桑叶乙醇提取物化学成分分析及提取工艺优化

doi:10.3969/j.issn.0253-2417.2023.01.015

摘要/Abstract

摘要：

对桑叶无水乙醇和体积分数70%乙醇提取物的组分进行GC-MS分析，以桑叶提取物得率为指标，考察了乙醇体积分数、提取温度、提取时间对桑叶乙醇提取物得率的影响, 并运用响应面法优化桑叶乙醇提取物水浴加热的提取工艺。研究结果表明：桑叶无水乙醇提取物中共鉴定出9种化合物，70%乙醇提取物中共鉴定出19种化合物。无水乙醇提取物中有机物GC含量从高到低分别为醇类(24.78%)、芳烃类(24.57%)、烷烃类(23.72 %)、氨基脲(0.68%)，GC含量最高的化合物为α, β-二甲基苯乙醇(24.78%)。70%乙醇提取物中有机物GC含量从高到低分别为酯类(32.99%)、烷烃类(24.35%)、酮类(9.57%)、酸类(7.07%)、腈类(0.52%)、醇类(0.45%)，GC含量最高的化合物为苯甲酸-2, 5-二(三甲基甲硅烷氧基)-三甲基甲硅烷基酯(20.01%)。桑叶乙醇提取物的最佳提取条件为：5 g桑叶粉，50 mL乙醇溶液，乙醇体积分数66%，提取温度85 ℃，提取时间182 min，此条件下桑叶乙醇提取物的得率为20.0%。

关键词: 桑叶, 水浴加热法, GC-MS, 响应面法优化

Abstract:

The components of absolute ethanol and 70%(volume fraction) ethanol extracts of mulberry leaves were analyzed by GC-MS. On this basis, taking the yield of mulberry leaf extract as the index, the effects of ethanol volume fraction, extraction temperature and extraction time on the yield of mulberry leaf ethanol extract were investigated, and the extraction process of mulberry leaf ethanol water bath heating extract was optimized by response surface methodology. The results showed that 9 kinds of substances were identified in the absolute ethanol extract of mulberry leaves, and 19 kinds of substances were identified in 70% ethanol extract. From high to low, the organic matter contents in anhydrous ethanol extract were alcohols of 24.78%, aromatics of 24.57%, alkanes of 23.72% and aminourea of 0.68%. The compound with the highest content was α, β-dimethyl phenylethanol(24.78%). The organic matter content in 70% ethanol extract was composed of esters(32.99%), alkanes(24.35%), ketones(9.57%), acids(7.07%), nitriles(0.52%) and alcohols(0.45%) from high to low. The compound with the highest content was benzoic acid-2, 5-bis(trimethylsiloxy)-trimethylsilyl ester(20.01%). The optimum extraction conditions of ethanol extract from mulberry leaves were 5 g of mulberry leaf powder, 50 mL of ethanol solution, ethanol volume fraction of 66%, extraction temperature of 85 ℃ and extraction time of 182 min. Under these conditions, the yield of ethanol extract from mulberry leaves was 20.0%.

Key words: mulberry leaves, water bath heating method, GC-MS, response surface methodology

中图分类号:

TQ35
TQ91

付佳, 吴禹践, 刘志明, 王海英. 桑叶乙醇提取物化学成分分析及提取工艺优化[J]. 林产化学与工业, 2023, 43(1): 120-126.

Jia FU, Yujian WU, Zhiming LIU, Haiying WANG. Chemical Constituents Analysis and Process Optimization of Ethanol Extract from Mulberry Leaves[J]. Chemistry and Industry of Forest Products, 2023, 43(1): 120-126.

图/表 6

表1

表2

桑叶70%乙醇提取物的GC-MS分析"

