气相色谱-质谱法测定植物油中8种维生素E及其在芝麻油真伪鉴别方面的应用

doi:10.3724/SP.J.1123.2019.09011

摘要/Abstract

摘要：

建立了气相色谱-质谱（GC-MS）同时测定植物油中α-、β-、γ-、δ-生育酚和α-、β-、γ-、δ-生育三烯酚等8种维生素E的分析方法。植物油样品经甲醇超声提取、浓缩、定容，在分时段选择离子监测（SIM）模式下分离分析，采用外标法进行定量。结果表明，8种维生素E可实现基线分离；在0.01~1 mg/L范围内，所有目标物均呈良好线性关系，相关系数均大于0.99；检出限和定量限分别为0.03~0.25 mg/kg和0.10~0.83 mg/kg；在芝麻油中分别添加10、50和250 mg/kg 3个水平的8种维生素E进行加标试验，平均回收率为87.5%~107.4%，相对标准偏差（RSD）≤ 7.5%。所建立的方法简单、准确、可靠，且灵敏度高，可用于测定植物油中8种维生素E的含量。采用上述方法对芝麻油、大豆油、菜籽油、葵花籽油、花生油、玉米油和棕榈油等7种共75个植物油样品中维生素E的含量进行测定。结果显示，芝麻油与其他6种植物油中的8种维生素E的组成和含量均有显著差异性，因此该方法可作为芝麻油掺入其他植物油的特征鉴定指标。

关键词: 气相色谱-质谱, 生育酚, 生育三烯酚, 维生素E, 芝麻油, 真伪鉴别

Abstract:

A method was established for the determination of eight vitamins E (α-, β-, γ-, δ-tocopherol and α-, β-, γ-, δ-tocotrienol) in vegetable oils using gas chromatography-mass spectrometry (GC-MS). The targets were extracted with methanol, and analyzed by GC-MS in the selected ion monitoring (SIM) mode after concentration to a constant volume, and quantified using the external standard method. Baseline separation were achieved for all the target compounds. The linearities of all the compounds were between 0.01 and 1 mg/L. The limits of detection (LODs) and limits of quantification (LOQs) were in the range of 0.03-0.25 mg/kg and 0.10-0.83 mg/kg, respectively. The average recoveries of all the targets in sesame oil samples were between 87.5% and 107.4% at three spiked levels (10, 50, and 250 mg/kg), and the RSDs were all less than 7.5%. The tocopherols and tocotrienols contents in sesame oil samples and in six lower-price vegetable oils (soybean, rapeseed, sunflower, peanut, corn and palm oils) were determined by the above mentioned method. The results showed that the vitamin E profiles of sesame oil were significantly different from those of the other six vegetable oils. Therefore, vitamin E can be used as a discriminating parameter for detecting the adulteration of sesame.

Key words: gas chromatography-mass spectrometry (GC-MS), tocopherol, tocotrienol, vitamin E, sesame oil, authentication

沈伟健, 王红, 陆慧媛, 余可垚, 胡国绅, 魏雪缘, 吴斌. 气相色谱-质谱法测定植物油中8种维生素E及其在芝麻油真伪鉴别方面的应用[J]. 色谱, 2020, 38(5): 595-599.

SHEN Weijian, WANG Hong, LU Huiyuan, YU Keyao, HU Guoshen, WEI Xueyuan, WU Bin. Determination of eight vitamin E in vegetable oils by gas chromatography-mass spectrometry and its application on authentication of sesame oil[J]. Chinese Journal of Chromatography, 2020, 38(5): 595-599.

Compound	RT/min	RT window/min	Monitoring ions (m/z)
* Quantitative ion.
δ-T	8.81	6.00-9.10	137, 177, 402^*
β-T	9.34	9.10-9.80	151, 191, 416^*
γ-T	9.46	9.10-9.80	151, 191, 416^*
δ-T3	9.53	9.10-9.80	137, 177, 396^*
α-T	10.03	9.80-10.70	165, 205, 430^*
β-T3	10.20	9.80-10.70	151, 191, 410^*
γ-T3	10.35	9.80-10.70	151, 191, 410^*
α-T3	11.07	10.70-14.00	165, 205, 424^*

