毛竹竹秆加压热水提取工艺优化及化学成分分析

doi:10.3969/j.issn.0253-2417.2023.04.015

摘要/Abstract

摘要：

以毛竹竹秆为原料，以毛竹竹秆提取物的干物质得率为优化指标，在单因素试验基础上，利用响应面法优化了竹秆加压热水提取工艺参数，得到较佳提取条件为4年生毛竹，提取温度165 ℃，提取时间30 min，料液比1∶12.5(g∶mL)。此条件下，毛竹竹秆提取物的干物质得率为12.44%，与预测值(12.56%)相近。采用气相色谱-质谱联用技术(GC/MS)检测了毛竹竹秆加压热水提取物和加热回流水提取物的化学组成，结果表明：鉴定出毛竹竹秆加压热水提取物化学组成成分23种(53.30%)，含量远高于加热回流水提取物的化学组成成分13种(27.90%)，其活性成分主要有松柏醛、香兰素、丁香醛、乙酰丁香酮、4-乙烯基-2-甲氧基苯酚、2, 3-二氢苯并呋喃和糠醛。

关键词: 毛竹竹秆, 加压热水提取, 响应面法, 干物质得率

Abstract:

Taking moso bamboo stalks as raw material and the dry matter yield of moso bamboo stalks extract as the optimization index, the response surface methodology was used to optimize the process parameters of pressurized hot water extraction of compounds from bamboo stalks. The optimum extraction conditions were as follows: 4-year-old moso bamboo, extraction temperature of 165 ℃, extraction time of 30 min, solid-liquid ratio of 1∶12.5. Under these conditions, the dry matter yield was 12.44%, which was close to the predicted value(12.56%). The chemical composition of the pressurized hot water extract and the heating reflux water extract of moso bamboo stem was detected by gas chromatography-mass spectrometry(GC/MS). The results of GC/MS analysis showed that the chemical composition(content of 53.30%) of 23 kinds of pressurized hot water extracts from bamboo stems was much higher than that of 13 kinds of heated reflux water extracts(27.90%), and mainly contained active ingredients such as coniferaldehyde, vanillin, syringaldehyde, acetosyringone, 4-vinyl-2-methoxyphenol, 2, 3-dihydrobenzofuran and furfural.

Key words: moso bamboo stalks, pressurized hot water extraction, response surface methodology(RSD), yield of dry matter

中图分类号:

TQ35

尤俊昊, 张保, 荀航, 姚曦, 王进, 汤锋. 毛竹竹秆加压热水提取工艺优化及化学成分分析[J]. 林产化学与工业, 2023, 43(4): 107-114.

Junhao YOU, Bao ZHANG, Hang XUN, Xi YAO, Jin WANG, Feng TANG. Optimization of Pressurized Hot Water Extraction Technology and Chemical Composition Analysis from Moso Bamboo Stalks[J]. Chemistry and Industry of Forest Products, 2023, 43(4): 107-114.

图/表 6

图1

表1

表2

图2

图3

表3

加压热水提取物和加热回流水提取物的化学成分"

