基于全二维气相色谱质谱法对全脂乳粉在不同水合工艺下挥发性成分的分析

刘媛; 靳春平; 贾志磊; 付永猛; 安保森; 徐飞鸿; 付瑞东; 王萍; 邹强; 李启明

doi:10.13386/j.issn1002-0306.2022070229

基于全二维气相色谱质谱法对全脂乳粉在不同水合工艺下挥发性成分的分析

doi: 10.13386/j.issn1002-0306.2022070229

1.
乳品营养与功能四川省重点实验室，四川省优质乳品制备与质量控制技术工程实验室，新希望乳业股份有限公司，四川成都 610000
2.
成都大学食品与生物工程学院，四川成都 610106
3.
青岛新希望琴牌乳业有限公司，山东青岛 266000

基金项目: 乳制品及牛肉制品精深加工关键技术研究与产业化应用示范（2020YFN0153）。

详细信息

作者简介:
刘媛（1980−），女，硕士，高级工程师，研究方向：乳品饮料加工技术，E-mail：liuyuan1121@163.com

通讯作者:
李启明（1979−），男，博士，高级工程师，研究方向：乳品技术开发研究，E-mail：qm258@126.com

中图分类号: TS252
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出版历程
- 收稿日期: 2022-07-20
- 网络出版日期: 2023-04-20
- 刊出日期: 2023-06-01

Analysis on Volatile Components of Whole Milk Powder under Different Rehydration Processes by Comprehensive Two-Dimensional Gas Chromatography-Mass Spectrometry

1.
Dairy Nutrition and Function Key Laboratory of Sichuan Province, Sichuan Engineering Laboratory for High-quality Dairy Product Preparation and Quality Control Technology, New Hope Dairy Corporated Limited Company, Chengdu 610000, China
2.
College of Food and Biological Engineering, Chengdu University, Chengdu 610106, China
3.
Qingdao Newhope Dairy Company, Qingdao 266000, China

摘要

摘要: 为了优化全脂乳粉水合工艺，探究低温水合对复原乳风味影响，本研究采用顶空固相微萃取（Headspace solid phase microextraction，HS-SPME）结合全二维气相色谱质谱法（Comprehensive two-dimensional gas chromatography-mass spectrometry，GC-GC-MS）考察全脂乳粉单段水合（55 ℃水合30 min）和两段水合（55 ℃水合30 min后4 ℃水合4、8、12 h）工艺条件下复原乳主要挥发性化合物相对含量，并利用ROAV法和主成分分析法分析挥发性物质对复原乳的风味贡献。结果表明：四组复原乳样品共鉴定出醇、醚、呋喃等9大类挥发性物质共68种，十二醇、正己醛、正辛醛、壬醛、反-2-辛烯醛、癸醛、反式-2-壬醛为四组复原乳共有的特征风味物质，醛类化合物对复原乳特征风味的贡献大于其他挥发性化合物；通过主成分分析，将单段水合复原乳与两段水合复原乳进行了良好区分，增加工序4 ℃水合工艺有利于降低1-辛烯-3-醇、十二醇、反式-2-癸烯醛造成的异味，其中4 ℃水合8 h最有利于提升复原乳有益风味，为最佳水合工艺。该结果为工业化复原乳的生产提供参考依据。
- 全二维气相色谱质谱法 /
- 复原乳 /
- 挥发性物质 /
- ROAV值 /
- 主成分分析
Abstract: In order to optimize the rehydration process of whole milk powder and explore the effect of low temperature rehydration on the flavor of reconstituted milk, headspace solid phase microextraction (HS-SPME) combined with comprehensive two-dimensional gas chromatography-mass spectrometry (GC-GC-MS) was used in this study. The percentage of main volatile compounds in the reconstituted milk was investigated under the process conditions of single-stage rehydration (55 ℃ for 30 min) and two-stage rehydration (4 ℃ for 4, 8 and 12 h after rehydration 55 ℃ for 30 min). The ROAV method and principal component analysis were used to analyze the flavor contribution of volatile substances to the reconstituted milk. The results showed that a total of 68 kinds of volatile substances divided into 9 types, such as alcohol, ether and furan were identified in the 4 groups of reconstituted milk samples. Among these substances, dodecanol, n-hexanal, n-octaldehyde, nonanal, trans-2-octenal, decanal, and trans-2-nonanal were the common characteristic flavor substances in the four groups of reconstituted milk, the contribute of aldehydes to the reconstituted milk was more than that of other volatile compounds. The single-stage hydration reconstituted milk was well differentiated from the two-stage hydration reconstituted milk by principal component analysis. The rehydration process at 4 ℃ was beneficial to reduce the smell caused by 1-octene-3-alcohol, dodecanol and trans-2-decenoaldehyde. The rehydration process at 4 ℃ for 8 h was the most beneficial to improve the beneficial flavor of the reconstituted milk, which was the best rehydration process. The results could provide a reference for the industrial production of reconstituted milk.
- comprehensive two-dimensional gas chromatography-mass spectrometry (GC-GC-MS) /
- reconstituted milk /
- volatile substances /
- ROAV value /
- principal component analysis

