JPH0633303B2 - How to recover saponin from asparagus waste - Google Patents

Description

Description: TECHNICAL FIELD The present invention relates to a method for extracting a saponin component in asparagus, particularly from a waste portion such as a stem portion of asparagus that has been discarded without being used for food. , A method for effectively recovering saponin by industrial means.

[Prior Art] It has been well known that saponins are contained in plants. In general, saponin is a glycoside that uses a complex alicyclic compound as an aglycone, and is a generic term for a group of plant components whose aqueous solution exhibits bubbling, fish toxicity, hemolysis and the like. Further, animal saponins such as sea cucumber and starfish saponins are also known.

Subsequent studies revealed the properties of saponin itself, and its classification was broadly divided into steroid saponins and triterpenoid saponins.

A solvent extraction method is known as a method for recovering the above-mentioned saponin component from these plants and animals. An extraction method is also known as a method for recovering saponins from white asparagus, which is an edible plant, but this uses asparagus edible parts as a raw material, so a large amount of material must be used, which is a cost problem. was there.

[Problems to be Solved by the Invention] As described above, as a conventional saponin recovery method, there is no method for obtaining a large amount of saponin at a low cost, and therefore the commercially available saponin must be expensive. It was

[Means for Solving Problems] The present inventors have conducted diligent research to solve the above problems, paying attention to the stems and roots of asparagus, which are unnecessary as plants, and are discarded as waste. I researched whether or not the saponin component was also contained in these,
It was found that the saponin component was contained in a sufficient amount, and the industrial recovery method of the present invention could be developed.

That is, the present invention is a method for industrially recovering saponin from a non-edible portion of asparagus by solvent extraction, using asparagus waste as a starting material, immersing the material in alcohol, and then extracting a concentrated extract. A first step of obtaining; a second step of extracting by adding a solvent to the concentrated extract obtained in the first step; a third step of concentrating and distilling the solvent of the extract obtained in the second step to obtain an extracted extract; Fourth step of degreasing for removing lipid components from the extract obtained in the third step; after adding a solvent to the degreasing step liquid obtained in the fourth step to extract the saponin component in the organic layer, Fifth step of concentrating and drying to obtain a crude saponin-containing extract; and, after dissolving the crude saponin-containing extract obtained in the fifth step with an organic solvent, the solution is transferred into ether to obtain a crude saponin-containing extract. Causes a precipitate to form and then And a sixth step of separating and recovering the precipitate; and a method for recovering saponin from asparagus waste.

[Operation] The raw materials used in the present invention are the roots and stems of asparagus, which are conventionally discarded after the edible portion is collected. Therefore, since these wastes are used as raw materials, the saponin component can be recovered at low cost.

As the alcohol used in the first step of the present invention, lower alcohols such as methanol and ethanol can be used. In this example, the water content of the raw material was measured and adjusted so that the total amount was 60% ethanol. A concentrated extract was obtained.

In this case, in the conventional extraction method, heating to several tens of degrees in order to enhance the extraction efficiency and a step of stirring are required, but in the present invention, it is immersed at room temperature and simply in a stationary state. Just enough.

In the second step, an organic solvent is added to the above-mentioned concentrated extract to extract the saponin component and the like in the organic layer. As the organic solvent in this case, for example, n-butanol (BuOH) is used.
It is possible to use a mixture of water and water at a ratio of 1: 1. This is because saponin is generally easily soluble in butanol, while a large amount of sugar contained in the extract is easily dissolved in water. Therefore, first, a mixed solution is used to remove a large amount of sugar as a contaminant. This is because it is preferable.

In the third step, the n-butanol layer is concentrated and then the solvent is distilled off to obtain an extract, which can be performed by using a rotary evaporator and evaporating only the solvent under reduced pressure.

In the fourth step, the extracted extract is defatted. In this case, benzene and chloroform can be added separately to remove lipids and impurities in the extracted extract.

In this case, the organic solvent may be only benzene,
We have found that using chloroform to achieve complete degreasing gives even better results.

In the fifth step, an organic solvent is added to the degreasing step liquid obtained in the fourth step. For example, n-butanol adjusted to 1: 1 with water is used to adjust the saponin component to n-.
It can be carried out by a method in which the butanol layer is extracted, and then the extract is concentrated and dried.

In the sixth step, the crude saponin-containing extract obtained in the fifth step is dissolved in an organic solvent to form a crude saponin precipitate in ether, which is then separated and recovered. It was found that it is preferable to use a device such as the one described above to perform dropwise addition little by little in order to form a crude saponin precipitate.

Hereinafter, one embodiment of the present invention will be described in detail.

[Example] 23.650 g of raw white asparagus root part as a raw material
Measured (as fresh weight), then 60% alcohol
It adjusted so that it might become%, and ethanol was added.

These were ground using a food mixer (National MX-M3) to obtain a mixture.

Then, a mixture consisting of these raw materials and a solvent was put in a poly bucket and allowed to stand at room temperature for one day to extract, and then the extract was collected by suction filtration into a suction filtration bottle.

