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CN102919806A - Lipid aroma condensate prepared through fat thermal oxidation and preparation method thereof - Google Patents

Lipid aroma condensate prepared through fat thermal oxidation and preparation method thereof Download PDF

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Publication number
CN102919806A
CN102919806A CN2012102411841A CN201210241184A CN102919806A CN 102919806 A CN102919806 A CN 102919806A CN 2012102411841 A CN2012102411841 A CN 2012102411841A CN 201210241184 A CN201210241184 A CN 201210241184A CN 102919806 A CN102919806 A CN 102919806A
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fat
concentrate
fragrant concentrate
fragrant
thermal oxide
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谢建春
曾慧英
高远
郑福平
陈海涛
孙宝国
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Beijing Technology and Business University
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Beijing Technology and Business University
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Abstract

本发明公开了一种以脂肪为原料采用加热氧化、降解两步工艺制备脂香浓缩物的方法及其产物。具体方法为:第一步、在抗氧化剂和水的存在下,将脂肪通入空气加热搅拌氧化,空气流量0.1~2m3/kg.h,温度100~180℃,时间0.5~5h,搅拌速度200~1000rpm/min;第二步、将第一步所得产物通入氮气加热降解,氮气流量0.1~0.5m3/kg.h,加热温度100~180℃,时间0.5~6h。所得产品脂香浓郁、和谐、圆润,可作为热反应香精原料使用,也可作为天然食品添加剂在鸡精、方便面调料、汤料、香肠、罐头、速冻水饺等多种调味料或食品中直接使用。The invention discloses a method and a product thereof for preparing a fat aroma concentrate by using fat as a raw material and adopting a two-step process of heating, oxidation and degradation. The specific method is as follows: the first step, in the presence of antioxidants and water, put the fat into the air to heat and stir to oxidize, the air flow rate is 0.1-2m 3 /kg.h, the temperature is 100-180°C, the time is 0.5-5h, and the stirring speed is 200-1000rpm/min; the second step, the product obtained in the first step is passed through nitrogen to heat and degrade, the nitrogen flow rate is 0.1-0.5m 3 /kg.h, the heating temperature is 100-180°C, and the time is 0.5-6h. The resulting product has a rich, harmonious and mellow fat aroma, and can be used as a raw material for heat-reactive flavors, or as a natural food additive in various seasonings or foods such as chicken essence, instant noodle seasoning, soup, sausage, canned food, and quick-frozen dumplings.

Description

一种脂肪热氧化制备的脂香浓缩物及制备方法Fat aroma concentrate prepared by thermal oxidation of fat and preparation method thereof

技术领域 technical field

本发明涉及一种以脂肪为原料经加热氧化、降解两步工艺制备脂香浓缩物的方法及其产品,所得脂香浓缩物脂香浓郁、和谐、圆润,可作为热反应香精原料使用,也可作为天然食品添加剂直接用于食品中。The invention relates to a method for preparing a fat aroma concentrate by using fat as a raw material through a two-step process of heating, oxidation and degradation and the product thereof. The obtained fat aroma concentrate has a rich, harmonious and mellow fat aroma, which can be used as a raw material for heat-reactive essence, and also It can be directly used in food as a natural food additive.

背景技术 Background technique

本发明涉及一种将脂肪热氧化制备脂香浓缩物的方法及其产品,所得脂香浓缩物脂香浓郁、和谐、圆润。The invention relates to a method for preparing a fat aroma concentrate by thermally oxidizing fat and the product thereof. The obtained fat aroma concentrate has a strong, harmonious and mellow fat aroma.

