气味指纹技术的建立及其在腌腊肉制品中的应用
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摘要
风味是食品最重要的感官品质和指标之一,主体风味成分的确定是过去几十年里食品风味研究的热点和难点。食品中挥发性化合物的检测技术已经非常成熟,最主要的困难是缺乏一种对主体风味成分的综合评价方法体系,过去一般采用主成分分析、判别分析、聚类分析、方差分析等统计学方法,但这些方法都是基于化合物含量进行分析的,没有考虑到人类嗅觉对不同物质敏感程度的差异。
腌腊肉制品是中国传统食品的杰出代表,因其具有浓郁的特色风味而著称于世。干腌火腿、腊肠和腊肉是三种最具典型的中国传统腌腊肉制品,它们符合华人对风味食品的消费嗜好,但成分复杂,多年来一直无法准确得知它们的主体风味成分。
本研究的目的主要是：以中国传统腌腊肉制品为主要研究对象,优化食品风味成分的评价方法,研究并建立一种客观而有效地量化确定食品主体风味成分的方法,即气味指纹(图谱)技术,同时建立腌腊肉制品气味指纹图谱,为研究食品风味形成机理、提高产品风味品质、开发新产品等工作提供理论依据。具体研究内容和结果如下：
1气味指纹技术的建立
以金华火腿为试验材料,建立了一种对食品风味成分的综合评价方法——“准内标”转换法；并在此基础上,结合各化合物的感觉阈值,建立了气味指纹(图谱)技术。该技术的具体实施方案为：应用特定的气体采集技术和化合物鉴定仪器分析食品中的挥发性化合物→确定潜在主体风味成分→峰面积归一化处理→计算转换峰浓度→查询相关化合物的感觉阈值→计算各化合物的气味指纹值(OFV)→确定主体风味成分→绘制气味指纹图谱。本研究应用顶空固相微萃取-气相色谱-质谱联用仪分析鉴定腌腊肉制品中的挥发性化合物。
应用该技术分析了来自原产地金华火腿的挥发性成分,结果表明,金华火腿主体风味成分为：二甲基三硫醚、3-甲基丁醛、二甲基二硫醚、1-辛烯-3-醇、辛醛、(E)-2-癸烯醛、壬醛；其它比较重要的风味成分主要包括己醛、庚醛、苯甲醛、苯乙醛、(E)-2-辛烯醛等。而羧酸对金华火腿总体风味没有显著贡献。
2腌腊肉制品气味指纹图谱
以不同来源的三种干腌火腿、五种腊肠和五种腊肉为主要研究对象,应用本研究建立的气味指纹技术,分析了中国传统腌腊肉制品挥发性化合物的组成,确定了主体风味成分。
结果表明,5-10个碳原子的脂肪族醛类化合物是干腌火腿、腊肠和腊肉三类腌腊肉制品主体风味成分的重要组分。但干腌火腿中主要是饱和醛,腊肠中主要是不饱和醛,而3-甲基丁醛则始终是主体风味的重要贡献者。
金华火腿和如皋火腿总体风味相似,宣威火腿因含有较多的芳香组分而产生一定的差异。但三者的总体风味都受到3-甲基丁醛、二甲基二硫醚、二甲基三硫醚的共同影响。
腊肠的主体风味成分主要是：①乙酯类化合物：丁酸乙酯、己酸乙酯、2-甲基丁酸乙酯、3-甲基丁酸乙酯等；②脂肪族醛类化合物：壬醛、辛醛、癸醛、己醛、3-甲基丁醛、(E)-2-壬烯醛等。由乙醇和低级脂肪酸形成的乙酯类化合物是腊肠主体风味成分中最重要的一类物质。
腊肉的主体风味成分主要有三类：①酚类：愈创木酚、2-甲氧基-4-乙烯基苯酚、异丁香酚、2-甲氧基-4-乙基苯酚、2-甲氧基-4-丙基苯酚、2-甲氧基-4-甲基苯酚等；②醛类：(Z)-2-癸烯醛、壬醛、己醛、苯乙醛等；③酯类：丁酸乙酯、己酸乙酯、乙酸乙酯、庚酸乙酯等。酚类化合物对腊肉总体风味具有重要贡献。
Odor is one of the most important sensory properties of food. The definition of Key Odor Compounds has been the most hot but difficult point for odor researchers in the past Although the technology in isolating volatile compounds from food samples has developed well and was applied widely, the great problem in distinguishing Key Odor Compounds is the lack of evaluation methods. Data processing methods such as Principal Components Analysis (PCA), Discriminant Factorial Analysis (DFA), Cluster Analysis (CA), Analysis of Variance (ANOVA), which are based on the content of compounds have been most commonly used in the past. While it was not considered that human olfactory sense changed to various compounds.
