番石榴叶中挥发油组分的固相微萃取分析

doi:10.3976/j.issn.1002-4026.2021.06.003

摘要/Abstract

摘要：

建立了一种应用顶空固相微萃取-气相色谱质谱分析番石榴叶中挥发油组分的方法。对固相微萃取纤维种类、萃取温度、萃取时间和样品溶液的离子强度进行了单因素优化试验,并得出了最优试验条件为:碳分子筛羧乙基/二乙烯基苯/聚二甲基硅氧烷(CAR/DVB/PDMS)萃取纤维,萃取温度65 ℃,萃取时间40 min,离子强度20%。该方法共鉴定出了47种组分,其中酮类化合物8种,醛类14种,酯类5种,醇类6种,烯烃类4种,酸类2种,剩余酚类等其他化合物8种。通过面积归一化法分析,鉴定出化合物结构的组分相对含量占总挥发油组分含量的93.97%。该方法为番石榴叶药用价值的研究提供方法及数据支持。

关键词: 顶空固相微萃取, 番石榴叶, 挥发油, 面积归一化, 气相色谱质谱法

Abstract:

In this study, a method using headspace solid phase microextraction (HS-SPME) and gas chromatography-mass spectrometry (GC-MS) for the analysis of volatile oil in guava leaves was developed. Several factors, including types of SPME fiber, extraction temperature, extraction time, and ionic strength of the sample solution, were optimized using single-factor optimization strategy. The optimal conditions were as follows: CAR/DVB/PDMS extraction fiber, extraction temperature of 65 ℃, extraction time of 40 min, and ionic strength of 20%. A total of 47 chemical compounds were identified, including eight types of ketones, 14 types of aldehydes, five types of esters, six types of alcohols, four types of olefins,two types of acids, and others, such as phenols. The identified components account for 93.97% of the total chemical constitutes in guava leaves, calculated using the peak area normalization method. This method provides methods and data support for the study of the medicinal value of guava leaves.

Key words: headspace solid phase microextraction, guava leaves, volatile oil, peak area normalization method, gas chromatography tandem mass spectrometry

中图分类号:

R284.1

许亦真. 番石榴叶中挥发油组分的固相微萃取分析[J]. 山东科学, 2021, 34(6): 15-21.

XU Yi-zhen. Analysis of volatile oil constitutes of guava leaves by solid phase microextraction[J]. Shandong Science, 2021, 34(6): 15-21.

图/表 6

图1

图2

图3

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图5

表1

番石榴叶中挥发油组分及含量"

