JPH0312862B2 - - Google Patents

Description

[Detailed description of the invention]

The present invention relates to a method for producing pickled plum juice extract that does not contain organic acids and salt. Pickled plum juice is the pickled juice that is left after the pickled plums are taken out after production. The characteristics of pickled plum juice are that it has a high salt content and is strongly acidic; therefore, 1) it cannot be used as a food product; 2) Not renounceable. 3) Cannot be discharged because biological treatment cannot be performed. 4) A large amount is excreted. It has many problems and is hardly used. Currently, there is a strong trend toward natural products, and proposals related to umeboshi are also being made.
35064) New method for producing umeboshi extract, 2) Tokkosho
57-24103 (Japanese Unexamined Patent Publication No. 50-88268) Seen in the method for producing natural plum sour agent. First of all, 1) is to remove water by distillation to create a concentrated liquid, add alcohol,
This is a method for producing a pickled plum extract, which is characterized by concentrating the hydroalcoholic solution after dissolving and separating insoluble matter. Next, 2) is a method for producing an aromatic tempura sour agent, which is characterized by using an ion exchange membrane to remove the salt content while concentrating and retaining the aroma and extract. The inventor explains that pickled plum juice is made from ``high salt concentration, high acidity,
It is an extract obtained from plum fruit over a long period of time at room temperature, and contains a large amount of powerful active ingredients. 1. The main component of pickled plums is crude fiber, and most of the active ingredients are residues dissolved into pickled plum juice. ”
From this perspective, I thought that pickled plum juice could be made into an excellent food by considering the processing method. What the two conventional methods described above have in common is that a large amount of heat or electrical energy is consumed in order to extract unnecessary components such as common salt. The present invention first adsorbs and deposits only the active ingredients from pickled plum juice onto an adsorption resin, and then separates unnecessary components such as salt and water from the system without adsorbing them and without adding any means. hand,
The concept is different from the conventional method described above. That is, in the present invention, pickled plum juice is treated with an adsorption resin to remove organic acids and salt as non-adsorbed components, and then water, an aqueous alcohol solution, or a weak alkali aqueous solution is added to the adsorption resin, and red pigment is extracted from the adsorption resin. characterized by eluting adsorbed components containing
The present invention provides a method for producing pickled plum juice extract that does not contain organic acids and salt. The first characteristic of pickled plum juice is that it contains a high concentration of salt, ranging from 16 to 25%. Second, the pH is 1~
2, exhibits strong acidity, and contains a large amount of organic acid. The main ingredients are citric acid and malic acid, with 4.5% citric acid and 0.8% malic acid. Other organic acids include acetic acid and lactic acid, but they are extremely rare. Third, it contains small amounts of proteins, lipids, carbohydrates, amino acids, inorganic salts, and pigments. Fourth, it has a more aromatic aroma than umeboshi and is stable over a long period of time. The reason why it was not used despite its many excellent features is thought to be due to the high concentration of common salt. As the adsorption resin, various kinds of synthetic adsorbents having a giant network structure, such as Amberlite XAD (manufactured by Rohm and Haas) and Diamond Resin HP (manufactured by Mitsubishi Kasei), can be used. These include copolymers of styne and divinylbenzene or acrylic acid ester copolymers, which are porous and have a large surface area. They are commercially available with different pore sizes, surface areas and densities. When pickled plum juice is brought into contact with swollen adsorption resins, components with small molecular weights such as salt and citric acid will not be adsorbed. The method of bringing the pickled plum juice into contact with the adsorption resin may be either a batch method or a column method, but since the salt concentration of the pickled plum juice is high, the adsorption resin with a low density may float to the surface of the liquid. In the case of a column type, you can make a column filled with adsorption resin swollen in water and send the pickled plum juice to the top of the column. The effluent is a colorless liquid containing salt, citric acid, etc., but the column is colored by adsorption of various components. If using the batch method, put the adsorption resin into a tank containing pickled plum juice and stir to make it adsorb. The liquid after adsorption is colorless. After adsorption, in the case of a column type, wash with a small amount of water to flush out non-adsorbed components. In the batch method, the mixture is poured and separated from the resin by filtration, and then washed with a small amount of water to remove non-adsorbed components. Water, an alcohol aqueous solution, or a weak alkaline aqueous solution is used to elute the adsorbed component from the resin after adsorption. The properties of the elution solvent should be selected depending on the type of adsorption resin, and some can be eluted with water and others cannot. It goes without saying that it is better to select an eluate that requires as little volume as possible. Alcohol, ethyl alcohol, shochu, alcoholic beverages, etc. are good, and other alcohols such as methanol, propanol, butanol, etc. can also be used for elution, but they are not preferred for use as foods. In addition, a weak alkaline aqueous solution is also possible. However, since it is intended to be used as food, sodium hydroxide is most desirable. The eluate may be used as it is, but if concentration is required, water or alcohol may be removed by vacuum distillation, normal pressure distillation, etc. Since an adsorption resin is used, the eluate does not contain acid, so there is no need for an acid-resistant distillation device. If a pretreatment is used to remove organic acids from pickled plum juice with insoluble calcium salts from pickled plum juice, and the pretreated pickled plum juice is treated with an adsorption resin, the titratable acidity should be measured in advance. The required amount of calcium should be added. The organic acid is mostly citric acid, which begins to crystallize if left for about 2 hours or more. Once the pH reaches about 4 and the formation of crystals is complete, they can be removed and the remaining liquid can be transferred to adsorption treatment. Since the calcium salt of citric acid dissolves in acidity, depending on the use, it is possible to add the calcium citrate to the pickled plum juice extract of the present invention, then make it acidic, dissolve it, and use it. The effects of the method of the present invention will be explained in detail using experimental examples as follows. The pickled plum juice used in the experiment had the properties shown in Table 1.

