JPH04214799A - Production of novel vanilla extract - Google Patents

Abstract

PURPOSE:To obtain a vanilla extract having a top aroma and a concentrated aromatic body feeling by extracting the aromatic ingredients of vanilla beans with the CO2 of a supercritical state (-near state) and subsequently extracting ingredients mainly comprising taste ingredients with an organic solvent. CONSTITUTION:Vanilla beans such as bourbon vanilla beans are treated with the CO2 of a supercritical state or its near state to extract ingredients mainly comprising aromatic ingredients in the beans. Ingredients mainly comprising taste ingredients are subsequently extracted from the treatment residues with a polar organic solvent comprising a monohydric alcohol, a polyhydric alcohol, a ketone, etc., (preferably ethanol or glycerol).

Description

DETAILED DESCRIPTION OF THE INVENTION [Industrial Application Field] The present invention relates to a method for producing a novel vanilla extract that has both a top aroma and a rich and mellow body feel, is rich in natural taste, and has excellent palatability.

More specifically, the present invention provides vanilla beans with water and/or
or a step of extracting and collecting the aroma-based components in the material into the carbon dioxide by treating it with carbon dioxide in a supercritical state or a state near it in the presence or absence of alcohol; The present invention relates to a novel method for producing vanilla extract, which comprises a step of extracting and collecting components mainly having flavor from a residue after treatment using a water-miscible organic solvent.

[Conventional technology] The unique aroma of vanilla extract is obtained after harvesting vanilla beans.
It is formed through a process called curing, in which vanilla beans are dried, fermented, and aged.

In the old days, vanilla beans were crushed and mixed into food and drinks for use, but now they are used in the form of extracts obtained by extracting vanilla beans with hydroalcohol, etc. It's being used.

As a method for obtaining vanilla extract, a solvent extraction method such as hydrous alcohol has been commonly used, but it has the disadvantage that the aroma immediately after extraction is extremely monotonous and lacks a mellow ripeness. In recent years, a method of extraction using carbon dioxide has been proposed.
Extracted with carbon dioxide at a pressure of 350 bar,
A method for extracting the aromatic substances of vanilla shell is disclosed in which the extract is separated at a temperature of 30 DEG C. and a pressure of 30 to 60 bar (Japanese Patent Application Laid-open No. 74797/1983).

[Problems to be Solved by the Invention] The above-mentioned conventional proposals each have their own advantages and disadvantages, and are not necessarily satisfactory. For example, water extraction sufficiently extracts water-soluble taste components, but hardly any aroma components, and conversely, extraction with an organic solvent does not sufficiently extract taste components. On the other hand, extraction with a water-containing organic solvent yields an extract with a relatively good balance and rich body feel, but it has the drawback of lacking top aroma.

On the other hand, an extract obtained by carbon dioxide extraction in a supercritical state or a state close to it yields aromatic components rich in top aroma, but an extract obtained by carbon dioxide extraction in a supercritical state or a state near it can be obtained by extraction with an organic solvent. Compared to other varieties, it is generally characterized by a top aroma, but on the other hand, it has the disadvantage of producing only a monotonous aroma lacking in richness, ripeness, thickness, richness, and rounded body. According to the research conducted by the present inventors, it has been found that this drawback cannot be compensated for even by adding water, alcohol, or other extraction aids to carbon dioxide in a supercritical state.

[Means for Solving the Problems] The present inventors have conducted extensive research to solve these problems. As a result, vanilla beans are treated with carbon dioxide in a supercritical state or a state near it in the presence or absence of water and/or alcohols to remove the aroma-based components in the material. The above-mentioned drawbacks can be solved all at once by combining the process of extracting and collecting the taste from the residue after the above-mentioned treatment using a water-miscible organic solvent. It was discovered that a novel vanilla extract can be obtained.

Therefore, the purpose of the present invention is to utilize the respective characteristics of supercritical carbon dioxide extraction method and organic solvent extraction method to create a high-quality, well-balanced aroma and flavor with a sharp natural top aroma, a feeling of ripeness, and a sense of body. The present invention provides a method for producing vanilla extract having the following properties.

Vanilla beans used in the present invention can be of any variety that is easily available on the market. Examples of such vanilla beans include Bourbon vanilla beans, Mexican vanilla beans, Indonesian vanilla beans, and Tahitian vanilla beans.