类别	编号		保留时间/min		中文名称		英文名称		相对含量/%		分子量		分子式		相对含量分类合计/%
酮类	1	28.97		植酮		2-Pentadecanone, 6,10,14-trimethyl-		5.39		268.3		C₁₈H₃₆O		18.82
	2	22.15		1-(4-叔丁基苯基)丙-2-酮		1-(4-tert-Butylphenyl)propan-2-one		4.36		190.1		C₁₃H₁₈O
	3	23.16		α-紫罗兰酮		.alpha.-Ionone		3.08		192.2		C₁₃H₂₀O
	4	23.23		4-叔丁基苯丙酮		1-(4-tert-Butylphenyl)propan-2-one		1.41		190.1		C₁₃H₁₈O
	5	23.56		香叶基丙酮		5,9-Undecadien-2-one, 6,10-dimethyl-, (E)-		1.33		194.2		C₁₃H₂₂O
	6	24.18		脱氢-β紫罗兰酮		Dehydro-β-ionone		1.23		190.1		C₁₃H₁₈O
	7	22.60		四氢香叶基丙酮		2-Undecanone, 6,10-dimethyl-		1.06		198.2		C₁₃H₂₆O
	8	24.24		β-紫罗兰酮		trans-.beta.-Ionone		0.96		192.2		C₁₃H₂₀O
醛类	9	18.91		2-十三碳烯醛		2-Tridecenal, (E)-		3.06		196.2		C₁₃H₂₄O		17.95
	10	11.01		正辛醛		Octanal		1.79		128.1		C₈H₁₆O
	11	12.76		2-辛烯醛		2-Octenal, (E)-		1.51		126.1		C₈H₁₄O
	12	15.93		2-壬烯醛		2-Nonenal, (E)-		1.48		140.1		C₉H₁₆O
	13	12.32		苯乙醛		Benzeneacetaldehyde		1.47		120.1		C8H8O
	14	17.88		5-羟甲基糠醛		5-Hydroxymethylfurfural		1.35		126.0		C₆H₆O₃
	15	15.74		2,6-壬二烯醛		2,6-Nonadienal, (E,E)-		1.10		138.1		C₉H₁₄O
	16	17.20		藏红花醛		1,3-Cyclohexadiene-1-carboxaldehyde, 2,6,6-trimethyl-		1.10		150.1		C₁₀H₁₄O
	17	17.30		癸醛		Decanal		0.96		156.2		C₁₀H₂₀O
	18	9.50		庚烯醛		2-Heptenal, (Z)-		0.91		112.1		C₇H₁₂O
	19	4.78		正己醛		Hexanal		0.90		100.1		C₆H₁₂O
	20	14.24		壬醛		Nonanal		0.82		142.1		C₉H₁₈O
	21	21.67		2-十二醛		2-Dodecenal		0.75		182.2		C₁₂H₂₂O
	22	11.24		2,4-庚二烯醛		2,4-Heptadienal, (E,E)-		0.74		110.1		C₇H₁₀O
酯类	23	25.06		二氢猕猴桃内酯		2(4H)-Benzofuranone, 5,6,7,7a-tetrahydro-4,4,7a-trimethyl-		7.69		180.1		C₁₁H₁₆O₂		14.41
	24	30.17		棕榈酸甲酯		n-Hexadecanoic acid		3.14		256.2		C₁₆H₃₂O₂
	25	28.20		苯甲酸苄酯		Benzyl Benzoate		1.73		212.1		C₁₄H₁₂O₂
	26	25.59		苯甲酸-3-己烯酯		3-Hexen-1-ol, benzoate, (Z)-		0.83		204.1		C₁₆H₃₂O₂
	27	34.81		辛酸硬酯酰		Hexanoic acid, 2-ethyl-, hexadecyl ester		1.02		368.4		C₂₄H₄₈O₂
烯烃类	28	29.28		石竹烯		Caryophyl lene		6.06		204.2		C₁₅H₂₄		13.43
	29	33.52		咕吧烯		Copaene		4.00		204.4		C₁₅H₂₄
	30	23.04		异松油烯		Cyclohexene, 1-methyl-4-(1-methylethylidene)-		2.05		136.1		C₁₀H₁₆
	31	38.48		菠菜烯		Supraene		1.32		410.4		C₃₀H₅₀
类别	编号		保留时间/min		中文名称		英文名称		相对含量/%		分子量		分子式		相对含量分类合计/%
醇类	32	14.11		芳樟醇		1,6-Octadien-3-ol, 3,7-dimethyl-		3.42		154.1		C₁₀H₁₈O		11.37
	33	10.25		蘑菇醇		1-Octen-3-ol		2.79		128.1		C₈H₁₆O
	34	16.93		α-松油醇		.alpha.-Terpineol		1.50		154.1		C₁₀H₁₈O
	35	13.18		辛醇		1-Octanol		1.37		130.1		C8H18O
	36	13.10		2-癸烯-1-醇		2-Decen-1-ol, (E)-		1.28		156.2		C₁₀H₂₀O
	37	12.89		2-亚甲基环戊醇		2-Methylene cyclopentanol		1.01		98.1		C₆H₁₀O
酚	38		14.47		麦芽酚		Maltol		10.65		126.0		C₆H₆O₃		10.65
酸类	39	32.17		十八烷酸		Octadecanoic acid		1.11		284.3		C₁₈H₃₆O₂		1.58
酸类	40	31.97		6-十八碳烯酸		6-Octadecenoic acid		0.47		282.3		C₁₈H₃₄O₂		1.58
其他类	41	28.49		蒽		Anthracene		1.22		178.1		C₁₄H₁₀		5.76
	42	24.03		D-阿洛糖		D-Allose		0.98		180.1		C₆H₁₂O₆
	43	10.68		2-正戊基呋喃		Furan, 2-pentyl-		0.93		138.1		C₉H₁₄O
	44	25.84		芴		Fluorene		0.74		166.1		C₁₃H₁₀
	45	19.42		2-(1-戊烯基)呋喃		Furan, 2-(1-pentenyl)-, (E)-		0.69		136.1		C₉H₁₂O
	46	24.78		二苯并呋喃		Dibenzofuran		0.68		168.1		C₁₂H₈O
	47	27.15		1,2,3-三甲基-4-[(E)-丙-1-烯基]萘		Naphthalene, 1,2,3-trimethyl-4-propenyl-, (E)-		0.52		210.1		C₁₆H₁₈

表1

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