油茶壳杀黏虫活性成分鉴定及其作用机制

doi:10.3864/j.issn.0578-1752.2025.13.008

Abstract

Abstract:

【Objective】 The objective of this study is to clarify the insecticidal active component and mechanism of Camellia oleifera shell on Mythimna separate, and to provide a basis for the development of botanical insecticides for M. separata. 【Method】 The insecticidal activity of petroleum ether, chloroform, ethyl acetate, and aqueous extracts of C. oleifera shell against 3rd instar larvae of M. separata was evaluated using the immersion and leaf-dipping methods. The petroleum ether extract was subjected to silica gel column chromatography for separation, followed by gas chromatography-mass spectrometry (GC-MS) analysis to identify the active components. Furthermore, a non-targeted metabolomics approach was employed to annotate, screen, and analyze differential metabolites in M. separata. 【Result】 The petroleum ether extract of C. oleifera shell exhibited the highest contact toxicity against M. separata, with LC₅₀values of 9.53, 8.00, 7.51, and 7.02 mg·mL^-1 on 1, 3, 5, and 7 d, respectively. The petroleum ether extract was separated by silica gel column chromatography to obtain 20 fractions, among which fraction 6 showed the best contact toxicity against M. separata, with LC₅₀ values of 3.99, 3.85, 3.72, and 3.72 mg·mL^-1 on 1, 3, 5, and 7 d, respectively. Further separation of fraction 6 yielded 21 subfractions, with subfraction 6.4 demonstrating the highest contact toxicity. GC-MS analysis identified hexadecane (19.33%), 1-hexadecene (14.21%), octacosane (4.03%), octadecane (9.24%), dichlorochrysanthemic acid (6.73%), 1-octadecene (7.27%), 1-tetracosanol (3.87%) and isophytol (5.92%) as the main compounds. Among these, dichlorochrysanthemic acid exhibited the strongest contact toxicity against M. separata, with LC₅₀ values of 91.62, 55.61, 34.94, and 24.43 μg·mL^-1 on 1, 3, 5, and 7 d, respectively. Its insecticidal efficacy was comparable to that of the positive control, pyrethrin. Non-targeted metabolomics analysis identified six differential metabolites, among which piceid, cannabinoid, 5-fluoro-cannabinoid metabolite, and caproylglycine were significantly upregulated, while 4-ethyl-2,6-dihydroxyphenyl sulfate and N-pentacosanoylglycine were significantly downregulated. These differential metabolites were primarily enriched in four metabolic pathways: cofactor biosynthesis, tryptophan metabolism, niacin and nicotinamide metabolism, ubiquinone and terpenoid-quinone biosynthesis. 【Conclusion】 Dichlorochrysanthemic acid from C. oleifera shell extract exhibits insecticidal activity against M. separata, providing a new avenue for the biological control of M. separata and the high-value utilization of C. oleifera shell.

Key words: Camellia oleifera shell, Mythimna separata, contact toxicity, dichlorochrysanthemic acid, metabolomics

ZHAN Li, LIANG ZongSuo, YU Jing, LU Jun, LIANG Qian. Insecticidal Active Component Identification of Camellia oleifera Shell Against Mythimna separata and Its Action Mechanism[J].Scientia Agricultura Sinica, 2025, 58(13): 2591-2603.