序号 No.	保留时间/min retention time	化合物 compound	分子式 molecular	GC含量/% GC content	匹配度/% matching degree
1	3.835	环乙烯巯基-5.α-雄甾烷-16-酮 cyclic ethylene mercaptole-5.α-androstan-16-one	C₂₁H₃₄S₂	0.10	62.70
2	5.755	α, β-二甲基苯乙醇 α, β-dimethyl phenylethanol	C₁₀H₁₄O	0.45	84.40
3	6.853	1, 2-环戊二酮 1, 2-cyclopentanedione	C₅H₆O₂	0.28	77.70
4	7.967	双(三甲基硅基)醚-2'，6'-二羟基苯乙酮 bis(trimethylsilyl) ether-2', 6'-dihydroxyacetophenone	C₁₄H₂₄O₃Si₂	9.19	85.70
5	8.575	四甲基丁腈 tetramethylbutanedinitrile	C₈H₁₂N₂	0.52	78.90
6	9.658	十一烷 undecane	C₁₁H₂₄	0.18	78.60
7	10.475	苯甲酸-2, 5-二(三甲基甲硅烷氧基)-三甲基甲硅烷基酯 benzoic acid-2, 5-bis(trimethylsiloxy)-, trimethylsilyl ester	C₁₈H₂₅N₃OSi₂	20.01	73.40
8	11.19	6-甲基-十三烷 6-methyl-tridecane	C₁₄H₃₀	0.28	73.50
9	12.961	十二甲基环己硅氧烷dodecamethyl-cyclohexasiloxane	C₁₂H₃₆O₆Si₆	8.57	94.30
10	17.028	3-三氟甲基苯甲酸-4-十六酯 3-trifluoromethylbenzoic acid-4-hexadecyl ester	C₂₄H₃₇F₃O₂	0.33	65.50
11	17.203	[[4-[1, 2-双[(三甲基硅基)氧基]乙基]-1, 2-亚苯基]双(氧基)]双[三甲基]-硅烷 [[4-[1, 2-bis[(trimethylsilyl)oxy]ethyl]-1, 2-phenylene]bis(oxy)]bis[trimethyl]-silane	C₂₀H₄₂O₄Si₄	4.12	70.70
12	18.936	1, 1, 1, 5, 7, 7, 7-七甲基-3, 3-双(三甲基硅氧基)-四硅氧烷 1, 1, 1, 5, 7, 7, 7-heptamethyl-3, 3-bis(trimethylsiloxy)-tetrasiloxane	C₁₃H₄₀O₅Si₆	5.66	69.10
13	19.282	十五酸 pentadecanoic acid	C₁₅H₃₀O₂	0.34	83.30
14	19.453	1, 2-苯二甲酸丁辛酯 1, 2-benzenedicarboxylic acid-butyl octyl ester	C₂₀H₃₀O₄	0.15	76.20
15	20.289	正十六酸 n-hexadecanoic acid	C₁₆H₃₂O₂	6.26	96.10
16	20.483	1, 1, 3, 3, 5, 5, 7, 7, 9, 9, 11, 11, 13, 13-十四甲基-七硅氧烷 1, 1, 3, 3, 5, 5, 7, 7, 9, 9, 11, 11, 13, 13-tetradecamethyl-heptasiloxane	C₁₄H₄₄O₆Si₇	5.54	74.90
17	21.905	苯乙酸-α，3, 4-三[(三甲基硅基)氧]-三甲基硅基酯 benzeneacetic acid-α, 3, 4-tris[(trimethylsilyl)oxy]-trimethylsilyl ester	C₂₀H₄₀O₅Si₄	5.79	69.30
18	22.175	十八酸 octadecanoic acid	C₁₈H₃₆O₂	0.47	80.40
19	26.580	苯甲酸-2, 5-二(三甲基硅氧基)-三甲基硅基酯 benzoic acid-2, 5-bis(trimethylsiloxy)- trimethylsilyl ester	C₁₆H₃₀O₄Si₃	6.71	61.10

表2

表3

表4

表5

图1

参考文献 21

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序号 No.	保留时间/min retention time	化合物 compound	分子式 molecular	GC含量/% GC content	匹配度/% matching degree
1	3.843	1, 2-15, 16-二环氧十六烷 1, 2-15, 16-diepoxyhexadecane	C₁₆H₃₀O₂	6.57	71.90
2	5.755	α, β-二甲基苯乙醇 α, β-dimethyl phenylethanol	C₁₀H₁₄O	24.78	83.40
3	6.170	对二甲苯 p-xylene	C₈H₁₀	10.23	69.80
4	8.013	1-(乙烯氧基)-十八烷 1-(ethenyloxy)-octadecane	C₂₀H₄₀O	3.06	66.30
5	8.123	1-(3, 5-二甲基-1-金刚烷基)氨基脲 1-(3, 5-dimethyl-1-adamantanoyl)semicarbazide	C₁₄H₂₃N₃O₂	0.68	62.90
6	8.899	1, 2-二乙苯 1, 2-diethyl-benzene	C₁₀H₁₄	10.31	83.00
7	9.001	1, 4-二乙苯 1, 4-diethyl-benzene	C₁₀H₁₄	4.03	83.60
8	9.659	十一烷 undecane	C₁₁H₂₄	11.08	71.10
9	11.194	6-甲基十八烷 6-methyl-octadecane	C₁₉H₄₀	3.01	71.30

条件 condition		得率/% yield
乙醇体积分数 ethanol volume fraction	60%	12.47
	70%	15.87
	80%	11.40
	90%	12.07
提取温度 extraction temperature	55 ℃	9.87
	65 ℃	11.20
	75 ℃	15.87
	85 ℃	18.40
提取时间 extraction time	1 h	8.66
	2 h	9.80
	3 h	11.20
	4 h	11.20

方差来源 source of variance	平方和 sum of squares	自由度 degree of freedom	均方 mean square	F值 F value	P值 P value	显著性 significance
模型 model	139.62	9	15.51	53.71	< 0.000 1	**
X₁	18.61	1	18.61	64.41	< 0.000 1	**
X₂	72.00	1	72.00	249.26	< 0.000 1	**
X₃	0.005	1	0.005	0.017	0.899 0
X₁X₂	3.61	1	3.61	12.50	0.009 5	**
X₁X₃	2.56	1	2.56	8.86	0.020 6	*
X₂X₃	0.25	1	0.25	0.87	0.383 2
X₁²	38.40	1	38.40	132.94	< 0.000 1	**
X₂²	0.003 8	1	0.003 8	0.013	0.912 0
X₃²	2.83	1	2.83	9.80	0.016 6	*
残差 residual	2.02	7	0.29
失拟 lack of fit	0.47	3	0.16	0.40	0.758 9
误差 pure error	1.55	4	0.39
总计 cor total	141.64	16

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