[Table] Analysis of the organic acid composition of pickled plum juice using high performance liquid chromatography reveals 4.40% citric acid and 0.8% malic acid.
%, and the amount of other organic acids was very small. When citric acid is precipitated as a calcium salt, its solubility is 0.0849 at 18℃ at neutral temperature and 0.0849 at 25℃.
It is 0.0959. Malic acid is 18℃0.9214, 25℃
Since it is 0.8552, theoretically most of the citric acid will precipitate, and less than about 1 g of malic acid will precipitate. When a theoretical amount of CaO was added and a precipitate was precipitated, the value was 4.0. The liquid obtained by filtering out the calcium salt precipitate was also treated with an adsorption resin in the same manner as the pickled plum juice.
The concentrations of citric acid and malic acid in the solution obtained by filtering the precipitate after treatment with CaO were 0.8% and 0.6%, respectively. Commercial adsorption resin products include Rohm and Haas Co.
There are XAD-2, XAD-4, and XAD-7, as well as Mitsubishi Plastics' HP-10, HP-20, and HP50.
Comparing the strength of adsorption for these, the second
It was right on the street. Since there are so many different types of adsorbed components that it is almost impossible to analyze all of them, we decided to use the red pigment component, which is a characteristic of pickled plum juice, to represent the adsorption power. Even if the air in the pores of the adsorption resin is replaced with methanol and water in that order, it will float in 16% saline solution.
Some substances settle even without such treatment.
It is convenient to use the floating adsorption resin in batches, and after adsorption, the two can be easily separated by draining the processing liquid from the bottom of the tank. On the other hand, in the case of an adsorption resin that settles, it is convenient to create a column. Incidentally, even if the adsorption resin floats, it is possible to use an upward type column, that is, a column in which the pickled plum liquid is passed from the bottom of the column.