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References 46

[1]	XIAO X M, HE L M, CHEN Y Y, WU L H, WANG L, LIU Z P. Anti-inflammatory and antioxidative effects of Camellia oleifera Abel components. Future Medicinal Chemistry, 2017, 9(17): 2069-2079.
[2]	ZHANG F H, LI Z, ZHOU J Q, GU Y Y, TAN X F. Comparative study on fruit development and oil synthesis in two cultivars of Camellia oleifera. BMC Plant Biology, 2021, 21(1): 348.
[3]	PRACHYA S, WATTANASIRI C, PANSANIT A. Cytotoxic endophyte from Camellia oleifera Abel - Penicillium chermesinum NR121310. Mycology, 2020, 11(4): 316-321.
[4]	XIE Y Z, GE S B, JIANG S C, LIU Z L, CHEN L, WANG L S, CHEN J T, QIN L C, PENG W X. Study on biomolecules in extractives of Camellia oleifera fruit shell by GC-MS. Saudi Journal of Biological Sciences, 2018, 25(2): 234-236.
[5]	LIAO D L, SHI W, GAO J, DENG B, YU R J. Modified Camellia oleifera shell carbon with enhanced performance for the adsorption of cooking fumes. Nanomaterials, 2021, 11(5): 1349.
[6]	WANG Q Q, CHANG S S, TAN Y J, HU J B. Mesopore structure in Camellia oleifera shell. Protoplasma, 2019, 256(4): 1145-1151.
[7]	HU J B, SHI Y, LIU Y, CHANG S S. Anatomical structure of Camellia oleifera shell. Protoplasma, 2018, 255(6): 1777-1784.
[8]	PATIL J, VIJAYAKUMAR R, LINGA V, SIVAKUMAR G. Susceptibility of oriental armyworm, Mythimna separata (Lepidoptera: Noctuidae) larvae and pupae to native entomopathogenic nematodes. Journal of Applied Entomology, 2020, 144(7): 647-654.
[9]	KIM K N, JO Y C, HUANG Z J, SONG H S, RYU K H, HUANG Q Y, LEI C L. Influence of green light illumination at night on biological characteristics of the oriental armyworm Mythimna separata (Lepidoptera: Noctuidae). Bulletin of Entomological Research, 2020, 110(1): 136-143. doi: 10.1017/S0007485319000397 pmid: 31203829
[10]	KIM K N, SIN U C, JO Y C, HUANG Z J, HASSAN A, HUANG Q Y, LEI C L. Influence of green light at night on juvenile hormone in the oriental armyworm Mythimna separata (Lepidoptera: Noctuidae). Physiological Entomology, 2019, 44(3/4): 245-251.
[11]	GUO Y F, QIU J R, CHEN T, GAO S J, BU S H, WANG R, WANG J D. Characterization and functional analysis of a β-adrenergic-like octopamine receptor from the oriental armyworm (Mythimna separata Walker). Archives of Insect Biochemistry and Physiology, 2021, 106(4): e21772.
[12]	LI F F, CUI J, SHAHEEN T, TANG G H, WANG T, WOOLFLEY T, LI M L. Biocidal efficacy of tutin and its influence on immune cells and expression of growth-blocking and neuroglian peptides in Mythimna separata (Lepidoptera: Noctuidae). Archives of Insect Biochemistry and Physiology, 2021, 107(1): e21767.
[13]	ZHAO Y Y, SU L, LI S, LI Y P, XU X L, CHENG W N, WANG Y, WU J X. Insecticide resistance of the field populations of oriental armyworm, Mythimna separata (Walker) in Shaanxi and Shanxi provinces of China. Journal of Integrative Agriculture, 2018, 17(7): 1556-1562.
[14]	WANG J D, WANG W Z, WANG Y R, GAO S J, ELZAKI M, WANG R, WANG R, WU M. Response of detoxification and immune genes and of transcriptome expression in Mythimna separata following chlorantraniliprole exposure. Comparative Biochemistry and Physiology. Part D, Genomics & Proteomics, 2018, 28: 90-98.
[15]	LI X R, LI Y, WANG W, HE N, TAN X L, YANG X Q. LC₅₀ of lambda-cyhalothrin stimulates reproduction on the moth Mythimna separata (Walker). Pesticide Biochemistry and Physiology, 2019, 153: 47-54.
[16]	RODRIGUES G C, DOS SANTOS MAIA M, CAVALCANTI A B, BARROS R P, SCOTTI L, CESPEDES-ACUNA C L, MURATOV E N, SCOTTI M T. Computer-assisted discovery of compounds with insecticidal activity against Musca domestica and Mythimna separata. Food and Chemical Toxicology, 2021, 147: 111899.