脂肪自动氧化产生令人不愉快的酸败气味,但一定条件下的脂肪热氧化,可生成具有浓郁油脂香、煎炸香的氧化产物。脂肪氧化产生的嗅感物质主要包括烃类、醛类、酮类、呋喃类等,其中脂肪族的醛和酮是构成脂香的主体成分,它们与烃类、呋喃类成分以适当配比组合,可形成令人喜爱的脂香、煎炸香。在热反应肉味香精制备中,脂肪族醛还可作为前体参与美拉德反应,生成阈值较低的杂环肉香成分。现有专利(孙宝国、谢建春、梁梦兰、彭秋菊、文志勇.一种脂肪控制氧化制备肉味香精前体物的方法ZL200410030864.4)采用无水条件下、通空气、加热的氧化工艺,制备富含小分子醛、酮的脂肪氧化产物,该氧化产物有较高的过氧化值、较高的羰基含量值、较低的酸值,脂香浓郁,用于热反应中(提供肉香前体物),所得肉味香精优点为肉的特征香气明显,风味饱满,但这种具有较高过氧化值的氧化产物,会导致所添加食品产品过氧化值较高不符合产品相关标准(国标对各种食品产品的过氧化值有控制要求),还可能因其在食品中自动氧化降解形成不良风味,不宜在食品中直接添加使用。Auto-oxidation of fat produces an unpleasant rancid smell, but thermal oxidation of fat under certain conditions can produce oxidation products with rich oily aroma and frying aroma. The olfactory substances produced by fat oxidation mainly include hydrocarbons, aldehydes, ketones, furans, etc., among which aliphatic aldehydes and ketones are the main components of fat fragrance, and they are combined with hydrocarbons and furans in an appropriate ratio , can form a pleasing aroma of fat and frying. In the preparation of heat-reactive meat flavors, aliphatic aldehydes can also be used as precursors to participate in the Maillard reaction to generate heterocyclic meat flavor components with a lower threshold. Existing patents (Sun Baoguo, Xie Jianchun, Liang Menglan, Peng Qiuju, Wen Zhiyong. A method for preparing meat flavor flavor precursors through controlled oxidation of fat ZL200410030864.4) adopt an oxidation process under anhydrous conditions, air ventilation, and heating to prepare Fat oxidation products rich in small molecular aldehydes and ketones. The oxidation products have higher peroxide value, higher carbonyl content value, lower acid value, and rich fat aroma. They are used in thermal reactions (providing meat aroma before) body), the advantage of the meat flavor obtained is that the characteristic aroma of meat is obvious and the flavor is full, but this oxidation product with a higher peroxide value will cause the added food product to have a higher peroxide value and not meet the relevant product standards (national standard There are control requirements for the peroxide value of various food products), and it may also cause bad flavor due to automatic oxidation and degradation in food, so it is not suitable for direct addition and use in food.

为解决现有技术中因所得脂肪氧化产物过氧化值较高而不适于在食品中直接添加使用的问题,本申请通过先通空气加热氧化、再在氮气条件下加热降解方法,提供了一种安全、易工业生产的低过氧化值、低酸值、高羰基含量值的脂香浓缩物制备方法,并得到了一种新型的具有低过氧化值的脂香浓缩物。这种低过氧化值的脂香浓缩物及其制备方法在现有技术中未见报道。In order to solve the problem in the prior art that the obtained fat oxidation product is not suitable for direct addition and use in food due to its high peroxide value, this application provides a The invention discloses a method for preparing a fat aroma concentrate with low peroxide value, low acid value and high carbonyl content value which is safe and easy for industrial production, and obtains a new type of fat aroma concentrate with low peroxide value. This low peroxide value fat aroma concentrate and its preparation method have not been reported in the prior art.

发明内容 Contents of the invention

本发明的目的是提供一种采用加热氧化、降解两步工艺获得脂香浓缩物的方法。此法克服了现有方法的缺点和不足。采用该工艺制备的脂香浓缩物,具有较低过氧化值、较高羰基含量值、较低酸值,不仅脂香浓郁,且香气和谐、圆润,既可作为热反应香精原料使用,也可作为天然食品添加剂在食品中直接使用。The object of the present invention is to provide a method for obtaining a fat aroma concentrate by adopting a two-step process of heating, oxidation and degradation. This method overcomes the shortcomings and deficiencies of the existing methods. The fat aroma concentrate prepared by this process has a lower peroxide value, a higher carbonyl content value, and a lower acid value. It not only has a rich fat aroma, but also has a harmonious and round aroma. It is used directly in food as a natural food additive.