In the present invention, first, the vanilla beans as described above are extracted with carbon dioxide in a supercritical state or a state near it to extract and collect components mainly consisting of aroma. During extraction, in addition to the water derived from vanilla beans, water and/or alcohol can be added as an extraction aid if desired.

Examples of such alcohols include monohydric alcohols such as methanol, ethanol, n-propyl alcohol, isopropyl alcohol, butanol, 2-butanol, and t-butanol; ethylene glycol, propylene glycol, glycerin, and 1,3-butylene glycol. Examples include polyhydric alcohols such as , 1,2-butylene glycol and the like. These alcohols can be used alone or in any mixture, but ethanol, glycerin, and any mixture thereof are particularly preferred.

The amount of water or alcohol used above is generally
Approximately 0.1-1000 for the vanilla beans used
The amount may be about 1% by weight, preferably about 1 to 100% by weight.

In addition, when using a mixture system of water and alcohol, the mixing ratio of water and alcohol can be selected arbitrarily.
Usually, a range of water:alcohol=5:95 to 70:30 is often adopted.

Furthermore, the amount of these mixed solvents used is within the same range as the amount of water or alcohol used above.

Carbon dioxide in a supercritical state or a state near it in the present invention refers to a critical temperature (31.0°C) and a critical pressure (72.9a
tm) or a fluid in a state near it.

The carbon dioxide in the extraction process of the present invention is generally at a pressure of 70 to 300 kg/cm2, preferably 80 kg/cm2.
~200 kg/cm2 is commonly used. pressure is 3
If it exceeds 00 kg/cm2, the extraction rate of fats and oils other than aroma components will increase, which is not preferable.

Extraction temperature is 20-150°C, preferably 20-80°C
Selected from a range of degrees. The process is carried out using carbon dioxide in a supercritical or near supercritical state using an appropriate combination of these temperatures and pressures.

Next, by treating the residue after performing carbon dioxide extraction as described above with a water-miscible organic solvent, components mainly having taste can be extracted and collected. Such water-miscible organic solvents include, for example, methanol, ethanol,
Monohydric alcohols such as n-propyl alcohol, isopropyl alcohol, butanol, 2-butanol, t-butanol; ethylene glycol, propylene glycol, glycerin, 1,3-butylene glycol, 1,2
- Polyhydric alcohols such as butylene glycol: Examples include ketones such as acetone and methyl ethyl ketone. These alcohols and ketones can be used alone or in any mixture.

Further, the above-mentioned water-miscible organic solvents can also be used in the form of water-containing substances. There are no particular restrictions on the mixing ratio of water-miscible organic solvent and water in this case, but the weight ratio is preferably about 95:5 to about 20:80, particularly preferably about 60:4.
A ratio of about 0 to about 30:70 can be mentioned.

The amount of the solvent to be used when extracting the carbon dioxide extraction residue of vanilla beans with these water-miscible organic solvents can be arbitrarily selected, but generally it is about 1 to 1 part by weight of the solvent per 1 part by weight of the residue. A range of about 100 parts by weight, preferably about 2 to 20 parts by weight, is employed.

The conditions for solvent extraction are often such that the extraction temperature is from about 20°C to the boiling point temperature of the solvent used, preferably from about 40 to about 60°C, for about 10 minutes to about 6 hours, preferably about 30 minutes to 2 hours. Adopted. Extraction can be performed by standing still or stirring, or if desired, the carbon dioxide extraction residue of vanilla beans can be packed into a column and continuous extraction can be performed using a water-miscible organic solvent.

After the extraction is completed, the extract can be collected by filtration, centrifugation, etc. using known methods, and the solvent can be further removed from the extract to obtain a concentrate mainly having a taste.

The water-miscible organic solvent extract mainly for flavor and the carbon dioxide extract mainly for aroma obtained by the present invention can be used alone, but by mixing them, it is possible to create a top aroma. A novel vanilla extract with an excellent balance of aroma and flavor with a good body feeling can be obtained.

Although the mixing ratio of aroma components and taste components can be arbitrarily selected, generally, the total amount of the extract obtained by each operation is mixed at the same ratio.

