亚临界R134a萃取樟树叶精油的工艺优化及抑菌研究

doi:10.3969/j.issn.0253-2417.2023.06.009

Abstract

Abstract:

In order to study the efficient extraction technology of camphor tree essential oil and broaden its application range, the subcritical extraction of essential oil from Cinnamomum camphora leaves was optimized by orthogonal design experiment with 1, 1, 1, 2-tetrafluoroethane(R134a) as extraction solvent. The differences in chemical compositions and antimicrobial activity of essential oil from C. camphora leaves extracted by subcritical R134a extraction and the traditional steam extraction were compared. The results showed that the optimal parameters for subcritical R134a extraction of essential oil from C. camphora leaves were as follows: the particle size of the raw material obtained by crushing with 2 mm aperture sieve, the solid-liquid ratio of 6:1(L: kg), the extraction temperature of 45 ℃, the extraction time of 40 min/times, and the extraction for 4 times. Under this condition, the extraction ratio of essential oil was(2.87±0.08)%. GC-MS analysis of the two leaves essential oils obtained from steam extraction and subcritical R134a extraction identified 39 and 35 compounds, with the relative total peak areas of 99.97% and 99.91%, respectively. The chemical components of the two leaves essential oils were mainly alcohols and hydrocarbons, and borneol was the main chemical component in the essential oils. The relative peak area of borneol in steam extraction essential oil(64.29%) was greater than that of subcritical R134a-extracted essential oil(58.09%). The two kinds of leaves essential oils from leaves had different degrees of antimicrobial effect on plant pathogens. The antimicrobial activity of leaves essential oil extracted by subcritical R134a extraction on pathogenic fungi was better than that of essential oil extracted by steam extraction. The two essential oils from leaves had the highest antimicrobial rate against Phytophthora capsici, which were 71.74% and 62.87%, respectively.

Key words: Cinnamomum camphora leaf essential oil, R134a, subcritical fluid extraction, orthogonal optimization, GC-MS analysis, bacteriostasis

CLC Number:

TQ35

Shan HU, Weiqu LIANG, Peiwu XIE, Huajian LUO, Huiming LIAN, Hao HUANG. Processing Optimization and Bacteriostasis of Cinnamomum camphora Leaves Essential Oil by Subcritical R134a Extraction[J]. Chemistry and Industry of Forest Products, 2023, 43(6): 65-73.

Figures/Tables 7

Table 1

Fig.1

Table 2

Table 3

Fig.2

Table 4

GC-MS analysis results of C.camphora leaf essential oil"

序号 No.	保留时间/min retention time	化合物 compound	相对峰面积relative peak area/%		匹配度/% matching degree
序号 No.	保留时间/min retention time	化合物 compound	水蒸气提取 steam extraction	亚临界R134a萃取 subcritical R134a extraction	匹配度/% matching degree
1	4.471	α-侧柏烯α-thujene	0.17	—	95
2	4.659	α-蒎烯α-pinene	1.82	0.04	97
3	5.05	莰烯camphene	1.40	0.04	96
4	5.584	桧烯sabinene	1.31	—	95
5	5.742	(-)-β-蒎烯(-)-β-pinene	1.14	0.05	96
6	5.942	β-月桂烯β-myrcene	0.93	0.08	94
7	6.53	β-水芹烯β-phellandrene	0.22	—	95
8	6.862	3-蒈烯3-carene	0.02	—	94
9	7.114	(+)-4-蒈烯(+)-4-carene	0.49	—	95
10	7.1	对伞花烃p-cymene	0.36	0.09	95
11	7.267	D-柠檬烯D-limonene	2.50	0.39	95
12	7.814	顺式-β-罗勒烯cis-β-ocimene	0.06	—	95
13	8.307	γ-萜品烯γ-terpinene	0.29	—	97
14	26.088	β-榄香烯β-elemene	0.09	0.28	94
15	27.806	石竹烯caryophyllene	1.37	4.66	96
16	29.976	α-石竹烯α-caryophyllene	1.21	4.65	95
17	31.126	γ-芹子烯γ-selinene	—	0.09	92
18	31.552	大根香叶烯D germacrene D	1.11	2.78	92
19	32.007	β-瑟林烯β-eudesmene	0.07	—	93
20	32.446	大根香叶烯B germacrene B	0.55	—	91
21	33.922	δ-杜松烯δ-cadinene	0.05	0.27	92
22	36.12	γ -榄香烯γ-elemene	0.37	0.92	91
23	37.479	氧化石竹烯caryophyllene oxide	0.31	1.12	93
24	39.11	环氧化蛇麻烯II humulene epoxide II	0.16	0.90	90
25	32.009	4(14), 11-桉叶二烯eudesma-4(14), 11-diene	—	1.76	94
26	32.199	(+)-喇叭烯(+)-ledene	—	0.26	93
27	32.451	异丁子香烯isocaryophillene	—	2.99	93
28	33.102	8-异丙烯基-1, 5-二甲基-1, 5-二烯-环葵烷 8-isopropenyl-1, 5-dimethyl-cyclodeca-1, 5-diene	0.06	0.23	93
29	33.915	菖蒲烯(-)-calamenene	—	0.23	90
30	7.38	桉叶油醇eucalyptol	6.42	1.58	90
31	8.782	顺式-β-松油醇cis-β-terpineol	0.32	0.49	93
32	9.974	芳樟醇linalool	0.21	0.17	92
33	11.16	反式-4-异丙基-1-甲基环己-2-烯-1-醇 trans-1-methyl-4-(1-methylethyl)-2-cyclohexen-1-ol	0.08	—	93
34	13.705	龙脑borneol	64.29	58.09	96
35	13.968	松油烯-4-醇terpinen-4-ol	1.55	0.86	95
36	14.73	α-松油醇α-terpineol	3.86	2.84	96
37	15.561	反式辣薄荷醇trans-piperitol	0.05	—	94
38	16.394	橙花醇nerol	0.12	—	94
39	37.288	6-芹子烯-4-醇selina-6-en-4-ol	—	0.31	93
40	40.596	桉油烯醇spathulenol	0.27	3.34	95
41	12.159	樟脑camphor	2.11	4.02	97
42	41.958	杜松脑juniper camphor	0.14	0.49	89
43	45.945	蒿酮artemisia ketone	0.93	1.03	89
44	49.367	植物酮hexahydrofarnesyl acetone	—	0.09	90
45	50.678	法尼基丙酮farnesyl acetone	—	0.05	88
46	19.686	乙酸龙脑酯bornyl acetate	2.42	4.26	96
47	36.613	乙酸橙花叔醇酯nerolidyl acetate	1.14	0.46	93

