JPS59137421A - Preparation of physiologically active substance - Google Patents

Abstract

PURPOSE:To obtain a physiologically active substance having anticholesteric and antilipemic activities, etc., such as saponin, flavonoid, etc., easily from the boiled soup, juice and whey produced from the preparation process of soybean foods, by the absorption and desorption of the substance using charcoal, active carbon, etc. CONSTITUTION:A physiologically active substance composed mainly of saponin, flavonoid and its glycoside is separated from the boiled soup, juice, and whey of soybeans, by the adsorption and desorption using charcoal, active coal and active resin. For example, the boiled soup, juice, etc. are transferred from the waste liquid tank 1 to the recovery column 3 packed with active coal to effect the adsorption of the physiologically active substance. Thereafter, ethanol is supplied from the ethanol tank 2 to the recovery column 3 to desorb the active fraction, which is distilled by the ethanol distillation apparatus 4. The residue is taken out of the apparatus 4 through the outlet 13, and dried to obtain the objective active substance. The active substance can be adsorbed easily with active coal, etc., and desorbed easily with ethanol. The active coal, etc. can be reused without causing lowering of adsorptivity.

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention is a method for producing boiled beans, miso, soy sauce, natto, frozen tofu, tofu, and isolated protein from the "broth,""yu," or "whey" produced in the manufacturing process and discarded as waste liquid. Physiologically active substances, mainly saponins, flavonoids, isoflavonoids, and their glycosides, which are involved in anticholesterolemic effects, antilipemic effects, and promotion of fat metabolism, are obtained by adsorption and desorption of charcoal, activated carbon, or activated resin. Concerning methods of manufacturing substances.

Overnutrition disorders (obesity, high blood pressure,
As symptoms of cerebral hemorrhage, heart diseases such as arteriosclerosis, diabetes, cancer, etc. are beginning to appear, the benefits of plant foods are beginning to attract attention. It has recently become clear that the effects of plant foods, especially soybean foods, are based on the antioxidant, antilipemic, anticholesterolemic, and lipid metabolism promoting effects of saponins and inflavones. (Ryo Okubo, Kiyohide Sone, "Food nutritional rejuvenation using saponins centered on soybeans," Food Development Vol. 1.6.

765.1981, Ryo Okubo, Katsumi Takahashi "Chemistry and physiological effects of soybean glycoside components" Food Development Vol. 17°A, 7
, 1982), the present inventors were able to clarify that the present invention was also based on an unidentified glycoside component. Therefore, there has been an urgent need to develop supplementary food materials that have these physiological effects.

The physiologically active substance obtained by the present invention is a mixture of soybean saponins, infravonoids, flavonoids, and their glycosides, and has antioxidant, anticholesterol, antilipidemic, and lipid metabolism promoting effects. This has become clear from detailed research by the present inventors described below.

The ``broth,''``yu,'' and ``whey'' generated in the manufacturing process of boiled beans, miso, soy sauce, natto, firm tofu, frozen tofu, and protein isolate are considered to be worthless, and rather, they are not used in excess because they pose a risk of pollution. The waste is treated in expensive and large-scale lagoons or activated sludge facilities, and then disposed of into rivers.

There is almost no research on "boiled soup", "yu" and "whey", and the present inventors focused on the causative substances of these waste liquids, which may cause pollution, and conducted detailed research, as shown below. The results were obtained. That is, the "broth", "yu" and "whey" were concentrated to dryness, and crude saponin and crude inflavone glycoside fractions were obtained by the operations shown below.

Sample] Reflux extraction with citanol, methanol extract, butanol layer settling The yield of the supernatant crude saponin fraction was very small, about 1/100 of the crude inflavone glycoside fraction. As a result of examining these by thin-layer chromatography, a band corresponding to saponin was clearly detected in the crude saponin category, which has a low yield, and in the crude inflavone category, genistein was overwhelmingly present in "boiled soup,""yu," and I-whey. followed by genistin, glycidin glycoside, guidine, daidiene,
Glycitin was detected, and many unidentified glycoside components were detected. The thin layer chromatography is shown in FIG.