According to the present invention, by mixing an extract mainly containing the aroma of vanilla beans and an extract mainly containing taste components, the flavor of each vanilla bean is improved compared to conventional extracts of this type. It is possible to obtain a novel, rich and long-lasting vanilla extract that has a well-balanced combination of a pleasant fresh top aroma and an oily body feel.

The vanilla extract obtained by the present invention can be used, for example, in beverages,
Various desserts such as Western confectionery, fermented milk, and ice cream; Various foods such as cookies, candies, bakery products, snack foods, chocolate and tobacco flavors, luxury goods, health and hygiene products, pharmaceuticals, cosmetics, etc. It can be used in various fields.

The amount of the vanilla extract of the present invention added to the above-mentioned foods and drinks can be arbitrarily selected, but generally a range of about 0.01 to 1% is adopted based on the weight of these foods and drinks. Ru.

EXAMPLES Hereinafter, excellent aspects of the present invention will be explained in more detail with reference to Examples.

[Example] Example 1 Vanilla chopped into approximately 1 cm pieces was placed in an extraction tower with a capacity of 5 liters.
Filled with 1 kg of beans (produced in Madagascar), the extraction temperature was 40°C and the pressure was 200 kg/kg by the process shown in Figure 1.
A pale yellow extract with a fresh top aroma is extracted using supercritical carbon dioxide (cm2) at a temperature of 30°C in a separator and a pressure of 50kg/cm2.
0g and 930g of extraction residue were obtained. Separate the extraction residue to another 10
Pour into a liter extraction pot and add 60% ethanol aqueous solution 5
After immersion extraction at 50℃ for 6 hours, solid-liquid separation yields 3,940g of body-tasting extract.
I got it. A high-quality vanilla extract with a sharp natural top aroma and an oily body is created by mixing the entire amount of the above carbon dioxide extract and water-containing ethanol extract.
900 g was obtained (product 1 of the present invention).

Example 2 The same extraction tower as in Example 1 was filled with 1 kg of vanilla beans (produced in Madagascar) chopped into approximately 1 cm pieces, and the extraction temperature was 20°C and the pressure was 100 kg/c by the process shown in Figure 1.
m2 subcritical carbon dioxide and 95% as extraction aid
Ethanol was fed at a flow rate of 125 g/hour and extracted for 6 hours. The temperature inside the separator is 30℃, the pressure is 50kg/c
720 g of a pale yellow extract with a fresh top aroma and 1,010 g of an extraction residue were obtained by lowering the extract to m2.

5 kg of a 40% ethanol aqueous solution was added to the residue, and after immersion extraction at 50° C. for 6 hours, solid-liquid separation was performed to obtain 3,950 g of a flavor-based extract with a full body feel. The entire amount of subcritical carbon dioxide extract and hydrous ethanol extract was mixed and clarified and filtered to obtain 4,100 g of high-quality vanilla extract having a sharp natural top aroma and an oily and rich body feeling (product of the present invention). 2).

Example 3 The same extraction tower as in Example 1 was filled with 1 kg of vanilla beans (produced in Indonesia) chopped into approximately 1 cm pieces, and the extraction temperature was 40°C and the pressure was 200 kg/c by the process shown in Figure 1.
Extracted using supercritical carbon dioxide of 50 m2, the temperature inside the separator was set at 30°C and the pressure was 50 kg/cm2 to obtain a pale yellow extract with a fresh top aroma.
g and 940 g of extraction residue were obtained. Then add 5 ml of acetone to the residue.
After immersion extraction at 40° C. for 1 hour, solid-liquid separation was performed to obtain 4 kg of separated liquid. The solvent of the separated liquid was distilled off under reduced pressure to obtain 60 g of a concentrate mainly having a body and taste. The entire amounts of the above carbon dioxide extract and acetone extract were mixed to obtain 110 g of a highly concentrated vanilla extract with a sharp natural top aroma and an oily body feel (Product 3 of the present invention).

Comparative Example 1 In the same manner as in Example 1, 1 kg of vanilla beans (from Madagascar) shredded into approximately 1 cm pieces was charged into an extraction column, and the extraction temperature was 40°C and the pressure was 200°C by the process shown in Figure 1.
Extract using carbon dioxide in a supercritical state at kg/cm2, and set the temperature inside the separator to 30°C and the pressure to 50kg/cm.
2 to obtain 60 g of a pale yellow extract with a fresh top aroma (Comparative Product 1).