本发明所采用的技术方案如下:The technical scheme adopted in the present invention is as follows:

一种脂肪热氧化制备脂香浓缩物的方法,以脂肪为原料,由加热氧化、降解两步工艺组成,第一步、在0.01~0.8wt%的抗氧化剂存在下加热,到达反应温度100~180℃时,加入脂肪量0.5~6wt%液体,维持100~180℃的反应温度,开始搅拌、通入空气并计时,进行氧化反应,时间0.5~5h;第二步、将第一步所得产物通入氮气加热降解,反应温度100~180℃,时间0.5~6h。A method for preparing fat aroma concentrate by thermal oxidation of fat, which uses fat as raw material and consists of a two-step process of heating oxidation and degradation. The first step is to heat in the presence of 0.01-0.8 wt% antioxidant to reach a reaction temperature of 100-100 At 180°C, add 0.5-6wt% fat liquid, maintain the reaction temperature of 100-180°C, start stirring, feed air and time, and carry out oxidation reaction for 0.5-5 hours; the second step is to prepare the product obtained in the first step Introduce nitrogen to heat and degrade, the reaction temperature is 100-180°C, and the time is 0.5-6h.

本发明所述脂肪为动物脂肪、植物油、脂肪酸三甘酯、天然不饱和脂肪酸的一种、或者上述各种油脂的组合。所述抗氧化剂为维生素C或维生素E或者两者的组合,抗氧化剂加入量为脂肪量的0.01~0.8wt%。The fat described in the present invention is one of animal fat, vegetable oil, fatty acid triglyceride, natural unsaturated fatty acid, or a combination of the above-mentioned various oils and fats. The antioxidant is vitamin C or vitamin E or a combination of the two, and the added amount of the antioxidant is 0.01-0.8% by weight of the fat.

本发明所述液体为自来水、矿泉水、蒸馏水、去离子水、或质量浓度为0.5~10%的氯化钠溶液;液体的加入量为脂肪量的0.5~6wt%。特别当使用氯化钠溶液时,水的蒸发损失较小,反应温度较稳定。The liquid in the present invention is tap water, mineral water, distilled water, deionized water, or sodium chloride solution with a mass concentration of 0.5-10%. The added amount of the liquid is 0.5-6 wt% of the fat content. Especially when sodium chloride solution is used, the evaporation loss of water is small and the reaction temperature is relatively stable.

本发明所述空气,由空气压缩机提供,不应含任何有毒、有害成分,经分子筛、或活性炭过滤处理。空气流量控制在0.1~2m3/kg.h。The air described in the present invention is provided by an air compressor, should not contain any poisonous or harmful components, and is filtered through molecular sieves or activated carbon. The air flow rate is controlled at 0.1~2m 3 /kg.h.

本发明所述氮气,可用钢瓶或氮气发生器提供,不应含任何有毒、有害成分,可为普通氮气或高纯氮气。氮气流量控制在0.1~0.5m3/kg.h。The nitrogen described in the present invention can be provided by steel cylinders or nitrogen generators, should not contain any poisonous and harmful components, and can be ordinary nitrogen or high-purity nitrogen. The nitrogen flow rate is controlled at 0.1-0.5m 3 /kg.h.

本发明所述反应温度,低于厨房煎、炸条件下的油温温度,为100~180℃,优选120~160℃。第一步与第二步的反应温度可相同或不同。The reaction temperature of the present invention is lower than the oil temperature under kitchen frying and frying conditions, and is 100-180°C, preferably 120-160°C. The reaction temperatures of the first step and the second step may be the same or different.

本发明所述氧化时间,依加水量、加热温度、通空气量等其他条件改变,氧化时间一般为0.5~5h。The oxidation time of the present invention varies according to other conditions such as the amount of water added, heating temperature, and air flow, and the oxidation time is generally 0.5 to 5 hours.

