JPH04234985A - Production of dustless enzymic powder - Google Patents

Abstract

PURPOSE:To provide a method for producing dustless enzymic powder by inhibiting dust of a readily dusting powdery enzymic pharmaceutical bulk in which the dust may produce strong effects on the skin or mucous membranous tissues of persons handling the dust. CONSTITUTION:The invention is composed of four claims as follows. A method for adding a dust inhibitor to a readily dusting enzymic pharmaceutical bulk and producing dustless enzymic powder and extending the aforementioned method.

Description

[Detailed description of the invention]

0001

[Industrial Field of Application] The invention according to claims 1 to 5 of the present invention relates to a method for producing a dust-free enzyme powder, in which a dust-suppressing substance is dissolved or dispersed in a small amount of a volatile organic solvent to form an enzyme raw powder. This invention relates to a simple method for producing dust-free enzyme powder, which is mixed and then vacuum-dried using a conventional method. The products produced by the method of the present invention have extremely stable enzymatic activity and good dissolution workability in water, and are widely used for food production, feed addition, medicine, etc.

0002

[Prior Art] Conventional fine powder enzyme preparations have poor compatibility with water when dissolved prior to use, and the dust generated from them during handling operations significantly degrades the environment, especially for highly active cellulases and proteases. , lipase, etc. dust can have a strong effect on the skin and mucous membrane tissues of workers, and it is desirable to take measures to avoid opportunities for contact as much as possible. A commonly used method for such enzymes is to make the enzyme into a liquid form, which has already been put into practical use for many enzyme preparations. However, it is generally difficult for liquid enzymes to stably maintain enzyme activity over a long period of time compared to powdered enzymes, so stabilizers and preservatives are normally used, but this is required by the Food Sanitation Act. Not only may there be a risk of conflict, but there are also various drawbacks such as increased product flavor, solubility, and weight, and especially unstable enzymes not only have high production costs but also require strict storage conditions. There are other restrictions. In addition, the following methods are generally used to prevent dust when the enzyme cannot be easily liquefied. (b) Concentrated enzyme solution + dust suppressant → spray drying or freeze drying → powdered enzyme agent (b) Enzyme powder + dust suppressant → granulated drying → granular enzyme agent (c) Enzyme powder + granulated core material + Melt coating material → spraying, dissolving (non-drying), granulation → granular enzyme (
(See JP-A No. 63-32485.) However, (a) and (b) above require special production equipment, and there is a considerable loss of activity due to the effects of shear pressure and heating on the enzyme during production. However, the process is complicated and requires a lot of drying cost and preparation time, which is economically problematic. In addition, (c) involves adding a large amount of granulated core material or molten material, making it difficult to prepare a high-titer enzyme preparation and causing many problems in terms of equipment and technology.

0003

[Problems to be Solved by the Invention] The present inventors have made extensive efforts while considering various manufacturing methods, with the aim of making enzyme preparations dust-free and adjusting them to desired titer without applying pressure or heat. As I was considering it, I came up with a surprisingly simple and reasonable method. In other words, as a means of adding substances with a dust suppressing function such as surfactants and oils and fats, the enzyme bulk powder is dissolved or dispersed in as small a volume of volatile organic solvent as possible without first dissolving the enzyme bulk powder in water. When mixed with powder, it penetrates easily and uniformly, and the latent heat of vaporization required for re-drying is small, so from now on, it is possible to economically produce a dust-free bulk powder without agglomeration in a short time by regular vacuum drying. The present invention was completed by investigating the suitable conditions.