Comparative Example 2 Add 50 kg of a 60% ethanol aqueous solution to 1 kg of vanilla beans (from Madagascar) chopped into approximately 1 cm pieces,
Extraction was carried out by immersion at 0°C for 6 hours. After extraction, solid-liquid separation yields 3,940g of extract with vanilla aroma and body.
(Comparative product 2).

Comparative Example 3 In the same manner as in Example 2, 1 kg of vanilla beans (produced in Madagascar), which were shredded into pieces of about 1 cm, was packed into an extraction tower, and extracted at a temperature of 20°C and a pressure of 100 kg by the process shown in Figure 1.
/cm2 of subcritical carbon dioxide and 9 as an extraction aid.
5% ethanol was fed at a flow rate of 125 g/hour and extracted for 6 hours. The temperature inside the separator is 30℃ and the pressure is 50kg.
/cm2, 720 g of a pale yellow extract with a fresh top aroma was obtained (comparative product 3).

Comparative Example 4 5 kg of acetone was added to 1 kg of vanilla beans (produced in Indonesia) cut into pieces of about 10 cm, and the mixture was immersed and extracted at 40° C. for 1 hour, followed by solid-liquid separation to obtain 4 kg of a separated liquid.

The solvent of the separated liquid was distilled off under reduced pressure conditions to obtain 100 g of a concentrate mainly having a body-like taste (comparative product 4).

Reference Example 1 Ice cream dough with 10% milk fat was prepared by a conventional method, and ice cream was prepared by adding 0.5% of each of the vanilla extracts obtained in Example 1 and Comparative Example 1. A panel of 20 well-trained people conducted a sensory evaluation of this ice cream using a two-point comparison method. The results are shown in Table-1.

Reference Example 3 An ice cream was prepared by adding 0.5% of each of the vanilla extracts obtained in Example 1 and Comparative Example 2 to the same ice cream dough as in Reference Example 1.

This ice cream was subjected to sensory evaluation in the same manner as in Reference Example 1. The results are shown in Table-2.

Reference Example 3 An ice cream was prepared by adding 0.5% of each of the vanilla extracts obtained in Example 2 and Comparative Example 3 to the same ice cream dough as in Reference Example 1. This ice cream was subjected to sensory evaluation in the same manner as in Reference Example 1. The results are shown in Table-3.

(The following is a blank space) Reference Example 4 An ice cream was prepared by adding 0.1% of each of the vanilla extracts obtained in Example 3 and Comparative Example 4 to the same ice cream dough as in Reference Example 1. This ice cream was subjected to sensory evaluation in the same manner as in Reference Example 1. The results are shown in Table 4.

As is clear from the results in Tables 1 to 4, the products of the present invention have extremely high palatability, combining a fresh top feeling, an oily, rich body feeling, and a mature feeling, compared to the corresponding comparative products. It was something.

[Effects of the Invention] According to the present invention, vanilla beans are treated with carbon dioxide in a supercritical state or a state close to it in the presence or absence of water and/or alcohol to reduce the aroma in the material. By combining the process of extracting and collecting the components mainly responsible for flavor and the process of extracting and collecting the components mainly responsible for flavor from the vanilla bean residue after processing using a water-miscible organic solvent, By taking advantage of the respective characteristics of the carbon dioxide extraction method and the organic solvent extraction method, it is possible to obtain a high-quality, well-balanced vanilla extract with a sharp natural top aroma, ripeness, and body.

[Brief explanation of the drawing]

FIG. 1 is a flow sheet showing one embodiment of the extraction method of the present invention.

Claims (2)

[Claims] [Claim 1] Vanilla. A first step of treating the beans with carbon dioxide in a supercritical state or a state close to it and extracting and collecting the aromatic components in the material with carbon dioxide gas, and extracting a water-miscible organic solvent from the residue after the above treatment. A novel method for producing vanilla extract, which consists of a second step of extracting and collecting components that mainly give a flavor. [Claim 2] Vanilla. In the first step of treating beans with carbon dioxide in a supercritical state or a state close to it and extracting and collecting aroma-based components in the material with carbon dioxide gas, water and/or alcohols are used as extraction aids. Claim 1
Method described.