JPS62134042A - Method for fractionating low cholesterol butter fat - Google Patents

Abstract

PURPOSE:In removing cholesterol from butter with a supercritical fluid, to fractionate and to produce the titled butter fat readily and without requiring excess energy, by extracting low cholesterol butter fat with a supercritical fluid. CONSTITUTION:In removing cholesterol from butter with a supercritical fluid (e.g., supercritical carbon dioxide), butter fat with low cholesterol is extracted with the supercritical fluid. For example, use of supercritical carbon dioxide under condition of 40 deg.C temperature and 300-350kg/cm<2> pressure preferably provides high extraction efficiency. In the operation, cholesterol is adsorbed on an adsorbent such as silicic acid, etc., and removed. Consequently, cholesterol is removed and low cholesterol butter fat agreeable to present healthy direction can be separated and produced. Since the supercritical fluid used here is usable approximately at normal temperature, operation is easy and no excess energy is required. Since no high-temperature treatment is carried out, there is no change in physical properties.

Description

DETAILED DESCRIPTION OF THE INVENTION (Industrial Application Field) The present invention relates to a method for removing cholesterol from butter using a supercritical fluid and for fractionating and producing low-cholesterol butterfat.

(Prior art) Butter is a food with excellent nutritional value, but its high cholesterol content does not match current consumption trends, and this is the reason why butter consumption is sluggish compared to margarine. It was one.

On the other hand, demand for low-cholesterol foods has been increasing in recent years, not only as therapeutic foods for arteriosclerosis patients, but also as health foods.

Various methods of removing cholesterol from butter have been studied. However, butter also has the characteristic of having a mellow flavor unique to milk fat, which is different from margarine, and it is desirable to maintain this characteristic. It has been difficult to find a method for producing low-cholesterol butter and a method for fractionating low-cholesterol butter that meets these conditions.

Conventionally, for example, butterfat is dissolved in an organic solvent such as ether or acetone, and then a solution of digitonin in ethanol is added to precipitate and remove cholesterol as digitonide. Alternatively, butterfat is dissolved in a low-boiling hydrocarbon and then removed using an adsorbent column. There were ways to get through it. However, all of these methods require a large amount of organic solvent and have the disadvantage that flavor components evaporate during solvent distillation. Furthermore, digitonin is very expensive and is not economically appropriate.

Furthermore, attempts to apply extraction methods using supercritical fluids developed for coal chemistry and ethanol concentration to the separation of butter components were made by Von WKaufmann et al.
at) by “Milhibirasenshaft J (M
Ilehwissenschaft), Vol. 37, No. 2 (1982).

This method extracts cholesterol into supercritical carbon dioxide, and it is also stated that low-molecular components are extracted in the extract and relatively high-molecular components are extracted in the extraction residue. was.

However, there was no specific method for efficiently separating cholesterol, nor was there any mention of conditions that would prevent the unique flavor of butter from deteriorating.

The present inventors also referred to the method of Kaufman et al. and conducted a follow-up attempt to remove cholesterol from butter using a conventional extraction device using supercritical carbon dioxide. It was discovered that using supercritical carbon dioxide at 40°C and a pressure of 150 kg/ct was used, but even when operated under these conditions, approximately 90% of the cholesterol in the bacteria was removed. Along with this, about 75% of butter fat is also extracted, and the selectivity for cholesterol is not high. Furthermore, the flavor components and taste components are also extracted, and the high molecular weight components are concentrated in the extraction residue, resulting in something like beef tallow, which no longer has any flavor or flavor and has the properties of butter, which is not something that can be put to practical use. There was no.

(Problems to be Solved by the Invention) Conventionally known methods, including the method of Kaufman et al., cannot selectively remove only cholesterol from butter, and the flavor and taste of butter may be extremely poor. There was a problem that it was lost. The inventors
As a result of intensive research to solve these problems, we have discovered a new method for removing cholesterol from butter, separating and producing low-cholesterol butterfat, and have completed the present invention.

(Means for Solving the Problems) The present invention provides a low-cholesterol butterfat that is felt to extract low-cholesterol butterfat into a supercritical fluid when removing cholesterol from butter using a supercritical fluid. This is an invention of a method for separating and manufacturing.

The butter used in the present invention may be regular butter, anhydrous butter, or the like. Anhydrous butter can be obtained by dehydrating regular butter, such as by extracting it with hexane. When anhydrous butter is used, there is no problem that water is absorbed into the supercritical fluid and the solubility decreases by that amount, and the extraction efficiency is excellent, but using butter also has a disadvantage in terms of the final extraction amount. It won't happen.

The supercritical fluid used in the present invention is a fluid that has a high density close to that of a liquid and a diffusive force close to that of a gas, and has properties between those of a gas and a liquid.In general, a gas has a certain temperature (critical temperature ), it will not liquefy, but the state above the critical temperature and critical pressure (supercritical state)
It is known that fluids (supercritical fluids) placed in the atmosphere dissolve various organic substances.