0004

[Means for Solving the Problems] The present invention relates to a method for producing a dust-free enzyme powder, and is comprised of claims 1 to 5. Claim 1 is a method for producing a dust-free enzyme powder. Claim 2 relates to a method for producing a dust-free enzyme powder by adding a dust-inhibiting substance to (), wherein the dust-inhibiting substance is one or two of surfactants, oils and fats, and excipients such as dextrin, maltose, and lactose. The method for producing a dust-free enzyme powder according to claim 1, characterized in that it is a combination of more than one species,
Claim 3 is the dust-free enzyme powder according to claim 1, wherein the amount of the dust-inhibiting substance added is 0.005 to 0.1 part (by weight) per 1 part (dry weight) of the bulk enzyme powder. Claim 4 relates to a method for producing a powder, and claim 4 is a method for adding the dust suppressing substance, which is dissolved or dispersed in a minimum amount of volatile organic solvent that can permeate the entire enzyme powder, and then mixed with the enzyme powder, and then a conventional method. The method for producing a dust-free enzyme powder according to claim 1, characterized in that the powder is vacuum-dried by vacuum drying, and claim 5 is characterized in that the volatile organic solvent is ethanol, methanol, isopropanol, acetone, etc., which are commonly used for enzyme purification. The method for producing a dust-free enzyme powder according to claim 1, characterized in that the method is directed to producing a dust-free enzyme powder without deactivation of the respective enzymes. be.

[0005] Suitable dust suppressing substances in the present invention include glycerin fatty acid ester, sorbitan fatty acid ester, propylene glycol fatty acid ester, soybean lecithin, egg lecithin, enzyme-treated lecithin, soybean oil, corn oil, cottonseed oil, castor oil, Examples include liquid paraffin and polyethylene glycol, and one or more of them may be used in combination. In addition, the amount of these additions is 1
(dry weight) part to 0.005 to 0.1 part (by weight) of the dust suppressing substance. The volatile organic solvent used in the present invention is ethanol, methanol, isopropanol, acetone, etc., which are generally used for enzyme purification, and the amount added is 0.1 part (dry weight) of enzyme bulk powder. A minimum amount of 0.7 to 0.7 parts (by volume), preferably 0.3 parts by volume, is sufficient for the solvent to permeate the entire enzyme bulk powder. In addition, this, together with the fact that there is no need to add water when adding a volatile organic solvent, is a factor in reducing drying costs and preventing enzyme deactivation. The enzyme agents used in the present invention include xylanase, cellulase, protease, β-galactosidase, pectinase, lipase, amylase, etc., and these can be used alone or in combination. In general, it is also effective for enzymes whose dust has a particularly negative effect on the working environment, and for enzymes whose liquefaction is extremely difficult due to physical properties and stability. Furthermore, the origin and purity of the enzyme bulk powder do not matter. In the present invention, as a dispersing agent, dextrin, lactose, galactose, etc. may be added as long as they are insoluble in the volatile organic solvent used in the method of the present invention and are common. The enzyme bulk powder and the dust suppressing substance are mixed by first dissolving (or dispersing) the dust suppressing substance in approximately 95% ethanol, and then adding the powder to the enzyme bulk powder and mixing. Although the invention of claim 4 includes vacuum drying by a conventional method, this vacuum drying may be carried out under normally used conditions. For example, the vacuum drying device may be a groove type vacuum dryer or an electric constant temperature vacuum dryer, and the temperature is preferably 5 to 30°C, the degree of vacuum is 10-3 to 10-1 mmHg, and the time is 5 to 24 hours, respectively. used. Hereinafter, the present invention will be explained in more detail with reference to Test Examples and Examples. However, the present invention is not limited to this description.

[0006]

[Example] ○Test Example 1 Xylanase bulk powder (60mesh manufactured by Shin Nippon Chemical Industry)
30ml of 95% ethanol in which 100g of PASS bulk powder) and 2g of various additives (dust suppressants) shown in Table 1 (equal amounts of 1g each when used in combination) are dissolved (or dispersed).
1 was mixed and dried for 18 hours at a temperature of 30° C. and a degree of vacuum of 10 −1 mmHg using a constant temperature vacuum dryer (manufactured by Satake Electric Machinery Co., Ltd.) to prepare an enzyme powder. As shown in Table 1, the results showed that the additives containing glycerin fatty acid ester, castor oil, and polyethylene glycol (molecular weight: 400) were dissolved in 95% ethanol, while the additives containing glycerin fatty acid ester, castor oil, and polyethylene glycol (molecular weight: 400) were dissolved in 95% ethanol; Lecithin and egg lecithin showed good dispersibility. Also, even oils and fats that exhibit a separated state, which do not dissolve or disperse in 95% ethanol when used alone, can be given similar dispersibility by mixing with a substance such as soybean lecithin. Furthermore, the activity yield after vacuum drying with 95% ethanol was 98 to 100%, demonstrating the dust-preventing effect of the enzyme powder.

