Solid beverage containing (R) -3-hydroxybutyric acid and preparation method thereof

文档序号:1895839 发布日期:2021-11-30 浏览:16次 中文

阅读说明:本技术 一种含(r)-3羟基丁酸的固体饮料及其制备方法 (Solid beverage containing (R) -3-hydroxybutyric acid and preparation method thereof ) 是由 薛凌云 吕金艳 余柳松 陈镇聪 郑序伦 阿丽娅 于 2021-09-13 设计创作,主要内容包括:本发明属于功能食品技术领域,具体涉及一种含(R)-3羟基丁酸的固体饮料及其制备方法。该固体饮料,按重量份计,包括以下组分:5-40份(R)-3-羟基丁酸和40-120份成型剂;成型剂选自变性淀粉、酪蛋白酸钠、麦芽糊精、α-环糊精、β-环糊精或膳食纤维中的至少两种。本发明采用成型剂对(R)-3-羟基丁酸进行半包覆,使制备的固体饮料中(R)-3羟基丁酸的稳定性良好,在长期放置期间不易产生杂质巴豆酸;且能够在水中迅速分散,形成液体饮料。该饮料可应用于改善大脑健康、调节运动机能、促进胃肠道健康等多种健康领域,其不添加任何防腐剂,长期使用无副作用。该固体饮料的制备工艺简便,方便运输。(The invention belongs to the technical field of functional foods, and particularly relates to a solid beverage containing (R) -3-hydroxybutyric acid and a preparation method thereof. The solid beverage comprises the following components in parts by weight: 5-40 parts of (R) -3-hydroxybutyric acid and 40-120 parts of a forming agent; the forming agent is at least two selected from modified starch, sodium caseinate, maltodextrin, alpha-cyclodextrin, beta-cyclodextrin or dietary fiber. The forming agent is adopted to semi-coat the (R) -3-hydroxybutyric acid, so that the stability of the (R) -3-hydroxybutyric acid in the prepared solid beverage is good, and the impurity crotonic acid is not easy to generate during long-term storage; and can be rapidly dispersed in water to form a liquid beverage. The beverage can be applied in various health fields such as brain health improvement, motor function regulation, gastrointestinal health promotion, etc., and has no antiseptic and no side effect after long-term use. The solid beverage has simple preparation process and convenient transportation.)

1. The solid beverage containing (R) -3-hydroxybutyric acid is characterized by comprising the following components in parts by weight: 5-40 parts of (R) -3-hydroxybutyric acid and 40-120 parts of a forming agent; the forming agent is at least two selected from modified starch, sodium caseinate, maltodextrin, alpha-cyclodextrin, beta-cyclodextrin or dietary fiber.

2. The solid beverage according to claim 1, comprising the following components in parts by weight: 10-30 parts of (R) -3-hydroxybutyric acid and 40-80 parts of a forming agent.

3. A solid beverage according to claim 1, wherein the dietary fibre comprises at least one of fructo-oligosaccharides, resistant dextrins, inulin, polydextrose, lacto-oligosaccharides, xylo-oligosaccharides, isomalto-oligosaccharides, soy oligosaccharides, carboxymethyl cellulose.

4. A solid beverage as claimed in any one of claims 1 to 3, further comprising a food additive comprising a food flavour and/or sweetener.

5. A solid beverage according to claim 4, wherein the sweetener is at least one selected from the group consisting of stevioside, sucralose, erythritol, Lo Han Guo extract, neotame, xylitol, and maltitol.

6. The solid beverage according to claim 4, wherein the food flavor comprises at least one of lime flavor, grape flavor, apple flavor, strawberry flavor, pineapple flavor, or white peach flavor.

7. A solid beverage as claimed in claim 4, comprising the following components in parts by weight: 10-30 parts of (R) -3-hydroxybutyric acid, 40-80 parts of forming agent, 1-5 parts of food essence and 1-5 parts of sweetening agent.

8. The method for preparing a solid beverage containing (R) -3-hydroxybutyric acid according to any of claims 1-7, comprising the steps of:

and heating and dissolving the forming agent, cooling, adding the (R) -3-hydroxybutyric acid solution, mixing, and drying to obtain the (R) -3-hydroxybutyric acid-containing solid beverage.