[17]	VELASQUES J, CARDOSO M H, ABRANTES G, FRIHLING B E, FRANCO O L, MIGLIOLO L. The rescue of botanical insecticides: A bioinspiration for new niches and needs. Pesticide Biochemistry and Physiology, 2017, 143: 14-25. doi: S0048-3575(17)30296-1 pmid: 29183583
[18]	董小绮, 康兆勇, 刘胜男, 高清志. 新型植物源天然产物杀虫剂研究进展. 农药学学报, 2023, 25(5): 969-989.
	DONG X Q, KANG Z Y, LIU S N, GAO Q Z. Research progress of novel botanical insecticides. Chinese Journal of Pesticide Science, 2023, 25(5): 969-989. (in Chinese)
[19]	LI Y K, WANG S K, AIOUB A A, QIE X T, WU W J, HU Z N. Identification and analysis of full-length transcripts involved in the biosynthesis of insecticidal lignan (+)-haedoxan A in Phryma leptostachya. Industrial Crops and Products, 2019, 142: 111868.
[20]	TIAN Y Y, CHEN Z J, HUANG X Q, ZHANG L X, ZHANG Z Q. Evaluation of botanicals for management of piercing-sucking pests and the effect on beneficial arthropod populations in tea trees Camellia sinensis (L.) O. Kuntze (Theaceae). Journal of Insect Science, 2020, 20(6): 27.
[21]	田晓霖, 方晓武, 戴纪琛, 马青淑, 胡嘉隽, 何军, 田向荣. 32种植物甲醇提取物杀虫活性评价. 陕西农业科学, 2018, 64(11): 68-73.
	TIAN X L, FANG X W, DAI J C, MA Q S, HU J J, HE J, TIAN X R. Insecticidal activity evaluation of 32 methanol extracts. Shaanxi Journal of Agricultural Sciences, 2018, 64(11): 68-73. (in Chinese)
[22]	沈静, 周玉, 李琰, 马志卿, 张秀云, 张兴. 129种植物丙酮提取物杀虫活性筛选. 西北农林科技大学学报(自然科学版), 2017, 45(10): 101-110.
	SHEN J, ZHOU Y, LI Y, MA Z Q, ZHANG X Y, ZHANG X. Screening of the insecticidal activities of acetone extracts from 129 plants. Journal of Northwest A&F University (Natural Science Edition), 2017, 45(10): 101-110. (in Chinese)
[23]	李晶, 李娜, 丁品, 付麟雲, 王涛, 杜文静, 张建军, 武建荣, 刘锦霞. 3种橐吾属植物提取物的杀虫抑菌活性. 草业科学, 2022, 39(5): 899-906.
	LI J, LI N, DING P, FU L Y, WANG T, DU W J, ZHANG J J, WU J R, LIU J X. Insecticidal and bacteriostatic activities of extracts from three species of Ligularia. Pratacultural Science, 2022, 39(5): 899-906. (in Chinese)
[24]	于化龙, 李晶晶, 任美儒, 刘禄威, 马树杰. 110种植物提取物杀虫活性初步研究. 热带作物学报, 2021, 42(7): 2085-2093. doi: 10.3969/j.issn.1000-2561.2021.07.036
	YU H L, LI J J, REN M R, LIU L W, MA S J. Insecticidal activity of extracts from 110 traditional Chinese medicines. Chinese Journal of Tropical Crops, 2021, 42(7): 2085-2093. (in Chinese) doi: 10.3969/j.issn.1000-2561.2021.07.036
[25]	张洁, 李雪娇. 五加皮丙酮提取物杀虫活性的初步研究. 西北农业学报, 2019, 28(11): 1906-1912.
	ZHANG J, LI X J. Study on insecticidal activity of acetone extracts from Acanthopanar gracilistylus. Acta Agriculturae Boreali-Occidentalis Sinica, 2019, 28(11): 1906-1912. (in Chinese)
[26]	马树杰, 李雪娇, 马志卿, 张兴. 中国粗榧杀虫活性初步研究. 西北农林科技大学学报(自然科学版), 2016, 44(8): 155-161.
	MA S J, LI X J, MA Z Q, ZHANG X. Preliminary study on insecticidal activity of extracts from Cephalotaxus sinensis. Journal of Northwest A&F University (Natural Science Edition), 2016, 44(8): 155-161. (in Chinese)
[27]	张新瑞. 红蓼提取物的杀虫作用和作用机理研究[D]. 兰州: 甘肃农业大学, 2009.
	ZHANG X R. Insecticidal action and insecticidal mechanism on extracts from Polygonum orientale L.[D]. Lanzhou: Gansu Agricultural University, 2009. (in Chinese)
[28]	CUI C J, YANG Y Q, ZHAO T Y, ZOU K K, PENG C Y, CAI H M, WAN X C, HOU R Y. Insecticidal activity and insecticidal mechanism of total saponins from Camellia oleifera. Molecules, 2019, 24: 4518.
[29]	刘泽文, 王伟, 黄永芳, 吴春银, 史晓雨, 单体江. 油茶果壳提取物及其生物活性. 经济林研究, 2022, 40(3): 259-264.
	LIU Z W, WANG W, HUANG Y F, WU C Y, SHI X Y, SHAN T J. Biological activities of the fruit shell extracts of Camellia oleifera. Non-Wood Forest Research, 2022, 40(3): 259-264. (in Chinese)
[30]	詹丽, 李敬丹, 赵传琦, 梁倩. 蔓长春花对草地贪夜蛾杀虫活性成分及机制研究. 环境昆虫学报, 2024, 46(5): 1202-1212.
	ZHAN L, LI J D, ZHAO C Q, LIANG Q. Studies on the insecticidal constituents and mechanism of Vinca major against Spodoptera frugiperda. Journal of Environmental Entomology, 2024, 46(5): 1202-1212. (in Chinese)
