棉籽壳中除草活性物质提取及鉴定

张城嘉; 李祖任; 柏连阳

doi:10.16801/j.issn.1008-7303.2019.0022

棉籽壳中除草活性物质提取及鉴定

doi: 10.16801/j.issn.1008-7303.2019.0022

张城嘉^{1, 2,},
李祖任^{1, 2},
柏连阳^{1, 2, ,}

1.
湖南农业大学植物保护学院，长沙 410128
2.
湖南省农业科学院湖南省农业生物技术研究所杂草生物学及安全防控湖南省重点实验室，长沙 410125

基金项目: 国家自然科学基金(31801754)；湖南省自然科学基金(2018JJ3289)

详细信息

作者简介:
张城嘉，男，硕士研究生，E-mail：531464470@qq.com

通讯作者:
柏连阳，通信作者(Author for correspondence)，男，教授，主要从事杂草防控研究，E-mail：bailianyang2005@aliyun.com

中图分类号: S482.1
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- 被引次数: 0
出版历程
- 收稿日期: 2019-01-31
- 录用日期: 2019-03-15
- 刊出日期: 2019-04-01

Extraction and identification of herbicidal active substances in cottonseed hulls

ZHANG Chengjia^{1, 2
,},
LI Zuren^{1, 2},
BAI Lianyang^{1, 2
, ,}

1.
College of Plant Protection, Hunan Agricultural University, Changsha 410128, China
2.
Hunan Provincial Key Laboratory for Biology and Control of Weeds, Hunan Agricultural Biotechnology Research Institute, Hunan Academy of Agricultural Sciences, Changsha 410125, China

摘要

摘要: 为了开发利用棉籽壳中的除草活性物质，分别以无水乙醇、正丁醇、石油醚和乙酸乙酯为溶剂，采用索氏提取法对棉籽壳中的活性物质进行了提取，并对各溶剂粗提物进行了除草活性测定。结果发现：用无水乙醇提取的粗提物对稗草生长的抑制活性最高，经气相色谱-质谱(GC-MS)联用分析，发现该粗提物中主要含有甘油、三环己基3-烯-6-辛酮、4-乙烯基-2-甲氧基苯酚、(邻甲基苯酚)-2-溴-2氯-乙酰酯、十四酸、十四酸乙酯、十六烷酸、辛酸异戊酯和亚油酸9种化合物。进一步的除草活性测定结果表明，亚油酸、辛酸异戊酯、4-乙烯基-2-甲氧基苯酚和(邻甲基苯酚)-2-溴-2氯-乙酰酯4种化合物对稗草表现出一定的除草活性，其中亚油酸活性最强，其IC₅₀值为14.5 mg/L。
- 棉籽壳 /
- 提取与鉴定 /
- 除草活性 /
- 稗草 /
- 气相色谱-质谱联用 /
- 亚油酸
Abstract: In order to investigate the potential application of the herbicidal active substances in the cottonseed hull, the herbicidal active substances of the cotton husk was extracted by Soxhlet extraction using anhydrous ethanol, n-butanol, petroleum ether and ethyl acetate were selected. The activities of the crude extracts were determined. It was found that anhydrous ethanol was the best solvent for the extraction of the active ingredients from cottonseed hull which could inhibit Echinochloa crusgalli (L.) Beauv.. Based on the gas chromatography-mass spectrography(GC-MS)analysis, 9 main compounds in the ethanol extract of cottonseed hull were detected, including glycerol, tricyclohexyl 3-ene-6-octanone, 4-vinyl-2-methoxyphenol, (o-methylphenol) 2-bromo-2-chloroacetyl ester, myristic acid, ethyl myristate, palmitic acid, isoamyl octanoate and linoleic acid. Further herbicidal activity assays showed that linolenic acid, isoamyl octanoate, 4-vinyl-2-methoxyphenol, and myristic acid were the main components in cottonseed hull extract with certain herbicidal activities. Linoleic acid has the highest inhibitory effect against E. crusgalli, with the IC₅₀ value for the inhibition of the growth of E. crusgalli was 14.5 mg/L.
- cottonseed hull /
- extraction and identification /
- herbicidal activity /
- Echinochloa crusgalli /
- gas chromatography-mass spectrography /
- linoleic acid

HTML全文

图 1 无水乙醇粗提物的气相色谱-质谱总离子流图

Figure 1. The total lon chromatography of the ethanol extracts of cottonseed hulls from GC-MS chromatogram

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表 1 不同溶剂粗提物对稗草的除草活性

Table 1. Herbicidal activities of the extracts obtained using four organic solvents against Echinochloa crusgalli