9. The method for preparing the compound of claim 8, wherein the temperature for heating and dissolving is 40-80 ℃; the temperature reduction process is to reduce the temperature to 10-40 ℃.

10. The production method according to claim 8, wherein the (R) -3-hydroxybutyric acid is present in the form of an aqueous solution of (R) -3-hydroxybutyric acid, wherein the mass concentration of (R) -3-hydroxybutyric acid in the aqueous solution of (R) -3-hydroxybutyric acid is 20% to 70%.

Technical Field

The invention belongs to the technical field of functional foods, and particularly relates to a solid beverage containing (R) -3-hydroxybutyric acid and a preparation method thereof.

Background

(R) -3-hydroxybutyric acid is one of three ketone bodies ((R) -3-hydroxybutyric acid, acetoacetate, acetone) produced by energy supply from fat metabolism in human body, and accounts for about 70% of the three substances. In mammals, (R) -3-hydroxybutyrate is produced by fat metabolism in the liver, and blood is transported to other tissues and organs and oxidized in the mitochondria of cells to generate energy. In recent years, more and more scientific researches show that (R) -3-hydroxybutyric acid not only can be used as an energy source, but also has various health benefits for human bodies, and research reports in the aspect of medicines are continuously reported.

At present, functional food of (R) -3-hydroxybutyric acid does not appear on the market. The (R) -3-hydroxybutyric acid-like products are mainly (R) -3-hydroxybutyrate and ester, and are mainly applied to the fields of ketogenic diet weight loss, high-intensity professional sports, cognition improvement and the like. However, (R) -3-hydroxybutyrate is basically a chemically prepared racemic mixture, and studies show that (S) -3-hydroxybutyrate in the racemic mixture has no physiological activity; the (R) -3-hydroxybutyrate is mainly a product which is sold on the market abroad, the taste is bitter and astringent, the product is difficult to be accepted by consumers, and the product needs to be metabolized by the liver in the human body in the metabolic process, so the product is not easy to be drunk for a long time.

The melting point of the (R) -3-hydroxybutyric acid is lower, and the boiling point is 49-50 ℃; pure crystals may liquefy at room temperature. The pH value of the liquid (R) -3-hydroxybutyric acid is low, and the requirements on equipment for storage, transportation and preparation of terminal products are high; when the (R) -3-hydroxybutyric acid is prepared into a beverage, the 3-hydroxybutyric acid is easily polymerized in an aqueous solution to form oligomers, and researches show that the mass concentration of the aqueous solution of the (R) -3-hydroxybutyric acid is 30%, wherein the oligomer content is about 3-5%; (R) -3-hydroxybutyric acid in 50% aqueous solution, wherein the oligomer content is about 7-9%; (R) -3-hydroxybutyric acid in an aqueous solution at a mass concentration of 80% and having an oligomer content of about 10-15%. Meanwhile, (R) -3-hydroxybutyric acid is liable to generate crotonic acid during the standing.

Therefore, it is highly desirable to provide a beverage containing (R) -3-hydroxybutyric acid, which is convenient to transport and has good stability.

Disclosure of Invention

The present invention is directed to solving at least one of the problems of the prior art described above. Therefore, the invention provides a solid beverage containing (R) -3-hydroxybutyric acid.

In a first aspect of the present invention, there is provided a solid beverage containing (R) -3-hydroxybutyric acid.

Specifically, the solid beverage containing (R) -3-hydroxybutyric acid comprises the following components in parts by weight: 5-40 parts of (R) -3-hydroxybutyric acid and 40-120 parts of a forming agent; the forming agent is at least two selected from modified starch, sodium caseinate, maltodextrin, alpha-cyclodextrin, beta-cyclodextrin or dietary fiber.

Preferably, the solid beverage comprises the following components in parts by weight: 5-30 parts of (R) -3-hydroxybutyric acid and 40-80 parts of a forming agent. Further preferably, the solid beverage comprises the following components in parts by weight: 10-25 parts of (R) -3-hydroxybutyric acid and 40-60 parts of a forming agent.

Preferably, the dietary fiber comprises at least one of fructo-oligosaccharide, resistant dextrin, inulin, polydextrose, lacto-oligosaccharide, xylo-oligosaccharide, isomalto-oligosaccharide, soybean oligosaccharide and carboxymethyl cellulose.

Preferably, the solid beverage further comprises food additives.

