24±0.23
5	0	0	0	0	7.61±0.28
6	0	+1	0	+1	6.23±0.26
7	+1	+1	0	0	6.47±0.17
8	−1	0	+1	0	6.69±0.12
9	0	−1	−1	0	6.38±0.21
10	−1	0	0	−1	6.25±0.08
11	0	0	0	0	7.57±0.14
12	−1	0	−1	0	5.54±0.15
13	0	0	+1	−1	6.95±0.14
14	0	0	0	0	7.58±0.17
15	+1	0	0	+1	6.62±0.18
16	0	+1	+1	0	6.92±0.19
17	−1	−1	0	0	6.63±0.22
18	+1	0	0	−1	6.54±0.23
19	−1	+1	0	0	5.83±0.21
20	0	−1	0	−1	6.13±0.25
21	0	+1	−1	0	5.74±028
22	+1	−1	0	0	5.99±0.21
23	0	−1	0	+1	6.18±0.13
24	0	0	0	0	7.88±0.12
25	0	−1	+1	0	6.47±0.23
26	+1	0	+1	0	6.86±0.18
27	−1	0	0	+1	6.36±0.16
28	0	0	−1	+1	6.91±0.14
29	0	+1	0	−1	5.65±0.15

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表 7 方差分析结果

Table 7. ANOVA of test results

来源	平方和	自由度	均差	F值	P值	显著性
模型	11.01	14	0.79	21.60	< 0.0001	**
X₁	0.26	1	0.26	7.01	0.0191	*
X₂	0.074	1	0.074	2.02	0.1768
X₃	0.91	1	0.91	24.93	0.0002	**
X₄	0.15	1	0.15	4.05	0.0638
X₁X₂	0.41	1	0.41	11.25	0.0047	**
X₁X₃	0.18	1	0.18	5.08	0.0408	*
X₁X₄	2.25×10⁻⁴	1	2.25×10⁻⁴	6.181×10⁻³	0.9384
X₂X₃	0.30	1	0.30	8.16	0.0127	*
X₂X₄	0.070	1	0.070	1.93	0.1865
X₃X₄	0.93	1	0.93	25.58	0.0002	**
X₁²	2.44	1	2.44	66.94	< 0.0001	**
X₂²	4.46	1	4.46	122.51	< 0.0001	**
X₃²	1.87	1	1.87	51.32	< 0.0001	**
X₄²	3.07	1	3.07	84.33	< 0.0001	**
残差	0.51	14	0.036
失拟项	0.44	10	0.044	2.72	0.1739	不显著
纯误差	0.065	4	0.016
总离差	11.52	28
R²	0.9557
R²_Adj	0.9115

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