本发明所述降解时间,依第一步所得产物的指标(过氧化值、酸值、羰基含量值)、第二步加热温度、通氮气量等其他条件改变,当第一步产物的过氧化值较高或第二步加热降解温度较低时,所需降解时间会较长。加热降解时间一般为0.5~6h,优选1~2h。The degradation time of the present invention changes according to other conditions such as the index (peroxide value, acid value, carbonyl content value) of the product obtained in the first step, the heating temperature of the second step, the nitrogen flow rate, etc., when the peroxidation of the first step product When the value is higher or the second heating degradation temperature is lower, the required degradation time will be longer. The heating degradation time is generally 0.5-6 hours, preferably 1-2 hours.

本发明的搅拌采用电动机械搅拌,搅拌速率为200~1000r.min-1,400~700r.min-1较佳。The stirring of the present invention adopts electromechanical stirring, and the stirring rate is 200-1000r.min -1 , preferably 400-700r.min -1 .

本发明第一步所得产物过氧化值为15~170meq氧/kg,最好为60~100meq氧/kg,酸值为0.5~2g KOH/kg或更小,最好<1g KOH/kg,羰基含量值为0.1~2%,最好为0.1~1.2%。本发明所得脂香浓缩物过氧化值为0~2meq氧/kg,最好为0meq氧/kg,酸值为0.5~2g.KOH/kg或更小,最好<1.0g KOH/kg,羰基含量值为0.1~2%,最好为0.6~1%。(过氧化值的分析方法参见:IOPAC,standard methods for the analysis of oils,fats and derivatives,the 6th,P199-200和P210-211页。酸值的分析方法参见:食品分析法,钱毅赵国君译,上海科学普及出版社。总羰基含量分析方法参见:有机半微量定性分析,科学出版社,P305-309页)。The peroxide value of the product obtained in the first step of the present invention is 15-170meq oxygen/kg, preferably 60-100meq oxygen/kg, and the acid value is 0.5-2g KOH/kg or less, preferably <1g KOH/kg, carbonyl The content is 0.1-2%, preferably 0.1-1.2%. The peroxide value of the fat incense concentrate obtained in the present invention is 0~2meq oxygen/kg, preferably 0meq oxygen/kg, and the acid value is 0.5~2g.KOH/kg or less, preferably <1.0g KOH/kg, carbonyl The content is 0.1-2%, preferably 0.6-1%. (For the analysis method of peroxide value, please refer to: IOPAC, standard methods for the analysis of oils, fats and derivatives, the 6th, P199-200 and P210-211 pages. For the analysis method of acid value, please refer to: Food Analysis Method, Qian Yi Zhao Guojun Translated, Shanghai Science Popularization Press. For the analysis method of total carbonyl content, see: Organic semi-trace qualitative analysis, Science Press, P305-309 pages).

本发明所述脂肪热氧化制备脂香浓缩物的方法,可以有效降低脂肪氧化产物的过氧化值、并保持较高的羰基含量值、较低酸值,常压氮气条件下降解的方式对设备要求低,安全性能好,且能防止降解所得醛、酮等羰基化合物的再次氧化,提高产品的产率。The method for preparing fat aroma concentrate by thermal oxidation of fat in the present invention can effectively reduce the peroxide value of fat oxidation products, and maintain a higher carbonyl content value and lower acid value. The requirement is low, the safety performance is good, and it can prevent the re-oxidation of carbonyl compounds such as aldehydes and ketones obtained by degradation, and improve the yield of products.

本发明所得脂香浓缩物产品,为一种具有较低过氧化值、较高羰基含量值、较低酸值的氧化产物,脂香浓郁,香气和谐、圆润,既可作为热反应香精原料使用,也可作为天然食品添加剂在鸡精、方便面调料、汤料、香肠、罐头、速冻水饺等多种调味料或食品中直接使用。The fat aroma concentrate product obtained in the present invention is an oxidation product with a lower peroxide value, a higher carbonyl content value, and a lower acid value. It can also be used as a natural food additive in various seasonings or foods such as chicken essence, instant noodle seasoning, soup, sausage, canned food, and quick-frozen dumplings.