Next, this crude saponin fraction, crude isoflavone fraction, and physiological saline as a control were administered to rats, and after rearing,
Anatomical findings, weight, blood cholesterol, triglyceride, free fatty acids, GOT and GPT were measured. As a result, as shown in Figure 2G)(B)(C),
Compared to the physiological saline administration group, the crude saponin administration group had a slight decrease in blood triglyceride and a somewhat higher measured weight and G.
Although it was OT, no significant effects of administration were observed overall.

In contrast, in the crude isoflavone group, blood cholesterol, triglyceride, and GOT were significantly reduced.

GPT levels were all significantly reduced, and clear anticholesterolemic, antilipidemic, and antihepatic dysfunction effects were observed.

Therefore, as a result of all studies on simple recovery methods for physiologically active fractions corresponding to the crude isoflavones from ``1-broth'', ``yu'' and ``whey'', we found that none of the components corresponding to the crude isoflavones were active carbon, charcoal, charcoal, Easily adsorbs to active resin,
It was found that it was easily desorbed with ethanol. Moreover,
The adsorption amount is 5 to 1 of the weight of activated carbon, charcoal, and activated resin.
It was also found that activated carbon, etc., after desorption can be used repeatedly to reduce adsorption capacity. To explain in detail using an example of recovery from "YU", waste liquid IYJf: As a result of desorption from 1 kg of escaped granular activated carbon with an ethanol water bath solution of various concentrations, as shown in Figure 3, 10%, 60%
, a desorption behavior with a peak seen in the 80% ethanol portion appears. Furthermore, as a result of examining these desorption sections by TLC (Figure 4), a small amount of saponin was detected in 60 to 80%, but in general, infravones were present, and 90% ethanol was not able to completely desorb them. Understood. Therefore, all physiologically active components can be desorbed with 90-100% ethanol.

Based on the above results, we developed a method for producing active preparations from waste liquid.
The process will be explained according to the process diagram shown in FIG. In Figure 5, (1) is a waste liquid tank, (2) is an ethanol tank, (3) is a recovery tank, (4) is an ethanol distillation device,
(5) is the waste liquid treatment facility, and (6) is the waste liquid tank (1
) and the collection tank (3), (7) is the pipe that connects the bottom of the ethanol tank (2) and the pipe (6) with a three-way valve (8), and (9) is the pipe that connects the collection tank (3) and the waste liquid. A pipe connecting the processing facility (5), 00) is a pipe connecting the bottom of the ethanol distillation device (4) and the pipe (9) with a three-way valve 0]), and a2) is a pipe connecting the top of the ethanol distillation device (4) to the ethanol distillation device (4). A pipe connecting the upper part of the tank (2), α3), is a take-out pipe provided at the bottom of the ethanol distillation device (4). First, the recovery tank (3) is filled with activated carbon, charcoal, or activated resin.
A waste liquid such as "broth", "yu" or "whey" is sent from the waste liquid tank (1) to the liquid waste tank (1), and the active ingredients are adsorbed. After adsorption, ethanol is sent from the ethanol tank (2) to the recovery tank (3), the active fraction is desorbed and sent to the ethanol distillation device (4), and the ethanol is transferred to the ethanol tank (2), where the active fraction is desorbed and the ethanol is transferred to the ethanol tank (2). Take it out from the take-out pipe α3),
Dry to obtain active preparation.

Next, examples of the present invention will be described.

Example 1 The collection tank shown in FIG. 5 is filled with 24.5 tons of adsorbent suspended in 8 kg of activated carbon and 20.4 tons of gold water.