[Table 1]

○Test Example 2 Xylanase bulk powder (60mesh manufactured by Shin Nippon Chemical Industry)
pass bulk powder) 100g and 95% ethanol 30 in which soybean lecithin and soybean oil are dispersed in the prescribed amounts shown in Table 2.
ml, and a constant temperature vacuum dryer (manufactured by Satake Electric Machinery Co., Ltd.)
18 at a temperature of 10°C and a vacuum of 10-1 mmHg.
The enzyme powder was prepared by drying for a while. As shown in Table 2, the activity yield of vacuum drying was 98 to 100%, the solubility of the enzyme powder in water was improved, and no deterioration of the solubility was observed when the amount of additives was 5% or less. First, the dust-preventing effect was obvious when 1% or more was added.

[Table 2]

○Test Example 3 Xylanase bulk powder (60mesh manufactured by Shin Nippon Chemical Industry)
pass bulk powder) and 100 g of each predetermined amount of glycerin fatty acid ester or castor oil shown in Table 3 were dissolved.
Mix with 30ml of 5% ethanol and place in a constant temperature vacuum dryer (
(manufactured by Satake Electric Machine Industry Co., Ltd.) at a temperature of 10℃ and a degree of vacuum of 1.
Enzyme powder was prepared by drying at 0-1 mmHg for 18 hours. As shown in Table 3, the activity yield after vacuum drying with 95% ethanol was 98 to 100%, the solubility in water was improved and the solubility was good, and the addition of 1% or more prevented dust. The effect was clear.

[Table 3]

○Test Example 4 Cellulase bulk powder (60mesh p
Mix 100 g of Ass bulk powder with 30 ml each of 95% ethanol, methanol, isopropanol, or acetone in which 2.0 g of soybean lecithin is dispersed, and dry at a temperature of 10°C using a constant temperature vacuum dryer (manufactured by Satake Electric Machinery Co., Ltd.). The enzyme powder was prepared by drying for 18 hours at a vacuum degree of 10-1 mmHg. As shown in Table 4, the yield after vacuum drying with 95% of various organic solvents was 99 to 100%, the solubility in water was improved, the solubility was good, and the dust prevention effect was obvious. It was hot.

[Table 4]

0010

[Examples] Xylanase originating from Trichoderma SP, protease and β-galactosidase originating from Aspergillus SP, pectinase and lipase originating from Aspergillus niger, Rhizopus S.
1.0 kg of each amylase bulk powder originating from P (both 60mesh pass bulk powder manufactured by Shin Nippon Chemical Industry) and 10 g of a mixture of equal amounts of soybean lecithin and castor oil (Japanese Pharmacopoeia)
Mix with 300 ml of 95% ethanol in which
An enzyme powder was prepared by drying for 18 hours at a temperature of 30° C. and a degree of vacuum of 10 −1 mmHg using a constant temperature vacuum dryer (manufactured by Satake Electric Machinery Co., Ltd.). As shown in Table 5, the activity yield of the vacuum-dried powder was 98 to 100%, the solubility in water was improved, the solubility was good, and the dust prevention property was obvious.