具体实施方式: Detailed ways:

实施例1Example 1

在装有电动搅拌器、温度计、回流冷凝管的500ml四口烧瓶中,加入100g猪脂、0.05gVE,加热到达130℃时,加入5mL氯化钠溶液(浓度10%),维持130℃,开始搅拌、通入空气(经活性炭过滤)并计时,空气流速0.24m3/kg.h,搅拌速度500r.min-1,氧化1.5h,停止反应,测得过氧化值为70meq氧/kg脂肪、酸值为0.69g.KOH/kg脂肪,羰基含量为1.17%。In a 500ml four-neck flask equipped with an electric stirrer, a thermometer, and a reflux condenser, add 100g of lard and 0.05gVE, and when the temperature reaches 130°C, add 5mL of sodium chloride solution (concentration: 10%), maintain 130°C, and start Stir, feed air (filtered by activated carbon) and time, the air flow rate is 0.24m 3 /kg.h, the stirring speed is 500r.min -1 , oxidize for 1.5h, stop the reaction, the measured peroxide value is 70meq oxygen/kg fat, The acid value is 0.69g.KOH/kg fat, and the carbonyl content is 1.17%.

改通氮气、加热继续实验,氮气流量0.1m3/kg.h,到达温度160℃时开始计时,加热降解2h,产品为乳白色,过氧化值为0.5meq氧/kg脂肪,酸值为1.56g.KOH/kg脂肪,羰基含量为0.66%。Change to nitrogen, heat to continue the experiment, the nitrogen flow rate is 0.1m 3 /kg.h, start timing when the temperature reaches 160°C, heat and degrade for 2 hours, the product is milky white, the peroxide value is 0.5meq oxygen/kg fat, and the acid value is 1.56g .KOH/kg fat, the carbonyl content is 0.66%.

实施例2Example 2

在装有电动搅拌器、温度计、回流冷凝管的500ml四口烧瓶中,加入100g牛脂,0.04gVE,到达温度125℃时,加入3mL水,维持125℃,开始搅拌、通入空气(经分子筛过滤)并计时,空气流量为0.12m3/kg.h,搅拌速度700r.min-1,氧化2h,停止反应,测得过氧化值100meq氧/kg脂肪、酸值0.8gKOH/kg脂肪、羰基含量1.3%。In a 500ml four-necked flask equipped with an electric stirrer, a thermometer, and a reflux condenser, add 100g of tallow and 0.04gVE , when the temperature reaches 125°C, add 3mL of water, keep it at 125°C, start stirring, and introduce air (through molecular sieves) Filtration) and timing, the air flow rate is 0.12m 3 /kg.h, the stirring speed is 700r.min -1 , oxidized for 2h, stop the reaction, the measured peroxide value is 100meq oxygen/kg fat, acid value is 0.8gKOH/kg fat, carbonyl Content 1.3%.

改通氮气、加热继续实验,氮气流量0.2m3/kg.h,到达温度156℃时开始计时,加热降解3h,产品为乳白色,过氧化值为2.0meq氧/kg脂肪,酸值为1.63g.KOH/kg脂肪,羰基含量为0.75%。Change to nitrogen, heat to continue the experiment, the nitrogen flow rate is 0.2m 3 /kg.h, start timing when the temperature reaches 156°C, heat and degrade for 3 hours, the product is milky white, the peroxide value is 2.0meq oxygen/kg fat, and the acid value is 1.63g .KOH/kg fat, the carbonyl content is 0.75%.

实施例3Example 3

在装有电动搅拌器、温度计、回流冷凝管的500ml四口烧瓶中,加入100g鸡脂,0.08g VE,到达温度120℃时,加入2mL氯化钠溶液(5%),维持温度120℃,开始搅拌、通入空气(活性炭过滤)并计时,空气流量为0.24m3/kg.h,搅拌速度700r.min-1,氧化0.5h,测得过氧化值为76meq氧/kg脂肪、酸值为0.47g.KOH/kg脂肪,羰基含量为1.08%;In a 500ml four-neck flask equipped with an electric stirrer, a thermometer, and a reflux condenser, add 100g of chicken fat and 0.08g of V E , and when the temperature reaches 120°C, add 2mL of sodium chloride solution (5%) to maintain the temperature at 120°C , start stirring, feed air (activated carbon filter) and time, the air flow rate is 0.24m 3 /kg.h, the stirring speed is 700r.min -1 , oxidize for 0.5h, and the measured peroxide value is 76meq oxygen/kg fat, acid The value is 0.47g.KOH/kg fat, and the carbonyl content is 1.08%;