[31]	FAROOQ M, FREED S. Infectivity of housefly, Musca domestica (Diptera: Muscidae) to different entomopathogenic fungi. Brazilian Journal of Microbiology, 2016, 47(4): 807-816.
[32]	CHI Y Y, QIAO K, JIANG H, LIN R H, WANG K Y. Comparison of two acute toxicity test methods for the silkworm (Lepidoptera: Bombycidae). Journal of Economic Entomology, 2015, 108(1): 145-149. doi: 10.1093/jee/tou016 pmid: 26470114
[33]	ALVES T J, CRUZ G S, WANDERLEY-TEIXEIRA V, TEIXEIRA A A, OLIVEIRA J V, CORREIA A A, CAMARA C A, CUNHA F M. Effects of Piper hispidinervum on spermatogenesis and histochemistry of ovarioles of Spodoptera frugiperda. Biotechnic & Histochemistry, 2014, 89(4): 245-255.
[34]	GANG F L, LI X T, YANG C F, HAN L J, QIAN H, WEI S P, WU W J, ZHANG J W. Synthesis and insecticidal activity evaluation of virtually screened phenylsulfonamides. Journal of Agricultural and Food Chemistry, 2020, 68(42): 11665-11671.
[35]	LI Y K, WEI J Q, FANG J M, LV W B, JI Y F, AIOUB A A, ZHANG J W, HU Z N. Insecticidal activity of four lignans isolated from Phryma leptostachya. Molecules, 2019, 24(10): 1976.
[36]	冀宇飞. 透骨草杀虫成分提取方法及分离研究[D]. 杨凌: 西北农林科技大学, 2017.
	JI Y F. Studies on the extraction methods and isolation of insecticidal components from Phryma leptostachya L.[D]. Yangling: Northwest A&F University, 2017. (in Chinese)
[37]	李春燕, 梁倩, 赵文兴, 梁宗锁, 王芳. 叉枝蒿对黏虫杀虫活性成分及作用机制研究. 南方农业学报, 2024, 55(1): 105-116.
	LI C Y, LIANG Q, ZHAO W X, LIANG Z S, WANG F. Insecticidal activity constituents and mechanism of Artemisia divaricata against Mythimna separata(Walker). Journal of Southern Agriculture, 2024, 55(1): 105-116. (in Chinese)
[38]	李春燕, 梁倩, 高成香, 梁宗锁, 王芳. 黄花蒿对黏虫杀虫活性成分及机制研究. 中国农业科技导报, 2024, 26(12): 129-137.
	LI C Y, LIANG Q, GAO C X, LIANG Z S, WANG F. Study on insecticidal activity constituents and mechanism of Artemisia annua against Mythimna separate. Journal of Agricultural Science and Technology, 2024, 26(12): 129-137. (in Chinese)
[39]	ZHU X Z, SUN M X, ZHANG Z W, LIU H X, HUANG J Y, HU Z N, WU W J, ZHANG J W. Design synthesis and insecticidal activities of 4-propargyloxybenzene sulfonamide derivatives substituted with amino acids. Journal of Asian Natural Products Research, 2023, 25(4): 379-386.
[40]	BURKON A, SOMOZA V. Quantification of free and protein-bound trans-resveratrol metabolites and identification of trans-resveratrol- C/O-conjugated diglucuronides - Two novel resveratrol metabolites in human plasma. Molecular Nutrition & Food Research, 2008, 52: 549-557.
[41]	AL-EITAN L, KHARMAH H A. Effect of EMB-FUBINACA on brain endothelial cell angiogenesis: Expression analysis of angiogenic markers. Naunyn-Schmiedeberg’s Archives of Pharmacology, 2025, 398: 1613-1624.
[42]	ARRESE E L, SOULAGES J L. Insect fat body: Energy, metabolism, and regulation. Annual Review of Entomology, 2010, 55: 207-225. doi: 10.1146/annurev-ento-112408-085356 pmid: 19725772
[43]	贾男, 臧国伟, 李春, 王颖. 辅因子在微生物细胞工厂中的代谢调控与应用. 中国生物工程杂志, 2022, 42(7): 79-89.
	JIA N, ZANG G W, LI C, WANG Y. Metabolic regulations and applications of cofactors in microbial cell factories. China Biotechnology, 2022, 42(7): 79-89. (in Chinese)
[44]	张源洁. 烟酸和烟酰胺对奶牛肝脂代谢的比较研究[D]. 杨凌: 西北农林科技大学, 2024.
	ZHANG Y J. Comparative study of niacin and niacinamide on liver lipid metabolism in dairy cows[D]. Yangling: Northwest A&F University, 2024. (in Chinese)
[45]	MOFFETT J R, NAMBOODIRI M A. Tryptophan and the immune response. Immunology and Cell Biology, 2003, 81: 247-265. doi: 10.1046/j.1440-1711.2003.t01-1-01177.x pmid: 12848846
[46]	NOWICKA B, KRUK J. Occurrence, biosynthesis and function of isoprenoid quinones. Biochimica et Biophysica Acta, 2010, 1797: 1587-1605. doi: 10.1016/j.bbabio.2010.06.007 pmid: 20599680