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图 1 四组复原乳SPME-GC-GC-MS色谱图

Figure 1. SPME-GC-GC-MS chromatograms of four groups of reconstituted milk

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图 2 四组复原乳挥发性风味物质Venny图

Figure 2. The Venny diagram of the volatile flavor substances in the four groups of reconstituted milk

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图 3 各复原乳在PC1、PC2、PC3上的因子得分

Figure 3. Factor scores of each reconstituted milk on PC1, PC2 and PC3

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表 1 水合复原乳挥发性风味物质信息表

Table 1. Information of volatile flavor substances in hydrated and reconstituted milk

分类	序号	中文名称	分子式	相对含量（%）
分类	序号	中文名称	分子式	A	B	C	D
醇	1	1-戊醇	C₅H₁₂O	0.15±0.04^b	0.27±0.06^a	0.28±0.05^a	0.23±0.02^a
	2	正己醇	C₆H₁₄O	0.18±0.02	—	—	—
	3	四氢芳樟醇	C₁₀H₂₂O	0.13±0.01^b	0.18±0.02^a	0.19±0.02^a	—
	4	1-辛烯-3-醇	C₈H₁₆O	0.16±0.02	—	—	—
	5	2,3-丁二醇	C₄H₁₀O₂	0.15±0.03	—	—	—
	6	十二醇	C₁₂H₂₆O	2.58±1.29^a	1.77±0.55^a	1.32±0.30^a	2.19±0.24^a
	7	1-十六烷醇	C₁₆H₃₄O	0.43±0.14^a	—	0.26±0.02^b	0.18±0.01^b
	8	芳樟醇	C₁₀H₁₈O	—	0.23±0.03^a	—	0.21±0.03^a
	9	辛醇	C₈H₁₈O	—	—	—	0.20±0.03
	10	3-十二烷醇	C₁₈H₃₈O₄	—	—	—	0.16±0.01
总醇				3.78±1.43^a	2.45±0.56^a	2.05±0.24^a	3.17±0.25^a
醚	11	十二烷基二乙二醇醚	C₁₆H₃₄O₃	0.56±0.22	—	—	—
总醚				0.56±0.22
呋喃	12	2-正戊基呋喃	C₉H₁₄O	0.29±0.07^a	—	0.40±0.14^a	—
呋喃	13	2-丁基四氢呋喃	C₈H₁₆O	0.28±0.04	—	—	—
总呋喃				0.57±0.05^a	—	0.40±0.14^a	—
醛	14	正己醛	C₆H₁₂O	12.44±2.42^a	10.85±2.07^a	15.51±1.89^a	8.08±3.33^b
	15	正辛醛	C₈H₁₆O	1.72±0.17^ab	1.55±0.28^b	2.05±0.3^a	1.51±0.22^b