Pour 1 ton of waste liquid from the tofu factory into a recovery tank.
After washing with 20% ethanol water, the adsorbed substances were eluted by flowing 60-95% ethanol 751-. This eluate was concentrated under reduced pressure to obtain a concentrate and recovered ethanol. This concentrate was frozen or spray dried to obtain the first target product 4082. After washing with 150 tons of water from the recovery tank, the waste liquid is
A second target product 4022 was obtained using the same procedure.

Repeat the above operation 5 times in total, and the yield is 407 for the 6th time.
7. In the 4th test at 698g and the 5th test at 4051, no decrease in adsorption capacity was observed, and the recovery tank could be used semi-permanently. As a result of analyzing the obtained physiologically active specimen, 6? It consisted of isoflavonoid components of chi and 8% of zabonin components, and the main infravonoid component was genistein. Note that ethanol can also be recovered and reused from the 20% ethanol eluate and the water washing solution.

Even when charcoal is used instead of activated carbon in the above operation, the charcoal is crushed in advance and packed into a recovery tank in the same way as activated carbon, and the first 3722, second 6762, 3rd 6611, 4th 6707, 5th 6
I was able to obtain a standard specimen of 787.

Example 2 Weakly basic anion exchange resin AGIX4.5t was packed in the recovery tank shown in Figure 5, 1 ton of washing liquid "YU" from the tofu factory was poured into the recovery tank, and after washing with 6-4N acetic acid IQt, 5-1
The adsorption substance was eluted with 20 tons of ON acetic acid. This eluate was concentrated under reduced pressure to obtain a concentrate and recovered acetic acid, and the concentrate was further frozen or spray-dried to obtain the first target product 3067. Subsequently, after washing the recovery tank with 40 tons of water, 1 ton of waste liquid "YU" was poured into it again, and all 294 grams of the second target product were recovered in the same manner. Repeat the above operation 5 times for all needles, and the yield is 6th 27th
07, 4th 2562 and 5th 2482, some decrease in adsorption capacity was observed, but by reactivating the resin with hydrochloric acid, it was possible to use it semi-permanently. As a result of analysis of the obtained physiologically active preparation, it was found that it consisted of 81% infravonoid components and 12 zabonin components, and the main component of the infravonoid components was genistein. In addition, acetic acid was also recovered from the 6-4N acetic acid eluate and the water washing solution17.
It can be reused.

Example 6 According to the method of Example 1, soybean broth, acid precipitated protein preparation [soybean whey, soybean water U, liquid]
・We obtained a physiologically active specimen. Table 1 shows the sample quantity, yield, and content of zaponin and infravonoid components.

Table 1 Example 4 According to the method of Example 2, physiologically active samples were obtained from soybean broth, soybean whey used in acid-precipitated protein preparation, and soybean washing liquid. Table 2 shows the amount of sample solution, yield, and content of saponin and isoflavonoid components.

Table 2

[Brief explanation of the drawing]

Figure 1 is thin layer chromatography of crude saponin and crude isoflavones, Figure 2 (a), (b), and (c) are measured weights, blood cholesterol, triglycerides, free fatty acids, and G.
A graph showing the effects of crude saponin and crude inflavone administration on OT and GPT. Figure 3 is a graph showing the desorption results of ethanol from 1 kg of adsorbed activated carbon. Figure 4 shows the desorption activity of ethanol from 1 kg of adsorbed activated carbon. Sectional thin layer chromatography, FIG. 5 is a diagram illustrating the process of the present invention. Agent Takeshi Shimizu, 7:″. -5-2 2-So Hayabusa, 5th (Wasen 4)

Claims (1)

[Claims] The "broth" produced during the production of boiled beans, miso, soy sauce, and natto
, physiologically active substances, mainly saponins, fujiboids, infravonoids, and their glycosides, are absorbed from the "yu" produced during the production of tofu or the "whey" produced during the production of isolated proteins by adsorption and desorption of charcoal, activated carbon, or activated resin. A method for producing a physiologically active substance, characterized in that it is obtained by.