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时间 Time (min)	流动相Mobile phase A (v%)	流动相B Mobile phase B (v%)
0	95	5
0.5	95	5
5.5	50	50
9.0	5	95
10.5	5	95
10.6	95	5
12.0	95	5

杀虫方式 Insecticidal method	提取物 Extract	校正死亡率Corrected mortality rate (%)
杀虫方式 Insecticidal method	提取物 Extract	1 d	3 d	5 d	7 d
触杀活性 Contact toxicity	石油醚Petroleum ether	84.00±2.45a	84.00±2.45a	84.00±2.45a	84.00±2.45a
	三氯甲烷Chloroform	6.00±2.45c	12.00±3.74c	12.00±3.74d	16.00±5.10d
	乙酸乙酯Ethyl acetate	42.00±12.81b	42.00±12.81b	42.00±12.81bc	46.00±13.27bc
	水Aqueous	4.00±2.45c	6.00±2.45c	10.00±3.16d	14.00±5.10d
胃毒活性 Stomach toxicity	石油醚Petroleum ether	82.00±7.35a	84.00±6.00a	86.00±6.78a	86.00±6.78a
	三氯甲烷Chloroform	52.00±8.60b	54.00±7.48b	58.00±8.00b	58.00±8.00b
	乙酸乙酯Ethyl acetate	14.00±2.45c	18.00±5.83c	18.00±5.83cd	26.00±6.78cd
	水Aqueous	14.00±5.10c	18.00±5.83c	18.00±5.83cd	22.00±3.74cd

杀虫方式 Insecticidal method	处理时间 Treatment time (d)	致死中浓度 LC₅₀ (mg∙mL^-1)	95%置信区间 95% CI	斜率±标准误 Slope±standard error	卡方 χ²	P值 P value
触杀活性 Contact toxicity	1	9.53	5.31-43.85	3.38±0.30	25.00	<0.001
	3	8.00	6.04-11.55	3.00±0.25	6.95	0.073
	5	7.51	6.68-8.55	2.83±0.23	4.87	0.181
	7	7.02	6.24-7.98	2.76±0.23	4.84	0.184
胃毒活性 Stomach toxicity	1	10.34	5.48-125.52	3.68±0.34	27.66	<0.001
	3	9.41	4.36-858.62	2.79±0.24	32.84	<0.001
	5	8.76	4.48-59.47	2.90±0.25	28.16	<0.001
	7	8.76	4.48-59.47	2.90±0.25	28.16	<0.001