Dry-cured meat products are prominent representatives of Chinese traditional food due to their unique odor, among which the Dry-cured Ham, Chinese Sausage and Chinese traditional Smoke-cured Bacon are three types of typical products with great popularity. However, as their volatile compounds are too complicated, their Key Odor Compounds can hardly accurately identified for years.
The aim of this research is to improve evaluation methods in analyzing "volatile compounds of food, such as Chinese traditional dry-cured meat products, to establish a new objective and effective method named Odor Fingerprint Technology (OFT) for identifying Key Odor Compounds, to draw Odor Fingerprint of Chinese traditional dry-cured meat products, and to provide a theory basis in investigating odor formation mechanism, improving odor quality of food and designing new products. The detailed contents and results are as follows.
1. Establishment of Odor Fingerprint Technology
Taken Jinhua Ham as experimental material, an evaluation methods in analyzing volatile compounds of food called "Correcting Quasi-internal Standard" method was established. Together with odor threshold of various volatile compounds, Odor Fingerprint Technology was established. Detailed schemes of the technology are as follows: Volatile compounds isolated from the sample with a certain sampling method coupled with a set of analysis instrument→Potential Key Odor Compounds→Normalization of peak area→Corrected Peak Concentration of the compounds→Odor Fingerprint Value (OFV) of the compounds calculated with their Corrected Peak Concentration and Odor Threshold→Drawing Odor Fingerprint (modified by radar graph). In this thesis, Headspace-Solid Phase Micro-Extraction was taken as an effective sampling method, and Gas Chromatography-Mass Spectrometry as analysis instrument, to analyze volatile compounds isolated from dry-cured meat products.
Volatile compounds isolated from five Jinhua Ham that sampled from an official producer in Jinhua Region, Zhejiang Province was analyzed with Odor Fingerprint Technology. As a result, Dimethyl trisulfide,3-Methyl butanal, Dimethyl disulfide, 1-Octen-3-ol, Octanal, (E)-2-decenal and Nonanal were qualified as Key Odor Compounds of Jinhua Ham. Moreover, Hexanal, Heptanal, Benzaldehyde, Benzeneacetaldehyde and (E)-2-octenal were concerned to be great contributors to its global odor perception. However, carboxylic acids that once correlated to the unique odor of Jinhua Ham contributes nothing to the overall odor of Jinhua Ham.
2. Odor Fingerprint of dry-cured meat products
Volatile compounds isolated from dry-cured hams, Chinese Sausage and Chinese traditional Smoke-cured Bacon with different originals were analyzed, and their Key Odor Compounds were qualified with Odor Fingerprint Technology.
As results shown, C5-C10 aldehydes played an important role in Key Odor Compounds of dry-cured hams, Chinese Sausage and Chinese traditional Smoke-cured Bacon. However, saturated aldehydes are more important for dry-cured hams, unsaturated ones for Chinese Sausage.3-methyl butanal is always significant contributor to the three types of dry-cured meat products.
Overall odor of Jinhua Ham and Rugao Ham were similar to each other, but different from that of Xuanwei Ham with more aromatic compounds. However,3-Methyl butanal, Dimethyl disulfide and Dimethyl trisulfide were common compounds of the three types of hams.
Key Odor Compounds of Chinese Sausage contain ethyl esters that reacted from ethanol and low molecular fatty acids such as Butanoic acid, ethyl ester, Hexanoic acid, ethyl ester,2-Methyl butanoic acid, ethyl ester,3-Methyl butanoic acid, ethyl ester, and so on, while aldehydes (Nonanal, Octanal, Decanal, Hexanal,3-Methyl butanal, (E)-2-Nonenal, et al) also contained.
Key Odor Compounds of Chinese traditional Smoke-cured Bacon contain①Phenols: 2-Methoxy phenol,2-Methoxy-4-vinyl phenol,2-Methoxy-4-(1-propenyl) phenol, 2-Methoxy-4-ethyl phenol,2-Methoxy-4-propyl phenol,2-Methoxy-4-methyl phenol, et al.②aldehydes:(Z)-2-Decenal, Nonanal, Hexanal, Benzeneacetaldehyde, et al.③ethyl esters:Butanoic acid, ethyl ester, Hexanoic acid, ethyl ester, Ethyl acetate, Heptanoic acid, ethyl ester, et al. Among which, phenols made the greatest contribution to the overall odor of Chinese traditional Smoke-cured Bacon.