	16	壬醛	C₉H₁₈O	6.30±0.69^a	6.65±0.84^a	7.69±0.79^a	7.44±1.95^a
	17	反-2-辛烯醛	C₈H₁₄O	0.77±0.19^a	0.52±0.11^a	0.82±0.28^a	0.51±0.06^a
	18	癸醛	C₁₀H₂₀O	0.67±0.08^a	0.65±0.01^a	0.78±0.24^a	0.62±0.14^a
	19	反式-2-壬醛	C₉H₁₆O	0.27±0.07^a	0.23±0.03^a	0.22±0.03^a	0.25±0.03^a
	20	反式-2-癸烯醛	C₁₀H₁₈O	0.19±0.08^a	—	0.23±0.07^a	—
	21	2-十一烯醛	C₁₁H₂₀O	0.25±0.09	—	—	—
	22	十四烷醛	C₁₄H₂₈O	0.19±0.03	—	—	—
	23	顺式二庚醛	C₇H₁₂O	0.47±0.02^a	0.46±0.07^a	—	—
	24	戊醛	C₅H₁₀O	—	1.05±0.11	—	—
	25	异戊醛	C₅H₁₀O	—	—	—	0.36±0.11
总醛				23.27±3.62^ab	21.96±2.75^ab	27.30±3.45^a	18.77±1.57^b
酸	26	己酸	C₆H₁₂O₂	0.34±0.16^a	0.34±0.04^a	—	—
	27	辛酸	C₈H₁₆O₂	0.38±0.05^ab	0.47±0.04^a	0.32±0.12^b	—
	28	正癸酸	C₁₀H₂₀O₂	0.74±0.24^a	0.97±0.25^a	0.88±0.07^a	0.34±0.10^b
	29	月桂酸	C₁₂H₂₄O₂	—	0.63±0.09^a	0.58±0.08^a	—
总脂肪酸				1.46±0.08^ab	2.41±0.34^a	1.78±0.10^ab	0.34±0.10^b
酮	30	5-甲基-2-己酮	C₇H₁₄O	2.34±0.36^a	1.77±0.17^ab	1.68±0.15^b	2.12±0.44^a
酮	31	甲基壬基甲酮	C₁₁H₂₂O	0.19±0.01^a	0.23±0.02^a	—	—
	32	十二烷-6,7-二酮	C₁₂H₂₂O₂	0.16±0.01	—	—	—
总酮				2.69±0.38^a	2.00±0.16^ab	1.68±0.15^b	2.12±0.44^ab
烷	33	4-甲基辛烷	C₉H₂₀	2.24±1.00^ab	1.87±0.56^b	3.05±0.31^ab	3.49±0.72^a
	34	十二烷	C₁₂H₂₆	0.44±0.02	—	—	—
	35	十一烷	C₁₁H₂₄	3.13±0.29^a	1.44±0.17^b	1.16±0.86^c	2.90±0.50^ab
	36	正十五烷	C₁₅H₃₂	0.40±0.02^b	0.47±0.05^b	0.25±0.02^c	0.97±0.07^a
	37	正十九烷	C₁₉H₄₀	0.67±0.38^a	0.63±0.06^ab	0.30±0.02^b	0.35±0.04^ab
	38	正二十一烷	C₂₁H₄₄	0.31±0.04	—	—	—
	39	姥鲛烷	C₁₉H₄₀	1.05±0.06	—	—	—
	40	正十七烷	C₁₇H₃₆	1.14±0.26^a	—	—	0.24±0.03^b
	41	正十八烷	C₁₈H₃₈	0.88±0.12	—	—	—
	42	5-苯基十一烷	C₁₇H₂₈	0.18±0.03	—	—	—