粗提物 Extract	回归方程 Regression equation	IC₅₀ 值 IC₅₀ value/(g/L)	95% 置信限 95% Confidence limit/(g/L)	相关系数 Correlation coefficient, r
无水乙醇粗提物 Ethanol extract	y = 4.231 4 + 1.450 2x	3.38	2.88~3.97	0.990 0
正丁醇粗提物 n-Butanol extract	y = 4.274 6 + 0.880 4x	6.66	4.96~8.95	0.973 3
石油醚粗提物 Petroleum ether extract	y = 3.884 2 + 0.699 8x	39.3	26.1~59.2	0.989 6
乙酸乙酯粗提物 Ethyl acetate extract	y = 4.048 3 + 0.735 6x	19.7	13.1~29.5	0.982 2

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表 2 棉籽壳无水乙醇粗提物主要化合物GC-MS联用鉴定结果

Table 2. Results of the GC-MS analysis of cottonseed hulls ethanoli extracts

峰号 Peaks	保留时间 Retention time/min	分子式 Molecular formula	相对分子质量 Molecular weight	相对含量(体积分数)/% Relative content(%V)	比对后化合物名称 Chemical compound after comparison
1	9.190	C₃H₈O₃	92	1.77	甘油 glycerol
2	12.125	C₁₁H₁₂O₃	192	0.03	三环己基-3-烯-6-辛酮 tricyclohexyl 3-ene-6-octanone
3	13.545	C₉H₁₀O₂	150	0.05	4-乙烯基-2-甲氧基苯酚 4-vinyl-2-methoxyphenol
4	16.246	C₁₀H₈BrClO₃	290	0.15	(邻甲基苯酚)-2-溴-2氯-乙酰酯 (o-methylphenol)-2-bromo-2-chloroacetyl ester
5	17.567	C₁₄H₂₈O₂	228	0.33	十四酸 tetradecanoic acid
6	19.531	C₁₆H₃₂O₂	256	0.07	十四酸乙酯 ethyl myristate
7	19.938	C₁₆H₃₂O₂	256	28.24	十六烷酸 hexadecanoic acid
8	20.731	C₁₃H₂₆O₂	214	0.13	辛酸异戊酯 isoamyl octanate
9	22.675	C₁₈H₃₂O₂	280	69.23	亚油酸 linoleic acid

下载: 导出CSV

表 3 无水乙醇粗提物中主要化合物对稗草的除草活性

Table 3. Herbicidal activities of major compounds in the ethanol extract against E. crusgalli

化合物 Compound	回归方程 Regression equation	IC₅₀ 值 IC₅₀ value/(mg/L)	95% 置信限 95% Confidence limit/ (mg/L)	相关系数 Correlation coefficient, r
亚油酸 linoleic acid	y = 3.269 6 + 1.491 5x	14.5	12.9~16.2	0.995 5
辛酸异戊酯 isoamyl octanate	y = 3.338 9 + 1.039 4x	39.7	31.6~49.7	0.986 3
4-乙烯基-2-甲氧基苯酚 4-vinyl-2-methoxyphenol	y = 3.378 9 + 0.900 5x	63.1	46.1~86.5	0.983 4
(邻甲基苯酚)-2-溴-2氯-乙酰酯 (o-methylphenol) -2-bromo-2-chloroacetyl ester	y = 3.277 6 + 0.928 2x	71.7	49.5~104	0.979 8
氰氟草酯 cyhalofop-butyl	y = 4.686 6 + 1.371 7x	1.69	1.51~1.89	0.995 2

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棉籽壳中除草活性物质提取及鉴定

doi: 10.16801/j.issn.1008-7303.2019.0022

作者简介:
张城嘉，男，硕士研究生，E-mail：531464470@qq.com

通讯作者:
柏连阳，通信作者(Author for correspondence)，男，教授，主要从事杂草防控研究，E-mail：bailianyang2005@aliyun.com

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Extraction and identification of herbicidal active substances in cottonseed hulls

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留言板

棉籽壳中除草活性物质提取及鉴定

doi: 10.16801/j.issn.1008-7303.2019.0022

作者简介: 张城嘉，男，硕士研究生，E-mail：531464470@qq.com

通讯作者: 柏连阳，通信作者(Author for correspondence)，男，教授，主要从事杂草防控研究，E-mail：bailianyang2005@aliyun.com

计量

出版历程

Extraction and identification of herbicidal active substances in cottonseed hulls

计量

出版历程

目录

作者简介:
张城嘉，男，硕士研究生，E-mail：531464470@qq.com

通讯作者:
柏连阳，通信作者(Author for correspondence)，男，教授，主要从事杂草防控研究，E-mail：bailianyang2005@aliyun.com