腌腊肉制品是中国传统食品的杰出代表,因其具有浓郁的特色风味而著称于世。干腌火腿、腊肠和腊肉是三种最具典型的中国传统腌腊肉制品,它们符合华人对风味食品的消费嗜好,但成分复杂,多年来一直无法准确得知它们的主体风味成分。
本研究的目的主要是：以中国传统腌腊肉制品为主要研究对象,优化食品风味成分的评价方法,研究并建立一种客观而有效地量化确定食品主体风味成分的方法,即气味指纹(图谱)技术,同时建立腌腊肉制品气味指纹图谱,为研究食品风味形成机理、提高产品风味品质、开发新产品等工作提供理论依据。具体研究内容和结果如下：
1气味指纹技术的建立
以金华火腿为试验材料,建立了一种对食品风味成分的综合评价方法——“准内标”转换法；并在此基础上,结合各化合物的感觉阈值,建立了气味指纹(图谱)技术。该技术的具体实施方案为：应用特定的气体采集技术和化合物鉴定仪器分析食品中的挥发性化合物→确定潜在主体风味成分→峰面积归一化处理→计算转换峰浓度→查询相关化合物的感觉阈值→计算各化合物的气味指纹值(OFV)→确定主体风味成分→绘制气味指纹图谱。本研究应用顶空固相微萃取-气相色谱-质谱联用仪分析鉴定腌腊肉制品中的挥发性化合物。
应用该技术分析了来自原产地金华火腿的挥发性成分,结果表明,金华火腿主体风味成分为：二甲基三硫醚、3-甲基丁醛、二甲基二硫醚、1-辛烯-3-醇、辛醛、(E)-2-癸烯醛、壬醛；其它比较重要的风味成分主要包括己醛、庚醛、苯甲醛、苯乙醛、(E)-2-辛烯醛等。而羧酸对金华火腿总体风味没有显著贡献。
2腌腊肉制品气味指纹图谱
以不同来源的三种干腌火腿、五种腊肠和五种腊肉为主要研究对象,应用本研究建立的气味指纹技术,分析了中国传统腌腊肉制品挥发性化合物的组成,确定了主体风味成分。
结果表明,5-10个碳原子的脂肪族醛类化合物是干腌火腿、腊肠和腊肉三类腌腊肉制品主体风味成分的重要组分。但干腌火腿中主要是饱和醛,腊肠中主要是不饱和醛,而3-甲基丁醛则始终是主体风味的重要贡献者。
金华火腿和如皋火腿总体风味相似,宣威火腿因含有较多的芳香组分而产生一定的差异。但三者的总体风味都受到3-甲基丁醛、二甲基二硫醚、二甲基三硫醚的共同影响。
腊肠的主体风味成分主要是：①乙酯类化合物：丁酸乙酯、己酸乙酯、2-甲基丁酸乙酯、3-甲基丁酸乙酯等；②脂肪族醛类化合物：壬醛、辛醛、癸醛、己醛、3-甲基丁醛、(E)-2-壬烯醛等。由乙醇和低级脂肪酸形成的乙酯类化合物是腊肠主体风味成分中最重要的一类物质。
腊肉的主体风味成分主要有三类：①酚类：愈创木酚、2-甲氧基-4-乙烯基苯酚、异丁香酚、2-甲氧基-4-乙基苯酚、2-甲氧基-4-丙基苯酚、2-甲氧基-4-甲基苯酚等；②醛类：(Z)-2-癸烯醛、壬醛、己醛、苯乙醛等；③酯类：丁酸乙酯、己酸乙酯、乙酸乙酯、庚酸乙酯等。酚类化合物对腊肉总体风味具有重要贡献。
Odor is one of the most important sensory properties of food. The definition of Key Odor Compounds has been the most hot but difficult point for odor researchers in the past Although the technology in isolating volatile compounds from food samples has developed well and was applied widely, the great problem in distinguishing Key Odor Compounds is the lack of evaluation methods. Data processing methods such as Principal Components Analysis (PCA), Discriminant Factorial Analysis (DFA), Cluster Analysis (CA), Analysis of Variance (ANOVA), which are based on the content of compounds have been most commonly used in the past. While it was not considered that human olfactory sense changed to various compounds.