Table 4

Table 5

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粉碎方式 comminution method	筛网孔径/mm mesh size	得率¹⁾/% yield
粗碎coarse crushing	5	0.83±0.07^a
粗碎coarse crushing	3	1.43±0.08^b
粉碎crushing	3	2.40±0.06^d
粉碎crushing	2	2.60±0.07^e
粉碎crushing	1	2.18±0.09^c

序号 No.	A 萃取温度/℃ extraction temperature	B 萃取时间/min extraction time	C 萃取次数/times extraction times	得率/% yield
1	40	30	2	1.93
2	40	40	3	2.69
3	40	50	4	2.73
4	45	30	3	2.54
5	45	40	4	2.82
6	45	50	2	2.06
7	50	30	4	2.51
8	50	40	2	2.10
9	50	50	3	2.63
k₁	2.45	2.33	2.03
k₂	2.47	2.54	2.62
k₃	2.41	2.47	2.69
R	0.06	0.21	0.66

差异来源 difference source	Ⅲ型平方和 type Ⅲ sum of squares	自由度 df	均方 mean square	F	P	显著性 significance
A	0.005	2	0.003	1.857	0.350
B	0.070	2	0.035	23.556	0.041	*
C	0.784	2	0.392	265.180	0.004	**
误差error	0.003	2	0.001

植物病原真菌 plant pathogenic fungi	菌落直径fungi colony diameter/cm				抑菌率antibacterial rate/%
植物病原真菌 plant pathogenic fungi	对照 control	2%吐温 2% tween	水蒸气提取 steam extraction	亚临界R134a萃取 subcritical R134a extraction	水蒸气提取 steam extraction	亚临界R134a萃取 subcritical R134a extraction
辣椒疫霉病菌 Phytophthora capsici	8.60±0.00	8.60±0.00	2.43±0.18	3.19±0.06	62.87	71.74
香蕉枯萎病菌 Fusarium oxysporum	8.60±0.00	8.47±0.06	4.82±0.34	6.54±0.08	23.95	43.99
冬瓜枯萎病菌 F. oxysporum(Schl.)	7.51±0.17	7.49±0.14	3.97±0.18	6.08±0.04	18.96	47.16
水稻稻瘟病菌 Magnaporthe oryzae	8.60±0.00	8.60±0.00	4.10±0.39	5.55±0.49	35.47	52.29
西瓜炭疽病菌 Colletorichum orbiculare	8.60±0.00	8.60±0.00	4.68±0.09	5.99±0.25	30.31	52.27
甘蔗赤腐病菌 C. falcatum	8.60±0.00	8.60±0.00	4.11±0.08	5.16±0.14	39.96	52.21
玉米小斑病菌 Bipolaris maydis	8.60±0.00	8.26±0.28	4.62±0.12	5.20±0.01	39.50	46.28
苹果轮纹病菌 Physalospora piricola	8.60±0.00	8.60±0.00	4.88±0.18	8.60±0.00	0.00	43.22
花生褐斑病菌 Cercospora arachidicola	6.75±0.08	6.72±0.09	3.51±0.17	2.55±0.27	47.92	62.25

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Processing Optimization and Bacteriostasis of Cinnamomum camphora Leaves Essential Oil by Subcritical R134a Extraction

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