If such a supercritical fluid is used in the process of extracting specific components from animal and plant resources, the process can be performed at a lower temperature than with conventional solvent extraction methods. For this reason, the decomposition of the extract
In addition to being able to prevent degeneration, it is also economical as it does not require an excessive supply of energy. Also, unlike solvent extraction methods, there is no concern that residual solvents such as hexane or toluene may have an adverse effect on health.

For this reason, there have been particular expectations for the application of supercritical fluids to food and pharmaceutical manufacturing processes that are closely related to health.

Carbon dioxide is most desirable as the supercritical fluid used in the present invention, but laughing gas, low molecular weight hydrocarbons, etc. can also be used, and the present invention is also applicable to these.

Carbon dioxide is abundantly available, inexpensive, non-toxic and non-residual (and can be used at room temperature), making it the most beneficial use of carbon dioxide.

In the method of the present invention, unlike the method of Kaufman et al., low-cholesterol butterfat is fractionally extracted in a supercritical fluid.

As extraction conditions, when supercritical carbon dioxide is used as the supercritical fluid, the temperature is 40°C and the pressure is 300 to 350 kg.
It is most preferable to set the condition of /c+J in terms of extraction efficiency. Under these conditions, low-cholesterol butter fat can be extracted in supercritical carbon dioxide, and the cholesterol to be removed can be most efficiently fractionated. Extraction under these conditions maximizes the amount of butterfat (triglyceridoid) extracted. On the other hand, the amount of cholesterol extracted under the conditions of a temperature of 40°C and a pressure of 300 to 350 kg/at/at is the same as that under the aforementioned conditions of a temperature of 40°C and a pressure of 150 kg/cd; Since the relative ratio to butterfat is reduced, this is preferable as the extraction condition for butterfat.

Of course, these conditions indicate a preferred embodiment, and the application of the present invention is not limited thereto.

In addition, when laughing gas is used as a supercritical fluid, the temperature is 40℃ and the pressure is 150 to 200kg/ct, and when propane is used, the temperature is 100℃ and the pressure is 300kg/ct.
If cd or butane is used, the temperature is 180℃ and the pressure is 30℃.
0 kg/c+/ is the preferred extraction condition.

Cholesterol will be adsorbed to the adsorbent and will remain. Since cholesterol exists in approximately 96% free form, it is possible to selectively adsorb cholesterol by utilizing the difference in the adsorption power of butter fat (triglyceride) and cholesterol to an adsorbent. On the other hand, butterfat with high molecular weight and high boiling point is partially adsorbed by the adsorbent, but butterfat with low molecular weight and low boiling point is not adsorbed by the adsorbent and is extracted by supercritical fluid, resulting in low-cholesterol butterfat. It is classified as

As the adsorbent, it is preferable to use silicic acid because it has high selectivity. The silicic acid may be any of orthosilicic acid, metasilicic acid, metatrisilicic acid, metatrisilicic acid, metatetrasilicic acid, etc., and is used after removing impurities.

In addition, activated carbon, florisil, alumina, etc. can also be used as the adsorbent.

In industrialization, by separating the extraction cell and the adsorbent column, it is possible to easily desorb the column and regenerate the adsorbent such as silicic acid, and to achieve a higher degree of separation and recovery.

When anhydrous butter is used and silicic acid is used as an adsorbent, it is efficient that the amount of the silicic acid tray is approximately equal to that of the anhydrous putter.

As the amount of silicic acid increases, not only cholesterol but also butterfat will be adsorbed to it, reducing the yield of butterfat.

By reducing the pressure of supercritical carbon dioxide that has passed through a silicic acid column or the like in a separation cell, it is possible to separate dissolved substances such as low-cholesterol butter and fat. Vitamin A etc. are also separated along with the butter fat.

(Effects of the Invention) By the method of the present invention, it is possible to separate cholesterol and fractionate and produce low-cholesterol butter that meets current health trends.

The supercritical fluid used for this can be used at almost room temperature, so
It is easy to operate and does not require excessive energy. Furthermore, since no high temperature treatment is performed, no change in physical properties occurs. These are particularly noticeable when supercritical carbon dioxide is used as the supercritical fluid.

Furthermore, according to the method of the present invention, high molecular weight among butter fats,
Since some of the high boiling point substances are removed, the extracted butter has a melting point lowered by about 5°C compared to before extraction, and has a low melting point and excellent spreadability. Furthermore, since low molecular weight, low boiling point flavor components are extracted as they are, the flavor is not inferior to that before treatment.

Thus, by the method of the present invention, it is possible to provide a health food with excellent flavor and low cholesterol.

(Example) Examples of the present invention will be shown below. Although the examples show the case where anhydrous butter is used, the present invention is not limited thereto, and the present invention is not limited in any way by the examples.