馏分 Fraction	校正死亡率Corrected mortality rate (%)
馏分 Fraction	1 d	3 d	5 d	7 d
1	22.00±2.00c	22.00±2.00cd	26.00±2.45cd	26.00±2.45cd
2	—	22.00±2.00cd	30.00±0c	30.00±0c
3	46.00±2.45b	52.00±2.00b	52.00±2.00b	54.00±2.45b
4	10.00±3.16def	10.00±3.16efg	10.00±3.16ghij	10.00±3.16ghij
5	6.00±2.45efgh	8.00±2.00efg	12.00±2.00fghi	12.00±2.00fghi
6	98.00±2.00a	98.00±2.00a	98.00±2.00a	98.00±2.00a
7	6.00±2.45efgh	8.00±2.00efg	10.00±0ghij	10.00±0ghij
8	12.00±2.00de	14.00±2.45def	16.00±2.45efg	16.00±2.45efg
9	8.00±2.00efg	14.00±2.45def	18.00±2.00ef	18.00±2.00ef
10	10.00±0def	16.00±2.45de	22.00±2.00de	22.00±2.00de
11	4.00±2.45fgh	4.00±2.45g	10.00±0ghij	10.00±0ghij
12	16.00±2.45cd	20.00±0cd	22.00±2.00de	22.00±2.00de
13	2.00±2.00gh	4.00±2.45g	8.00±2.00hij	8.00±2.00hij
14	2.00±2.00gh	2.00±2.00g	4.00±2.45j	4.00±2.45j
15	2.00±2.00gh	8.00±2.00efg	8.00±2.00hij	10.00±0ghij
16	2.00±2.00gh	6.00±2.45fg	16.00±2.45efg	16.00±2.45efg
17	52.00±2.00b	56.00±2.45b	56.00±2.45b	56.00±2.45b
18	4.00±2.45fgh	6.00±2.45fg	14.00±2.45fgh	14.00±2.45fgh
19	—	2.00±2.00g	6.00±2.45ij	6.00±2.45ij
20	22.00±2.00c	26.00±2.45c	28.00±2.00cd	28.00±2.00cd

处理时间 Treatment time (d)	致死中浓度 LC₅₀ (mg∙mL^-1)	95%置信区间 95% CI	斜率±标准误 Slope±standard error	卡方 χ²	P值 P value
1	3.99	1.78-19.41	2.71±0.21	32.94	<0.001
3	3.85	1.58-26.52	2.49±0.20	34.31	<0.001
5	3.72	1.36-45.36	2.31±0.18	35.96	<0.001
7	3.72	1.36-45.36	2.31±0.18	35.96	<0.001

Insecticidal Active Component Identification of Camellia oleifera Shell Against Mythimna separata and Its Action Mechanism

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馏分 Fraction	校正死亡率Corrected mortality rate (%)
馏分 Fraction	1 d	3 d	5 d	7 d
6.1	38.00±2.00ij	42.00±2.00h	44.00±2.45f	44.00±2.45f
6.2	84.00±2.45b	84.00±2.45b	84.00±2.45b	84.00±2.45b
6.3	26.00±2.45kl	26.00±2.45jk	26.00±2.45hi	26.00±2.45hi
6.4	100.00±0a	100.00±0a	100.00±0a	100.00±0a
6.5	56.00±2.45fg	56.00±2.45ef	58.00±2.00e	60.00±0e
6.6	22.00±2.00l	24.00±2.45jk	24.00±2.45hi	24.00±2.45hi
6.7	26.00±2.45kl	28.00±2.00ij	28.00±2.00gh	28.00±2.00gh
6.8	60.00±0def	60.00±0de	62.00±2.00de	62.00±2.00de
6.9	34.00±2.45j	34.00±2.45i	34.00±2.45g	34.00±2.45g
6.10	50.00±0gh	50.00±0fg	50.00±0f	50.00±0f
6.11	46.00±2.45h	46.00±2.45gh	46.00±2.45f	46.00±2.45f
6.12	62.00±2.00def	64.00±2.45cd	64.00±2.45cde	64.00±2.45cde
6.13	60.00±0def	60.00±0de	62.00±2.00de	62.00±2.00de
6.14	66.00±2.45cd	68.00±2.00c	70.00±0c	70.00±0c
6.15	64.00±2.45cde	64.00±2.45cd	68.00±2.00cd	68.00±2.00cd
6.16	60.00±0def	60.00±0de	60.00±0e	60.00±0e
6.17	58.00±2.00ef	60.00±0de	60.00±0e	60.00±0e
6.18	32.00±2.00jk	34.00±2.45i	34.00±2.45g	34.00±2.45g
6.19	44.00±2.45hi	46.00±2.45gh	46.00±2.45f	46.00±2.45f
6.20	70.00±0c	70.00±0c	70.00±0c	70.00±0c
6.21	20.00±0l	20.00±0k	20.00±0i	20.00±0i