	43	戊基环丙烷	C₈H₁₆	0.23±0.02^a	0.21±0.04^a	0.22±0.03^a	0.25±0.02^a
	44	2,6,10-三甲基十四烷	C₁₇H₃₆	1.03±0.07	—	—	—
	45	十三烷	C₁₃H₂₈	—	—	—	1.12±0.15
	46	十四烷	C₁₄H₃₀	—	0.55±0.05	—	—
	47	正十六烷	C₁₆H₃₄	—	—	—	0.83±0.50
	48	1-氢过氧己烷	C₆H₁₄O₂	—	0.17±0.02^a	0.18±0.01^a	—
	49	1-环丙基戊烷	C₈H₁₆	0.21±0.02^a	0.18±0.03^a	0.20±0.00^a	0.22±0.02^a
	50	2,4,6-三甲基癸烷	C₁₃H₂₈	—	—	0.17±0.01	—
	51	2,6-二甲基癸烷	C₁₂H₂₆	—	—	0.26±0.01	—
	52	1-甲基-2-辛基-环丙烷	C₁₂H₂₄	—	—	0.50±0.04	—
	53	环十二烷	C₁₂H₂₄	—	—	—	0.50±0.03
总烷				11.90±0.70^a	5.52±0.56^b	6.29±0.77^b	10.87±0.85^a
烯	55	（R）-1-甲基-5-（1-甲基乙烯基）-环己烯	C₁₀H₁₆	22.14±1.55^a	21.32±2.68^a	23.67±1.88^a	23.79±1.65^a
烯	55	月桂烯	C₁₀H₁₆	—	—	—	0.20±0.03
总烯				22.14±1.55^a	21.32±2.68^a	23.67±1.88^a	23.99±1.64^a
酯	56	甲酸庚酯	C₈H₁₆O₂	0.12±0.01	—	—	—
	57	丁位癸内酯	C₁₀H₁₈O₂	0.75±0.05^b	1.09±0.08^a	0.80±0.07^b	0.80±0.09^b
	58	棕榈酸甲酯	C₁₇H₃₄O₂	0.71±0.16^a	—	0.38±0.02^b	0.30±0.04^b
	59	乙二醇月桂酸酯	C₁₄H₃₀O₂	1.07±0.12^a	0.87±0.09^ab	0.85±0.13^b	0.48±0.04^c
	60	丁位十二内酯	C₁₂H₂₂O₂	0.35±0.06^a	0.47±0.07^a	0.41±0.08^a	0.40±0.05^a
	61	油酸甲酯	C₁₉H₃₆O₂	0.41±0.06^a	—	0.25±0.01^b	—
	62	亚油酸甲酯	C₁₉H₃₄O₂	0.98±0.13	—	—	—
	63	邻苯二甲酸二异丁酯	C₁₆H₂₂O₄	0.62±0.06	—	—	—
	64	亚麻酸甲酯	C₁₉H₃₂O₂	0.19±0.03	—	—	—
	65	二氯乙酸十二烷基酯	C₁₄H₂₆Cl₂O₂	0.2±0.02	—	—	—
	66	γ-十二内酯	C₁₂H₂₂O₂	—	—	0.18±0.02	—
	67	邻苯二甲酸正丁异辛酯	C₂₀H₃₀O₄	—	—	0.29±0.03	—
	68	9-顺式,11-反式十八碳二烯酸甲酯	C₁₉H₃₄O₂	—	—	0.55±0.08^a	0.40±0.03^a
总酯				5.40±0.37^a	2.43±0.22^c	3.71±0.24^b	2.38±0.16^c
总挥发性物质				71.75±4.44^a	58.07±2.09^c	66.89±2.58^ab	61.61±1.68^bc
注：同行不同字母代表组间具有显著差异（P<0.05）；“—”表示未检出。