Preferably, the food additive comprises a food flavor and/or a sweetener.

Preferably, the sweetener is at least one selected from stevioside, sucralose, erythritol, luo han guo extract, neotame, xylitol, maltitol, and the like.

Preferably, the food essence comprises at least one of lime essence, grape essence, apple essence, strawberry essence, pineapple essence or white peach essence. The food flavor may be used in solid form or liquid form.

Preferably, the solid beverage further comprises white granulated sugar and/or glucose.

Preferably, the solid beverage comprises the following components in parts by weight: 10-30 parts of (R) -3-hydroxybutyric acid, 40-80 parts of forming agent, 1-5 parts of food essence and 1-5 parts of sweetening agent.

Further preferably, the solid beverage comprises the following components in parts by weight: 10-25 parts of (R) -3-hydroxybutyric acid, 40-60 parts of forming agent, 1-4 parts of food essence and 1-4 parts of sweetening agent.

In a second aspect, the present invention provides a method for preparing a solid beverage containing (R) -3-hydroxybutyric acid.

Specifically, the preparation method comprises the following steps:

and heating and dissolving the forming agent, cooling, adding (R) -3-hydroxybutyric acid, mixing, and drying to obtain the solid beverage containing (R) -3-hydroxybutyric acid.

Preferably, the temperature for heating and dissolving is 40-80 ℃; further preferably, the temperature for dissolving by heating is 40-70 ℃.

Preferably, the temperature is reduced to 10-40 ℃; further preferably, the temperature is reduced to 20-40 ℃.

Preferably, the method of drying comprises spray drying or freeze drying.

Preferably, when the solid beverage further contains a food additive, the process of adding the food additive for dissolution is further included after the forming agent is heated for dissolution.

Preferably, the (R) -3-hydroxybutyric acid is present in the form of an aqueous solution of (R) -3-hydroxybutyric acid.

Preferably, the mass concentration of the (R) -3-hydroxybutyric acid in the (R) -3-hydroxybutyric acid aqueous solution is 20-70%; further preferably, the mass concentration of the (R) -3-hydroxybutyric acid in the (R) -3-hydroxybutyric acid aqueous solution is 30-60%.

The invention takes (R) -3-hydroxybutyric acid aqueous solution with the mass concentration of 20-70% as a raw material, and semi-embeds liquid (R) -3-hydroxybutyric acid by selecting a proper forming agent, so that the liquid performance of the liquid (R) -3-hydroxybutyric acid is reduced by utilizing the solid performance of the forming agent, and the stability of the (R) -3-hydroxybutyric acid is improved.

Compared with the prior art, the invention has the following beneficial effects:

(1) the invention adopts the forming agent to carry out half-coating on the (R) -3-hydroxybutyric acid, the forming agent disperses the liquid (R) -3-hydroxybutyric acid in a solid form, and finally the half-coating is realized through drying to form the solid beverage. The invention controls the selection and the variety of the forming agent, so that the stability of the (R) -3-hydroxybutyric acid in the prepared solid beverage is good, the content is stable during long-term storage, and the impurity crotonic acid is not easy to generate; and the solid beverage can be rapidly dispersed in water to form a beverage.

(2) The invention provides a solid functional product containing (R) -3-hydroxybutyric acid, wherein the contained (R) -3-hydroxybutyric acid can be directly absorbed by a human body, rapidly enters blood and cells, provides energy for the cells, relieves fatigue, improves cognition and regulates metabolism, and can be applied to various health fields such as brain health improvement, motor function regulation, gastrointestinal tract health promotion and the like. The solid beverage is free of any preservative, and has long shelf life and no side effect after long-term use.

(3) The solid beverage containing (R) -3-hydroxybutyric acid provided by the invention is simple and convenient in preparation process and easy for industrial production; the solid beverage is convenient for transportation and carrying, and has good palatability.

Detailed Description

In order to make the technical solutions of the present invention more apparent to those skilled in the art, the following examples are given for illustration. It should be noted that the following examples are not intended to limit the scope of the claimed invention.

The starting materials, reagents or apparatuses used in the following examples are conventionally commercially available or can be obtained by conventionally known methods, unless otherwise specified.

Example 1

A solid beverage containing (R) -3-hydroxybutyric acid comprises the following components in parts by weight: 10 parts of (R) -3-hydroxybutyric acid, 30 parts of resistant dextrin, 30 parts of modified starch, 1.6 parts of lime essence and 1.6 parts of stevioside.