序号 No.	保留时间 Retention time (min)	化合物 Compound	相对含量 Relative content (%)
1	1.839	正十六烷Hexadecane	19.33
2	1.971	1-十六烯1-Hexadecene	14.21
3	2.251	二十八烷Octacosane	4.03
4	2.503	十八烷Octadecane	9.24
5	2.595	二氯菊酸甲酯Dichlorochrysanthemic acid methyl ester	6.73
6	2.766	1-十八烯1-Octadecene	7.27
7	4.197	二十四烷醇1-Tetracosanol	3.87
8	6.909	异植醇Isophytol	5.92

化合物 Compound	校正死亡率Corrected mortality rate (%)
化合物 Compound	1 d	3 d	5 d	7 d
正十六烷Hexadecane	12.00±2.00c	14.00±2.45c	14.00±2.45d	14.00±2.45cd
1-十六烯1-Hexadecene	18.00±2.00b	30.00±0b	30.00±0b	32.00±2.00b
二十八烷Octacosane	—	2.00±2.00e	2.00±2.00f	4.00±2.45e
十八烷Octadecane	—	—	—	—
二氯菊酸Dichlorochrysanthemic acid	100.00±0a	100.00±0a	100.00±0a	100.00±0a
1-十八烯1-Octadecene	10.00±0cd	16.00±2.45c	18.00±2.00c	18.00±2.00c
二十四烷醇1-Tetracosanol	—	—	—	—
异植醇Isophytol	8.00±2.00d	10.00±0d	10.00±0e	10.00±0d

处理 Treatment	处理时间 Treatment time (d)	致死中浓度 LC₅₀ (μg∙mL^-1)	95%置信区间 95% CI	斜率±标准误 Slope±standard error	卡方 χ²	P值 P value
二氯菊酸 Dichlorochrysanthemic acid	1	91.62	76.93-110.12	2.42±0.08	258.93	<0.001
	3	55.61	46.62-66.40	1.49±0.05	132.25	<0.001
	5	34.94	28.04-42.64	1.19±0.05	115.49	<0.001
	7	24.43	18.20-31.08	1.10±0.05	129.87	<0.001
除虫菊酯 Pyrethrin	1	39.50	23.80-65.65	0.53±0.03	100.34	<0.001
	3	23.19	12.67-40.16	0.56±0.03	133.79	<0.001
	5	11.98	6.40-20.08	0.53±0.03	104.19	<0.001
	7	8.10	3.90-14.22	0.54±0.03	117.25	<0.001

序号 No.	名称 Name	变异倍数 Fold change	P值 P value	保留时间 Retention time (min)
1	4-乙基-2,6-二羟基苯基硫酸氢酯 4-Ethyl-2,6-dihydroxyphenyl hydrogen sulfate	0.423	0.017	0.713
2	云杉苷Piceid	2.150	0.004	2.849
3	大麻素Cannabinoid	2.669	0.032	3.027
4	己酰甘氨酸Caproylglycine	2.069	0.012	3.326
5	5-氟大麻素代谢物5-Fluoro-cannabinoid metabolite	2.460	0.040	4.216
6	N-二十五酰甘氨酸N-Pentacosanoylglycine	0.487	0.047	8.806

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