Dry-cured meat products are prominent representatives of Chinese traditional food due to their unique odor, among which the Dry-cured Ham, Chinese Sausage and Chinese traditional Smoke-cured Bacon are three types of typical products with great popularity. However, as their volatile compounds are too complicated, their Key Odor Compounds can hardly accurately identified for years.
The aim of this research is to improve evaluation methods in analyzing "volatile compounds of food, such as Chinese traditional dry-cured meat products, to establish a new objective and effective method named Odor Fingerprint Technology (OFT) for identifying Key Odor Compounds, to draw Odor Fingerprint of Chinese traditional dry-cured meat products, and to provide a theory basis in investigating odor formation mechanism, improving odor quality of food and designing new products. The detailed contents and results are as follows.
1. Establishment of Odor Fingerprint Technology
Taken Jinhua Ham as experimental material, an evaluation methods in analyzing volatile compounds of food called "Correcting Quasi-internal Standard" method was established. Together with odor threshold of various volatile compounds, Odor Fingerprint Technology was established. Detailed schemes of the technology are as follows: Volatile compounds isolated from the sample with a certain sampling method coupled with a set of analysis instrument→Potential Key Odor Compounds→Normalization of peak area→Corrected Peak Concentration of the compounds→Odor Fingerprint Value (OFV) of the compounds calculated with their Corrected Peak Concentration and Odor Threshold→Drawing Odor Fingerprint (modified by radar graph). In this thesis, Headspace-Solid Phase Micro-Extraction was taken as an effective sampling method, and Gas Chromatography-Mass Spectrometry as analysis instrument, to analyze volatile compounds isolated from dry-cured meat products.
Volatile compounds isolated from five Jinhua Ham that sampled from an official producer in Jinhua Region, Zhejiang Province was analyzed with Odor Fingerprint Technology. As a result, Dimethyl trisulfide,3-Methyl butanal, Dimethyl disulfide, 1-Octen-3-ol, Octanal, (E)-2-decenal and Nonanal were qualified as Key Odor Compounds of Jinhua Ham. Moreover, Hexanal, Heptanal, Benzaldehyde, Benzeneacetaldehyde and (E)-2-octenal were concerned to be great contributors to its global odor perception. However, carboxylic acids that once correlated to the unique odor of Jinhua Ham contributes nothing to the overall odor of Jinhua Ham.
2. Odor Fingerprint of dry-cured meat products
Volatile compounds isolated from dry-cured hams, Chinese Sausage and Chinese traditional Smoke-cured Bacon with different originals were analyzed, and their Key Odor Compounds were qualified with Odor Fingerprint Technology.
As results shown, C5-C10 aldehydes played an important role in Key Odor Compounds of dry-cured hams, Chinese Sausage and Chinese traditional Smoke-cured Bacon. However, saturated aldehydes are more important for dry-cured hams, unsaturated ones for Chinese Sausage.3-methyl butanal is always significant contributor to the three types of dry-cured meat products.
Overall odor of Jinhua Ham and Rugao Ham were similar to each other, but different from that of Xuanwei Ham with more aromatic compounds. However,3-Methyl butanal, Dimethyl disulfide and Dimethyl trisulfide were common compounds of the three types of hams.
Key Odor Compounds of Chinese Sausage contain ethyl esters that reacted from ethanol and low molecular fatty acids such as Butanoic acid, ethyl ester, Hexanoic acid, ethyl ester,2-Methyl butanoic acid, ethyl ester,3-Methyl butanoic acid, ethyl ester, and so on, while aldehydes (Nonanal, Octanal, Decanal, Hexanal,3-Methyl butanal, (E)-2-Nonenal, et al) also contained.
Key Odor Compounds of Chinese traditional Smoke-cured Bacon contain①Phenols: 2-Methoxy phenol,2-Methoxy-4-vinyl phenol,2-Methoxy-4-(1-propenyl) phenol, 2-Methoxy-4-ethyl phenol,2-Methoxy-4-propyl phenol,2-Methoxy-4-methyl phenol, et al.②aldehydes:(Z)-2-Decenal, Nonanal, Hexanal, Benzeneacetaldehyde, et al.③ethyl esters:Butanoic acid, ethyl ester, Hexanoic acid, ethyl ester, Ethyl acetate, Heptanoic acid, ethyl ester, et al. Among which, phenols made the greatest contribution to the overall odor of Chinese traditional Smoke-cured Bacon.
引文
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