A method for preparing a solid beverage containing (R) -3-hydroxybutyric acid, comprising the steps of:

(1) adding 200 parts of water into a container, heating to 70 ℃ in a water bath, adding 30 parts of resistant dextrin and 30 parts of modified starch, stirring and dissolving until the liquid is uniform, and preserving heat for 30 minutes until the liquid is fully and uniformly mixed;

(2) adding 1.6 parts of lime essence and 1.6 parts of stevioside RA 97% into the solution obtained in the step (1), uniformly stirring, and cooling to room temperature;

(3) adding 20 parts of (R) -3-hydroxybutyric acid aqueous solution (the mass concentration of (R) -3-hydroxybutyric acid is 50%) into the solution in the step (2), and uniformly stirring to obtain a viscous body;

(4) and (4) putting the viscous body in the step (3) into a food-grade clean tray, and freeze-drying to obtain a solid containing the (R) -3-hydroxybutyric acid.

(5) And (4) crushing and screening the solid in the step (4), uniformly mixing the part of the solid with a 40-mesh sieve, and packaging to obtain the solid beverage containing the (R) -3-hydroxybutyric acid.

Example 2

A solid beverage containing (R) -3-hydroxybutyric acid comprises the following components in parts by weight: 17.5 parts of (R) -3-hydroxybutyric acid, 60 parts of sodium caseinate, 40 parts of isomaltose hypgather, 2.5 parts of pineapple essence, 1.5 parts of fructus momordicae extract and 0.2 part of sucralose.

A method for preparing a solid beverage containing (R) -3-hydroxybutyric acid, comprising the steps of:

(1) adding 200 parts of water into a container, heating to 60 ℃ in a water bath, adding 60 parts of sodium caseinate and 40 parts of isomaltooligosaccharide, stirring to dissolve until the liquid is uniform, and preserving heat for 30 minutes until the liquid is fully and uniformly mixed;

(2) adding 2.5 parts of pineapple essence, 1.5 parts of fructus momordicae extract and 0.2 part of sucralose into the solution obtained in the step (1), uniformly stirring, and cooling to room temperature;

(3) adding 35 parts of (R) -3-hydroxybutyric acid aqueous solution (the mass concentration of (R) -3-hydroxybutyric acid is 50%) into the solution in the step (2), and uniformly stirring to obtain a mixed solution;

(4) spray drying the mixed solution in the step (3) to obtain solid powder containing (R) -3-hydroxybutyric acid;

(5) and (4) screening the solid powder in the step (4), uniformly mixing parts of the powder with a 40-mesh sieve, and packaging to obtain the solid beverage containing the (R) -3-hydroxybutyric acid.

Example 3

A solid beverage containing (R) -3-hydroxybutyric acid comprises the following components in parts by weight: 15 parts of (R) -3-hydroxybutyric acid, 30 parts of sodium caseinate, 20 parts of isomaltooligosaccharide, 2.5 parts of pineapple essence, 1.5 parts of fructus momordicae extract and 0.2 part of sucralose.

A method for preparing a solid beverage containing (R) -3-hydroxybutyric acid, comprising the steps of:

(1) adding 200 parts of water into a container, heating to 60 ℃ in a water bath, adding 30 parts of sodium caseinate and 20 parts of isomaltooligosaccharide, stirring to dissolve until the liquid is uniform, and preserving heat for 30 minutes until the liquid is fully and uniformly mixed;

(2) adding 2.5 parts of pineapple essence, 1.5 parts of fructus momordicae extract and 0.2 part of sucralose into the solution obtained in the step (1), uniformly stirring, and cooling to room temperature;

(3) adding 30 parts of (R) -3-hydroxybutyric acid aqueous solution (the mass concentration of (R) -3-hydroxybutyric acid is 50%) into the solution in the step (2), and uniformly stirring to obtain a mixed solution;

(4) spray drying the mixed solution in the step (3) to obtain solid powder containing (R) -3-hydroxybutyric acid;

(5) and (4) screening the solid powder in the step (4), uniformly mixing parts of the powder with a 40-mesh sieve, and packaging to obtain the solid beverage containing the (R) -3-hydroxybutyric acid.