Example 1 Using the apparatus shown in the flowchart of FIG. 1, cholesterol in anhydrous butter was removed to produce low-cholesterol butter fat.

FIG. 2 is a partially enlarged view of the extraction cell (14) in FIG. 1.

Carbon dioxide passes through the cooler (4) as a liquid from the liquid carbon dioxide cylinder (1) and is compressed by the compressor (6) to a predetermined pressure, which is then accurately controlled by the back pressure control valve (8). Be kept. Next, it is brought to a predetermined critical temperature by a fluid temperature control coil (10) in a constant temperature bath (dashed line in Figure 1), and reaches the extraction cell (14) as supercritical carbon dioxide.

The internal volume of the extraction cell (14) was 250 mJ, and 20 g of anhydrous butter (19) was placed in the lower part of the cell, and a column (18) containing 20 pieces of silicic acid (Wakogel CC-100) was placed.
was installed, and a gap was provided between the two to prevent splashes of anhydrous butter from reaching them.

1,600 normal liters of supercritical carbon dioxide was brought into contact with the anhydrous butter from the bottom of the extraction cell at a flow rate of 10 normal liters/min at a temperature of 40° C. and a pressure of 300 to 350 kg/cd. After dissolving anhydrous butter in supercritical carbon dioxide, cholesterol and a portion of high molecular weight butter fat are adsorbed in a silicic acid column (18), and the extract is separated from the carbon dioxide returned to normal pressure to produce low-cholesterol anhydrous butter. I got fat.

The recovery rate and cholesterol removal rate of anhydrous butter were as follows. (The constant of cholesterol is 5-α-
(by gas chromatography constant volume method using Cholestan as internal standard).

Example 2 The same treatment as in Example 1 was carried out, and the amount of silicic acid used was reduced to 60
g (3 times the weight of anhydrous butter).

In this case, the recovery rate and cholesterol removal rate of anhydrous butter were as follows.

Increasing the amount of silicic acid to three times the weight of anhydrous butter removes 97.4% of the cholesterol. However, on the other hand, the yield of anhydrous butter also decreases to 50%.

Example 3 The same treatment as in Example 1 was carried out, and activated carbon 10 was used as an adsorbent.
g and 10 g of Celite 545 were used.

In this case, the recovery rate and cholesterol removal rate of anhydrous butter were as follows.

[Brief explanation of drawings]

The drawings show one embodiment of the apparatus used in the method of the present invention, and the scope of the present invention is not limited by these drawings. FIG. 1 is a flowchart of one embodiment, and FIG. 2 shows an extraction cell. In each drawing, 1 is a liquid carbon dioxide cylinder, 2 is a pressure gauge, 3 is a chuck valve, 4 is a cooler, 5 is a gas filter, 6 is a compressor, 7 is a regulating gas pressure gauge, 8 is a back pressure regulating valve, 9 is a shutoff valve, 10 is a fluid temperature control coil, 11 is a pressure sensor, 12
is a thermometer, 13 is a safety plate, 14 is an extraction cell, 15 is a gas meter valve, 16 is a separation cell, 17 is a flow meter, 18
1 is a silicate column, 19 is anhydrous butter, 20 is a sintered plate, and the area inside the broken line is a constant temperature bath. Patent Applicant Foundation Food Research Group Go to Figure 2 11 Go to 16 Supercritical carbon dioxide procedure amendment (method/directive) Commissioner of the Patent Office Michibe Uga 1 Indication of the case 1985 Patent Application No. 272453'2 Invention Name: Method for separating low-cholesterol butterfat 3 Relationship with the case of the person making the amendment Patent applicant: 1-21-3 Sakae-cho, Higashimurayama-shi, Tokyo Foundation Food Research Association 4: Agent: 2-17-54 Akasaka, Minato-ku, Tokyo No. 919, Building 1, Valle Royale submit. 8 List of attached documents

Claims (7)

[Claims] (1) A method for fractionating low-cholesterol butterfat, which comprises extracting low-cholesterol butterfat into a supercritical fluid when removing cholesterol from butter using a supercritical fluid. (2) The method for fractionating low-cholesterol butterfat according to claim 1, wherein the butter is anhydrous butter. (3) The method for fractionating low-cholesterol butter and fat according to claim 1 or 2, wherein the supercritical fluid is supercritical carbon dioxide. (4) Supercritical carbon dioxide at a temperature of 40℃ and a pressure of 300~3
50 kg/cm^2 The method for fractionating low cholesterol butterfat according to claim 3. (5) A method for fractionating low-cholesterol butter and fat according to claims 1 to 4, in which the cholesterol to be removed is adsorbed on an adsorbent. (6) Claim 5 in which the adsorbent is a silicic acid column
2. Method for fractionating low-cholesterol butterfat. (7) The method for fractionating low-cholesterol butterfat according to claim 6, wherein the weight of silicic acid is approximately equal to that of anhydrous butter.