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表 2 四种复原乳的挥发性风味物质及ROAV值

Table 2. Volatile flavor compounds and ROAV values of four reconstituted milks

序号	中文名称	阈值^[35-36] （mg/kg）	ROAV
序号	中文名称	阈值^[35-36] （mg/kg）	A	B	C	D
1	1-戊醇	0.15	0.02	0.03	0.03	0.02
2	正己醇	0.0056	0.57	—	—	—
3	1-辛烯-3-醇	0.0015	1.84	—	—	—
4	2,3-丁二醇	>100	0.00	—	—	—
5	十二醇	0.016	2.81	1.83	1.18	2.02
6	芳樟醇	0.00022	—	17.30	—	14.11
7	辛醇	0.1258	—	—	—	0.02
8	2-正戊基呋喃	0.0058	0.87	—	0.98	—
9	正己醛	0.005	43.44	35.92	44.39	23.88
10	正辛醛	0.0008	37.48	31.96	36.74	27.85
11	壬醛	0.0011	100.00	100.00	100.00	100.00
12	反-2-辛烯醛	0.003	4.46	2.85	3.93	2.52
13	癸醛	0.003	3.92	3.60	3.70	3.04
14	反式-2-壬醛	0.00019	24.51	20.44	16.87	19.78
15	反式-2-癸烯醛	0.0004	8.46	—	8.39	—
16	十四烷醛	0.11	0.03	—	—	—
17	戊醛	0.012	—	1.45	—	—
18	异戊醛	0.0011	—	—	—	4.89
19	己酸	3	0.00	0.00	—	—
20	辛酸	3	0.00	0.00	0.00	—
21	正癸酸	5	0.00	0.00	0.00	0.00
22	5-甲基-2-己酮	0.062	0.66	0.47	0.39	0.51
23	甲基壬基甲酮	0.0055	0.59	0.70	—	—
24	十二烷	10	0.00	—	—	—
25	十一烷	10	0.01	0.00	0.00	0.00
26	正十五烷	1	0.01	0.01	0.00	0.01
27	丁位癸内酯	0.066	0.20	0.27	0.17	0.18
28	棕榈酸甲酯	2	0.01	—	0.00	0.00
29	丁位十二内酯	0.098	0.06	0.08	0.06	0.06
30	邻苯二甲酸二异丁酯	0.03	0.36	—	—	—
31	γ-十二内酯	0.002	—	—	1.32	—

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表 3 主成分方差贡献率

Table 3. Principal component variance contribution rate

成分	初始特征值			提取载荷平方和
成分	总计	方差百分比（%）	累积（%）	总计	方差百分比（%）	累积（%）
1	8.14	42.840	42.840	8.14	42.840	42.840
2	6.895	36.292	79.132	6.895	36.292	79.132
3	3.965	20.868	100	3.965	20.868	100

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表 4 因子载荷矩阵

Table 4. Factor loading matrix

挥发性成分	主成分
挥发性成分	1	2	3
正己醇	−0.04	1.00	−0.08
1-辛烯-3-醇	−0.04	1.00	−0.08
十二醇	−0.65	0.74	0.17
芳樟醇	−0.57	−0.30	0.77
2-正戊基呋喃	0.90	0.43	0.10
正己醛	0.95	0.18	−0.24
正辛醛	0.99	0.08	0.08
壬醛	0.42	−0.67	0.61
反-2-辛烯醛	0.86	0.52	0.06
癸醛	1.00	−0.05	−0.03
反式-2-壬醛	−0.51	0.83	0.24
反式-2-癸烯醛	0.86	0.51	0.09
戊醛	−0.33	−0.42	−0.85
异戊醛	−0.57	−0.30	0.77
5-甲基-2-己酮	−0.50	0.79	0.35
甲基壬基甲酮	−0.35	0.36	−0.87
丁位癸内酯	−0.29	−0.54	−0.79
邻苯二甲酸二异丁酯	−0.04	1.00	−0.08
γ−十二内酯	0.95	−0.28	0.16

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