改通氮气、加热继续实验,氮气流量0.4m3/kg.h,当到达温度160℃时开始计时,加热降解2h,产品为淡黄色,过氧化值为0meq氧/kg脂肪,酸值为0.95g.KOH/kg脂肪,羰基含量为1.2%。Change to nitrogen and continue the experiment with heating. The nitrogen flow rate is 0.4m 3 /kg.h. When the temperature reaches 160°C, start timing. Heat and degrade for 2 hours. The product is light yellow, the peroxide value is 0meq oxygen/kg fat, and the acid value is 0.95 g. KOH/kg fat, the carbonyl content is 1.2%.

Claims (9)

1. a fatty thermal oxide prepares the method for the fragrant concentrate of fat, it is characterized in that: take fat as raw material, formed by heated oxide, degraded two step process, the first step, heating in the presence of the antioxidant of 0.01~0.8wt% when arriving 100~180 ℃ reaction temperature, add the liquid of 0.5~6wt% of fat mass, keep 100~180 ℃ reaction temperature, begin to stir, pass into air and timing, carry out oxidation reaction, the time is 0.5~5h; Second step, first step products therefrom is passed into nitrogen add thermal degradation, 100~180 ℃ of reaction temperatures, time 0.5~6h.
2. described fatty thermal oxide prepares the method for the fragrant concentrate of fat according to claim 1, and it is characterized in that: fat is a kind of for animal tallow or vegetable oil or aliphatic acid triglyceride or natural unrighted acid, or the combination of above-mentioned various greases.
3. described fatty thermal oxide prepares the method for the fragrant concentrate of fat according to claim 1, and it is characterized in that: described liquid is running water or mineral water or distilled water or deionized water, or mass concentration is 0.5~10% sodium chloride solution.
4. described fatty thermal oxide prepares the method for the fragrant concentrate of fat according to claim 1, and it is characterized in that: the flow that passes into air during first step oxidation reaction is 0.1~2m 3/ kg.h, mixing speed is 200~1000r.min -1, the flow when second step passes into nitrogen is 0.1~0.5m 3/ kg.h, the reaction temperature of the first step and second step is identical or different, and reaction temperature is 120~160 ℃.
5. described fatty thermal oxide prepares the method for the fragrant concentrate of fat according to claim 1, and it is characterized in that: described antioxidant is vitamin C or vitamin E or both combinations.
6. described fatty thermal oxide prepares the method for the fragrant concentrate of fat according to claim 1, and it is characterized in that: the peroxide value of the fragrant concentrate of gained fat is 0~2meq oxygen/kg, and acid number is 0.5~2g.KOH/kg, and carbonyl content is 0.1~2%.
7. the fragrant concentrate of the fat that obtains of one of described method according to claim 1-6, it is characterized in that: the peroxide value of the fragrant concentrate of gained fat is 0~2meq oxygen/kg, and acid number is 0.5~2g.KOH/kg, and carbonyl content is 0.1~2%.
8. the fragrant concentrate of described fat according to claim 7 is characterized in that peroxide value is 0meq oxygen/kg, and acid number<1.0gKOH/kg, carbonyl content are 0.6~1%.
9. the purposes of the fragrant concentrate of described fat according to claim 7 is characterized in that preparing meat flavor or directly using in flavoring or food as natural additive for foodstuff as the thermal response raw material.
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CN105876730A (en) * 2016-05-03 2016-08-24 北京工商大学 Fat-flavored concentrate as well as preparation method and application thereof
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CN115644411A (en) * 2022-10-28 2023-01-31 湖南文理学院 Meat flavor based on aquatic product processing by-products and preparation method thereof
CN119073443A (en) * 2024-09-18 2024-12-06 广东鹰金钱海宝食品有限公司 A method for preparing lecithin flavor base by thermal oxidation

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