编号 No.	保留时间/min retention time	化合物 compound	分子式 molecular formula	相对峰面积relative peak area/%
编号 No.	保留时间/min retention time	化合物 compound	分子式 molecular formula	加压热水提取 pressurized hot water extraction	加热回流水提取 heating reflux water extraction
1	3.65	羟基乙酸甲酯methyl glycolate	C₃H₆O₃	0.18	0.31
2	4.53	丙酮酸甲酯methyl pyruvate	C₄H₆O₃	1.56	—
3	5.16	糠醛furfural	C₅H₄O₂	1.00	—
4	8.06	苯酚phenol	C₆H₆O	0.41	—
5	11.19	愈创木酚guaiacol	C₇H₈O₂	0.40	0.28
6	15.61	2, 3-二氢苯并呋喃2, 3-dihydrobenzofuran	C₈H₈O	17.25	5.81
7	18.75	4-乙烯基-2-甲氧基苯酚2-vinyl-4-methoxyphenol	C₉H₁₀O₂	7.38	2.98
8	20.33	2, 6-二甲氧基苯酚2, 6-dimethoxyphenol	C₈H₁₀O₃	1.05	0.34
9	22.66	香兰素vanillin	C₈H₈O₃	1.66	—
10	24.78	异丁香酚isoeugenol	C₁₀H₁₂O₂	0.75	0.31
11	25.06	2-甲氧基-4-丙基-苯酚2-methoxy-4-ropylphenol	C₁₀H₁₄O₂	0.38	—
12	25.77	4-羟基-3-甲氧基苯丙酮4-hydroxy-3-methoxyphenylacetone	C₁₀H₁₂O₃	0.73	—
13	32.11	丁香醛syringaldehyde	C₉H₁₀O₄	3.85	0.28
14	33.42	(E)-2, 6-二甲氧基-4-(丙-1-烯-1-基)苯酚 phenol, 2, 6-dimethoxy-4-(1E)-1-propen-1-yl-	C₁₁H₁₄O₃	—	1.64
15	34.11	1-羟基-3-(4-羟基-3-甲氧基苯基)丙烷-2-酮 1-hydroxy-3-(4-hydroxy-3-methoxyphenyl)-2-propane-2-one	C₁₀H₁₂O₄	1.07	—
16	34.12	4-羟基-3-甲氧基苯乙酸甲酯 methyl 4-hydroxy-3-methoxyphenylacetate	C₁₀H₁₂O₄	0.64	—
17	34.27	乙酰丁香酮acetosyringone	C₁₀H₁₂O₄	1.26	—
18	34.42	松柏醛4-hydroxy-3-methoxycinnamaldehyde	C₁₀H₁₀O₃	1.88	—
19	34.6	4-((1E)-3-羟基-1-丙烯基)-2-甲氧基苯酚 4-((1E)-3-hydroxy-1-propenyl)- 2-methoxyphenol	C₁₀H₁₂O₃	—	1.33
20	35.4	3, 5-二甲氧基-4-羟基苯酰肼 3, 5-dimethoxy-4-hydroxyphenylhydrazide	C₉H₁₂N₂O₄	0.56	—
21	36.66	二苯基-2, 2′-二甲醛biphenyl-2, 2′-dicarboxaldehyde	C₁₄H₁₀O₂	1.09	—
22	36.84	肉豆蔻酸异丙酯isopropyl myristate	C₁₇H₃₄O₂	0.86	1.83
23	38.39	棕榈酸甲酯methyl palmitate	C₁₇H₃₄O₂	—	1.30
24	38.80	二苯基乙酸甲酯methyl diphenylacetate	C₁₅H₁₄O₂	4.16	—
25	39.14	4-[(1E)-3-羟基-1-丙烯基]-2, 6-二甲氧基苯酚 4-[(1E)-3-hydroxy-1-propenyl]- 2, 6-dimethoxyphenol	C₁₁H₁₄O₄	5.02	8.90
26	39.32	反式-3, 5-二甲氧基-4-羟基肉桂醛 (E)-3-(4-hydroxy-3, 5-dimethoxyphenyl) acrylaldehyde	C₁₁H₁₂O₄	0.18	2.59

表3

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编号 No.	X₁ 竹龄/a bamboo age	X₂ 提取温度/℃ extraction temperature	X₃ 提取时间/min extraction time	X₄ 料液比(g∶mL) solid-liquid ratio	Y 干物质得率/% dry matter yield
1	3	155	30	1∶12.5	4.80±0.63
2	3	155	20	1∶10	5.88±0.22
3	3	165	20	1∶12.5	4.26±0.09
4	3	165	20	1∶7.5	6.72±0.45
5	2	155	20	1∶12.5	5.82±0.45
6	2	155	20	1∶7.5	11.70±0.46
7	2	155	10	1∶10	6.93±0.20
8	3	155	10	1∶7.5	7.14±0.36
9	3	145	10	1∶10	7.38±0.72
10	4	145	20	1∶10	6.24±0.02
11	2	155	30	1∶10	5.22±0.36
12	3	155	30	1∶7.5	4.98±0.48
13	4	155	20	1∶12.5	5.04±0.32
14	2	165	20	1∶10	6.84±0.87
15	3	155	20	1∶10	4.44±0.79
16	4	155	10	1∶10	9.60±0.29
17	3	145	20	1∶12.5	10.62±0.49
18	3	155	20	1∶10	5.31±0.05
19	3	155	10	1∶12.5	4.44±0.02
20	2	145	20	1∶10	6.18±0.57
21	3	145	20	1∶7.5	8.94±0.81
22	3	165	10	1∶10	6.33±0.02
23	3	165	30	1∶10	5.40±0.07
24	3	145	30	1∶10	4.68±0.34
25	4	155	30	1∶10	5.28±0.43
26	4	165	20	1∶10	5.70±0.17
27	4	155	20	1∶7.5	6.06±0.07

方差来源source of variation	平方和SS	自由度df	均方MS	F值F value	P值P value
模型model	83.05	14	5.93	7.6	0.000 6
X₁	1.43	1	1.43	1.83	0.201 2
X₂	49.09	1	49.09	62.86	< 0.000 1
X₃	6.53	1	6.53	8.36	0.013 5
X₄	0.39	1	0.39	0.5	0.493 9
X₁X₂	0.051	1	0.051	0.065	0.803 3
X₁X₃	1.37	1	1.37	1.75	0.210 1
X₁X₄	0.95	1	0.95	1.22	0.291 5
X₂X₃	3.24	1	3.24	4.15	0.064 3
X₂X₄	0.022	1	0.022	0.029	0.868 0
X₃X₄	0.19	1	0.19	0.24	0.631 4
X₁²	13.34	1	13.34	17.08	0.001 4
X₂²	3.65	1	3.65	4.68	0.051 5
X₃²	0.012	1	0.012	0.015	0.903 3
X₄²	0.41	1	0.41	0.53	0.480 3
残差residual	9.37	12	0.78
失拟项lock of fit	9.23	10	0.92	13.5	0.070 9
纯误差pure error	0.14	2	0.068
总和cor total	92.42	26

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