Compound	RT/min	RT window/min	Monitoring ions (m/z)
* Quantitative ion.
δ-T	8.81	6.00-9.10	137, 177, 402^*
β-T	9.34	9.10-9.80	151, 191, 416^*
γ-T	9.46	9.10-9.80	151, 191, 416^*
δ-T3	9.53	9.10-9.80	137, 177, 396^*
α-T	10.03	9.80-10.70	165, 205, 430^*
β-T3	10.20	9.80-10.70	151, 191, 410^*
γ-T3	10.35	9.80-10.70	151, 191, 410^*
α-T3	11.07	10.70-14.00	165, 205, 424^*

Compound	Linear equation	r	LOD/ (mg/kg)	LOQ/ (mg/kg)
Y: peak area of quantitative ion; X: mass concentration, mg/L.
δ-T	Y=42554X-69.713	0.9997	0.03	0.10
β-T	Y=49282X-76.982	0.9995	0.05	0.17
γ-T	Y=47434X-215.47	0.9993	0.03	0.10
δ-T3	Y=15776X+5.9508	0.9996	0.15	0.50
α-T	Y=51856X-506.92	0.9967	0.08	0.27
β-T3	Y=34969X-124.86	0.9994	0.07	0.23
γ-T3	Y=13774X+20.720	0.9998	0.25	0.83
α-T3	Y=23791X-75.181	0.9995	0.15	0.50

Compound	Linear equation	r	LOD/ (mg/kg)	LOQ/ (mg/kg)
Y: peak area of quantitative ion; X: mass concentration, mg/L.
δ-T	Y=42554X-69.713	0.9997	0.03	0.10
β-T	Y=49282X-76.982	0.9995	0.05	0.17
γ-T	Y=47434X-215.47	0.9993	0.03	0.10
δ-T3	Y=15776X+5.9508	0.9996	0.15	0.50
α-T	Y=51856X-506.92	0.9967	0.08	0.27
β-T3	Y=34969X-124.86	0.9994	0.07	0.23
γ-T3	Y=13774X+20.720	0.9998	0.25	0.83
α-T3	Y=23791X-75.181	0.9995	0.15	0.50

Compound	Spiked level/ (mg/kg)	Background/ (mg/kg)	Detected/ (mg/kg)	Average recovery/ %	RSD/ %
ND: below LOD.
δ-T	10	13.48	22.32	88.4	6.2
	50		62.68	98.4	4.8
	250		251.28	95.1	5.3
β-T	10	0.45	10.97	105.2	4.3
	50		51.65	102.4	5.2
	250		249.35	99.6	4.9
γ-T	10	368.91	378.54	96.3	6.5
	50		415.61	93.4	5.8
	250		596.61	91.1	3.8
δ-T3	10	ND	10.62	106.2	6.0
	50		48.60	97.2	6.5
	250		218.80	87.5	7.3
α-T	10	10.46	20.09	96.3	7.2
	50		57.36	93.8	5.9
	250		244.56	93.6	6.7
β-T3	10	ND	10.22	102.2	7.5
	50		53.70	107.4	5.5
	250		263.20	105.3	6.6
γ-T3	10	ND	9.15	91.5	4.8
	50		51.60	103.2	5.6
	250		235.50	94.2	6.9
α-T3	10	ND	10.34	103.4	7.3
	50		52.90	105.8	6.3
	250		241.60	96.6	6.8

气相色谱-质谱法测定植物油中8种维生素E及其在芝麻油真伪鉴别方面的应用

Determination of eight vitamin E in vegetable oils by gas chromatography-mass spectrometry and its application on authentication of sesame oil

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Metrics

Compound	Sesame oil (n=15)	Soybean oil (n=10)	Rapeseed oil (n=10)	Sunflower oil (n=10)	Peanut oil (n=10)	Maize oil (n=10)	Palm oil (n=10)
δ-T	14.54	253.42	16.47	0.60	10.31	32.08	ND
β-T	0.31	25.92	3.16	20.33	6.59	11.23	1.71
γ-T	447.83	739.42	370.89	7.70	98.50	522.53	3.57
α-T	8.56	167.95	247.07	527.70	152.45	180.88	170.56
δ-T3	ND	ND	ND	ND	ND	ND	86.62
β-T3	ND	ND	ND	ND	ND	ND	15.00
γ-T3	ND	ND	ND	ND	ND	16.38	337.74
α-T3	ND	ND	ND	ND	ND	11.54	218.06

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