Example 4

A solid beverage containing (R) -3-hydroxybutyric acid comprises the following components in parts by weight: 20 parts of (R) -3-hydroxybutyric acid, 25 parts of xylo-oligosaccharide, 25 parts of beta-cyclodextrin, 10 parts of sodium caseinate, 2 parts of lime essence and 2 parts of stevioside.

A method for preparing a solid beverage containing (R) -3-hydroxybutyric acid, comprising the steps of:

(1) adding 200 parts of water into a container, heating to 70 ℃ in a water bath, adding 25 parts of xylo-oligosaccharide, 25 parts of beta-cyclodextrin and 10 parts of sodium caseinate, stirring and dissolving until the liquid is uniform, and preserving heat for 30 minutes until the liquid is fully and uniformly mixed;

(2) adding 2 parts of lime essence and 2 parts of stevioside into the solution obtained in the step (1), uniformly stirring, and cooling to room temperature;

(3) adding 40 parts of (R) -3-hydroxybutyric acid aqueous solution (the mass concentration of (R) -3-hydroxybutyric acid is 50%) into the solution in the step (2), and uniformly stirring to obtain a viscous body;

(4) and (4) putting the viscous body in the step (3) into a food-grade clean tray, and freeze-drying to obtain a solid containing the (R) -3-hydroxybutyric acid.

(5) And (4) crushing and screening the solid in the step (4), uniformly mixing the part of the solid with a 40-mesh sieve, and packaging to obtain the solid beverage containing the (R) -3-hydroxybutyric acid.

Example 5

A solid beverage containing (R) -3-hydroxybutyric acid comprises the following components in parts by weight: 10 parts of (R) -3-hydroxybutyric acid, 30 parts of resistant dextrin, 30 parts of modified starch, 1.6 parts of lime essence and 1.6 parts of stevioside.

A method for preparing a solid beverage containing (R) -3-hydroxybutyric acid, comprising the steps of:

(1) adding 200 parts of water into a container, heating to 70 ℃ in a water bath, adding 30 parts of resistant dextrin and 30 parts of modified starch, stirring and dissolving until the liquid is uniform, and preserving heat for 30 minutes until the liquid is fully and uniformly mixed;

(2) adding 1.6 parts of lime essence and 1.6 parts of stevioside RA 97% into the solution obtained in the step (1), and uniformly stirring;

(3) directly adding 20 parts of (R) -3-hydroxybutyric acid aqueous solution (the mass concentration of (R) -3-hydroxybutyric acid is 50%) into the solution in the step (2) without cooling to room temperature, and uniformly stirring to obtain a viscous body;

(4) and (4) putting the viscous body in the step (3) into a food-grade clean tray, and freeze-drying to obtain a solid containing the (R) -3-hydroxybutyric acid.

(5) And (4) crushing and screening the solid in the step (4), uniformly mixing the part of the solid with a 40-mesh sieve, and packaging to obtain the solid beverage containing the (R) -3-hydroxybutyric acid.

Comparative example 1

Comparative example 1 is different from example 3 in that only one forming agent is used, and the rest of the raw materials and the preparation method are the same as those of example 3.

A solid beverage containing (R) -3-hydroxybutyric acid comprises the following components in parts by weight: 15 parts of (R) -3-hydroxybutyric acid, 30 parts of sodium caseinate, 20 parts of isomaltooligosaccharide, 2.5 parts of pineapple essence, 1.5 parts of fructus momordicae extract and 0.2 part of sucralose.

A method for preparing a solid beverage containing (R) -3-hydroxybutyric acid, comprising the steps of:

(1) adding 200 parts of water into a container, heating to 60 ℃ in a water bath, adding 30 parts of sodium caseinate and 20 parts of isomaltooligosaccharide, stirring to dissolve until the liquid is uniform, and preserving heat for 30 minutes until the liquid is fully and uniformly mixed;

(2) adding 2.5 parts of pineapple essence, 1.5 parts of fructus momordicae extract and 0.2 part of sucralose into the solution obtained in the step (1), uniformly stirring, and cooling to room temperature;

(3) adding 30 parts of (R) -3-hydroxybutyric acid aqueous solution (the mass concentration of (R) -3-hydroxybutyric acid is 50%) into the solution in the step (2), and uniformly stirring to obtain a mixed solution;

(4) spray drying the mixed solution in the step (3) to obtain powder containing (R) -3-hydroxybutyric acid;

(5) and (4) crushing and screening the solid in the step (4), uniformly mixing the part of the solid with a 40-mesh sieve, and packaging to obtain the solid beverage containing the (R) -3-hydroxybutyric acid.