To the extraction residue, 25% of 60% ethanol was added again, and after repeating the above operation, about 66 of the extract was concentrated by a rotary evaporator and the solvent was distilled off to obtain a brown concentrated extract at 1000
g was obtained (first step).

Then, a mixed solvent of n-ptanol and water (1: 1) was added until the concentrated extract was completely dissolved, and the mixture was shaken well,
Centrifuge for about 30 minutes in a centrifuge for 30 minutes,
The saponin component and the like were extracted and separated into the n-butanol layer (second step).

Then, the n-butanol layer was concentrated by a rotary evaporator and the solvent was distilled off to obtain about 110 g of an extract (third step).

Then, water and benzene were added to the extract in an equivalent amount and suspended to obtain a milky white solution. This solution is centrifuged at 10,000 rpm for 30 minutes using a centrifuge, and the separated benzene layer is tilted by centrifuging the tube to discard the benzene in the upper layer, or by sucking off only the upper layer with a pipette tube and removing the extract. In addition to removing the lipid component of, the remaining water layer part,
The same operation was performed by adding the same amount of new benzene. The degreasing step may be performed only by adding benzene, but it has been confirmed that efficient degreasing can be performed by using another solvent such as chloroform or ether (fourth step).

Then, from the obtained water layer portion, water was concentrated by a rotary evaporator to dryness, and then about 1 of a mixed solvent of n-butanol and water (1: 1) was added to dissolve the extract, and the mixture was placed in a separating funnel. The saponin component was extracted into the butanol layer by standing still overnight.

Then, the butanol layer was concentrated by a rotary evaporator and dried to obtain about 18 g of crude saponin (brown extract) (fifth step).

Next, 300 ml of methanol was added to the brown extract to dissolve it, and 75 ml of each was slowly dropped into a separately prepared ethyl ether (2) using an injection needle to form a white precipitate, which was allowed to stand for a while. Most of the ether was removed by decantation, and the precipitate was collected by suction filtration, and fresh ether was washed several times over the precipitate to wash away the dissolved ether of contaminants.

The almost white precipitate obtained by such an operation was dried in a vacuum desiccator and then ground in a mortar to obtain about 11 g of a crude saponin component. The yield is shown in Table 1. From this table, it is understood that the crude saponin could be finally recovered in a high yield of 0.38%.

Then, 10 ml of the crude saponin powder was dissolved in 1 ml of methanol and added onto a silica gel plate for thin layer chromatography, and chloroform: methanol: water (70:30:
After development with the mixed solution of 5), anisaldehyde-sulfuric acid solution was sprayed and heated at 70 ° C. for several minutes to detect eight yellow spots characteristic of steroid saponin.

Further, when 10% sulfuric acid was sprayed and color was developed for several minutes at 110 ° C. and impurities were examined, several very thin spots were detected and it was found that some impurities were included.

Similarly, the content of the saponin component in each step is shown in Fig. 2. In Fig. 2, chloroform: methanol: water (70: 30: 5), a color former, and an anthaldehyde-sulfuric acid mixed solution were sprayed as a developing solvent. After that, heat to 70 ° C and detect spots specific to the yellow steroid saponin,
It is a thin-layer chromatogram in which 10% sulfuric acid was sprayed and heated at 120 ° C. to detect the presence or absence of impurities. It is understood that impurities are removed by passing through each step.

[Advantages of the Invention] As described above, the present invention is capable of effectively utilizing the waste and also capable of recovering the crude saponin component at low cost by industrial means.

[Brief description of drawings]

1 is a flow sheet of the method of the present invention, and FIG. 2 is
It is an analysis chart which shows the analysis result of the crude saponin by TLC method.

 ─────────────────────────────────────────────────── ─── Continuation of the front page (56) References Chemical & Pharmaceutical Bulletin, Vol. 27, No. 12, pp. 3086-94 (1979) Agricultural & Bio-Biological Chemistry, Vol. 39, No. 10, pp. 1999-2002 (1975)

Claims (1)

[Claims] 1. A first step of using asparagus waste as a starting material, immersing the raw material in an ethyl alcohol solution, and then obtaining a concentrated extract at room temperature; n-butanol added to the concentrated extract obtained in the first step. Second step of adding a solvent consisting of a mixture of water and water for extraction; third step of concentrating the extract obtained in the second step and distilling the solvent to obtain an extract; obtained in the third step Fourth step of degreasing in a mixed solution of benzene and chloroform to remove lipid components from the extracted extract; a solvent composed of a mixed solution of n-butanol and water is added to the degreasing step obtained in the fourth step. After the saponin component is extracted into the organic layer by concentration, the solution is concentrated to dryness to obtain a crude saponin-containing extract in the fifth step; and the crude saponin-containing extract obtained in the fifth step is dissolved in methanol, and then the solution is dissolved. Yut in ether Ri dropwise allowed to produce a precipitate, and then the sixth step of separating and recovering the precipitate of the crude saponin; saponin recovery method from asparagus waste, comprising the.