[Table] An adsorption column was created by swelling 55 ml of XAD-7 with water and forming it into a column with a diameter of 1.8 cm and a height of 31.5 cm. 1000 ml of pickled plum juice was passed through this under the condition of SV = 3.4. All red dye was adsorbed. Elution was carried out with 135 ml of 35% alcohol aqueous solution to obtain an orange to red pigment fraction. When comparing the elution power with 60% alcohol, the elution power with 35% alcohol was greater. The fraction that did not adsorb to the column and flowed out, i.e.
The non-adsorbed component of XAD-7 was 249.4 g, the solid content of 1000 ml of pickled plum juice was 316 g, and the solid content of the eluate was 60 g. Swell HP-2015ml with water and add 40ml of pickled plum juice.
was added for adsorption treatment, and filtered to obtain a colorless and transparent liquid containing non-adsorbed components and a washing liquid. The filtered and separated adsorption resin was taken and eluted with 35% alcohol to obtain a red alcoholic solution of adsorbed components. The solid content of the eluate was 0.2 g. The relationship between the alcohol concentration of the eluate and elution is that when the alcohol concentration is low, the adsorption band becomes large, but when the alcohol concentration is increased, the adsorption band becomes small. However, pure alcohol hardly flows out. Therefore, an appropriately concentrated eluate with the narrowest band width between 35% and 60% was obtained. Next, the method of the present invention will be explained with reference to examples. Example 1 Column φ1.8 made of pickled plum juice 1 using XAD-7
A red adsorption band with a length of 7 cm was created by passing the sample through a 35 cm x 35 cm tube. Next, the solution was washed with 100 ml of ion-exchanged water, and after the salt and citric acid had flowed out, the solution was eluted through ion-exchanged water. The eluate was concentrated to obtain 350 ml of reddish plum extract, which had a plum aroma, was salt-free, and did not contain citric acid. Example 2 Column φ1.8 made of pickled plum juice 1 with XAD-7
A 7 cm long adsorption band was created by passing the sample through a 40 cm x 40 cm tube. Then, after washing with 100ml of water, 35% alcohol 130
eluted in ml. The eluate was collected and concentrated to 20 ml to obtain an extract with the aroma of umeboshi. As in Example 1, it did not contain salt or organic acid. Example 3 1000 ml of pickled plum juice was passed through an XAD-7 column to create an adsorption zone in the same column as in Example 1. After adding 100ml of water and washing, 0.01N
Elution was carried out by adding 100 ml of NaOH. The properties of the eluate were the same as in Example 1. Example 4 20 g of CaO was added little by little to 1000 ml of pickled plum juice while stirring, and the solution was allowed to stand for 5 hours to precipitate crystals mainly consisting of calcium citrate. The filtrate was collected by filtration, and passed through the same column as in Example 1 for adsorption. The eluate was collected after the sodium chloride was drained through ion-exchanged water. Elution was stopped when the red dye had finished elution, and an eluate was obtained. Add the calcium citrate obtained earlier to the eluate and dissolve it to create an adsorption resin treatment solution for pickled plum juice that does not contain salt and has a sour taste.
I got 800ml. Example 5 1000 ml of pickled plum juice was added to 300 ml of HP-20 adsorption resin swollen with 400 ml of water in a 2000 ml water tank, stirred and adsorbed. After the lower pickled plum juice layer became colorless and transparent, the adsorption resin was added. was collected by filtration. After washing with 300 ml of water, 35% alcohol was added to obtain 1000 ml of a deep red eluate. As is clear from the above description, according to the present invention, a pickled plum juice extract that does not contain organic acids and salt can be easily obtained using an adsorption resin. Furthermore, the present invention has many advantages, such as the elution of the pickled plum juice extract from the adsorption resin, which does not require energy consumption to remove unnecessary substances, and also serves as a part of the regeneration operation of the adsorption resin.

Claims (1)

[Claims] 1. After treating the pickled plum juice with an adsorption resin to remove organic acids and salt as non-adsorbed components, water, an aqueous alcohol solution, or a weak alkaline aqueous solution is added to the adsorption resin, and the adsorption containing red pigment is extracted from the adsorption resin. A method for producing pickled plum juice extract free of organic acids and salt, characterized by eluting components.