Comparative example 2

Comparative example 2 is different from example 3 in that all raw materials are mixed together to prepare a mixed solution, and then dried to prepare a solid beverage containing (R) -3-hydroxybutyric acid.

A solid beverage containing (R) -3-hydroxybutyric acid comprises the following components in parts by weight: 15 parts of (R) -3-hydroxybutyric acid, 30 parts of sodium caseinate, 20 parts of isomaltooligosaccharide, 2.5 parts of pineapple essence, 1.5 parts of fructus momordicae extract and 0.2 part of sucralose.

A method for preparing a solid beverage containing (R) -3-hydroxybutyric acid, comprising the steps of:

(1) adding 200 parts of water into a container, heating to 60 ℃ in a water bath, adding 30 parts of sodium caseinate, 20 parts of isomaltooligosaccharide, 2.5 parts of pineapple essence, 1.5 parts of fructus momordicae extract, 0.2 part of sucralose and 30 parts of (R) -3-hydroxybutyric acid aqueous solution, wherein the mass concentration of (R) -3-hydroxybutyric acid is 50 percent, and uniformly stirring to obtain a mixed solution;

(2) spray drying the mixed solution in the step (1) to obtain solid powder containing (R) -3-hydroxybutyric acid;

(3) and (3) screening the solid powder in the step (2), uniformly mixing the part of the powder with a 40-mesh sieve, and packaging to obtain the solid beverage containing the (R) -3-hydroxybutyric acid.

Product effectiveness testing

The solid beverages containing (R) -3-hydroxybutyric acid prepared in examples 1-5 and comparative examples 1-2 were examined and mainly included the dispersion time of the solid beverages and the stability of the solid beverages. The stability of the solid beverage is mainly determined by testing the content change of the (R) -3-hydroxybutyric acid and the content change of impurity crotonic acid under high-temperature placement.

The moisture content of the solid beverage containing (R) -3-hydroxybutyric acid prepared in examples 1-5 and comparative examples 1-2 was about 2% -7%.

(1) Time of dispersion

10g of the solid beverage containing (R) -3-hydroxybutyric acid prepared in examples 1-5 and comparative examples 1-2 were weighed out, added to 200mL of water, left to stand at a water temperature of 35 ℃ and the time from the time of addition was counted to record the time for complete dissolution and dispersion of the solid beverage in water. The test results are shown in Table 1.

TABLE 1

As is clear from Table 1, the solid beverages containing (R) -3-hydroxybutyric acid prepared in the examples and comparative examples all had good dispersibility and were able to be rapidly dispersed in water to form liquid beverages.

(2) Stability of solid beverages

The solid beverage containing (R) -3-hydroxybutyric acid was analyzed by High Performance Liquid Chromatography (HPLC) for the content change of (R) -3-hydroxybutyric acid and crotonic acid as an impurity after being left at 40 deg.C for 3 months.

HPLC detection conditions:

a chromatographic column: a stainless steel octadecylsilane chemically bonded silica chromatographic column with a length of 25cm, an inner diameter of 4.6mm and a particle size of 5 microns;

mobile phase: 0.2% formic acid water: methanol (volume ratio 80: 20);

flow rate: 1.0 mL/min;

detection wavelength: 210 nm;

column temperature: 30 ℃;

sample introduction amount: 20 μ L.

As a result of examination, the solid beverages containing (R) -3-hydroxybutyric acid prepared in examples 1-5 and comparative examples 1-2 showed the changes in the contents of (R) -3-hydroxybutyric acid and crotonic acid as an impurity during storage as shown in Table 2.

TABLE 2

As can be seen from Table 2, the solid beverages prepared in the examples of the present invention showed less variation in the content of (R) -3-hydroxybutyric acid and less production of crotonic acid as an impurity during standing, particularly the products prepared in examples 1 to 4. In contrast, comparative example 1, when only one forming agent was used for half-coating, a good half-coating effect could not be achieved, and the stability of (R) -3-hydroxybutyric acid was poor during standing; comparative example 2 also did not achieve good coating by changing the preparation process.

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