[Table 5] The measurement method for each agent used in the present invention will be described below. Xylanase measurement method: Using xylan as a substrate, the enzyme is allowed to act at pH 5.0 and 40°C, and the resulting reducing sugars are determined colorimetrically using the Somogyi-Nelson method. Cellulase measurement method CMC (Carboxymethyl Cell)
The enzyme is allowed to act on the enzyme at pH 4.0 and 40° C. using the enzyme (Lulose) as a substrate, and the resulting reducing sugar is determined colorimetrically using the Somogyi-Nelson method. Protease measurement method: pH 6.0, 30 using milk casein as a substrate
The enzyme is allowed to act at 0.degree. C., and the produced TCA-soluble substance is colored with Folin's reagent and quantified colorimetrically. β-galactosidase measurement method ONPG (2-Nitropheny1-β-
The enzyme is applied to D-galactopyranoside as a substrate at pH 4.5 and 30°C, and 0-nitrophenol produced by the decomposition is determined colorimetrically. Pectinase measurement method: pH 4.5, 40 using apple pectin as a substrate
Enzyme is applied at °C to decompose the ester bonds within the pectin molecule, and the resulting carboxyl groups are quantified by alkaline titration. Lipase measurement method Enzyme is allowed to act on olive oil at pH 6.0 and 37°C as a substrate, and the fatty acids produced are determined by alkaline titration. Amylase measurement method pH 4.5, 40 using soluble starch as substrate
Fehling and reducing sugars are produced by using enzymes at ℃.
Quantitate using the Lehmann-Shaul method.

[0011]

[Effects of the Invention] Claim 1 of the present invention provides a method for producing a dust-free enzyme powder by adding a dust suppressing substance as a dust prevention measure for a powdered enzyme agent that is not easily liquefied and easily generates dust. Accordingly, this method can suppress the generation of dust. Claim 2 is the dust-free enzyme powder according to claim 1, wherein the dust suppressing substance is one or a combination of two or more of surfactants, oils and fats, and excipients such as dextrin, maltose, and lactose. By specifying the dust suppressing substance as described above, the effects of the invention of claim 1 can be advantageously achieved. Claim 3 is the dust-free enzyme powder according to claim 1, wherein the amount of the dust-inhibiting substance added is 0.005 to 0.1 part (by weight) per 1 part (dry weight) of the bulk enzyme powder. By specifying the amount of the dust suppressing substance to be added to the bulk enzyme powder as described above, the effects of the invention of claim 1 can be made even more advantageous. Claim 4 provides that the dust suppressing substance is added by dissolving or dispersing it in the minimum amount of volatile organic solvent that can permeate the entire enzyme bulk powder, mixing it with the enzyme bulk powder, and then vacuum drying it by a conventional method. Claim 1
According to the method for producing a dust-free enzyme powder, the effects of the invention of claim 1 can be made even more advantageous by minimizing the dispersion, mixing, and addition of the dust suppressing substance. Claim 5 provides that the volatile organic solvent is ethanol, methanol, isopropanol,
The present invention relates to a method for producing a dust-free enzyme powder such as acetone, which is generally used for the purification of enzymes, and further facilitates the implementation of the invention as claimed in claim 1. Considering claims 1 to 5 of the present invention as a whole, a simple method is to dissolve or disperse in a volatile organic solvent and mix it with the bulk enzyme powder, and then remove only the organic solvent by vacuum drying using a conventional method. This makes it possible to quickly and economically produce dust-free enzyme powder without applying pressure, heating, or adding water, which are factors that cause enzyme inactivation. In the dust-free enzyme powder obtained by the method of the present invention, if no agglomerates are present in the enzyme raw powder and the dispersing agent before dust prevention treatment, the dried product will no longer form into agglomerates. In addition, this method causes almost no loss of enzyme activity, and the produced dust-free enzyme powder does not aggregate, making it easy to dissolve the enzyme powder in water, and the quality is stable even during long-term storage. Therefore, extremely advantageous effects can be obtained industrially. In addition, since almost no loss of activity is observed, a high yield can be obtained, it can withstand long-term storage, maintains good solubility in water, and does not generate dust. This dust-free enzyme powder can be used for food production, feed addition, medicine, etc., and its production method can be used for the production of dust-free preparations in the food industry and pharmaceutical industry.

Claims (5)

[Claims] 1. A method for producing a dust-free enzyme powder by adding a dust-inhibiting substance to an enzyme bulk powder that tends to generate dust. 2. The dust-free enzyme according to claim 1, wherein the dust suppressing substance is one or a combination of two or more of surfactants, oils and fats, and excipients such as dextrin, maltose, and lactose. Method of manufacturing powder. [Claim 3] The amount of the dust suppressing substance added is 1 (
0.005 to 0.1 (weight) per part (dry weight)
2. The method for producing a dust-free enzyme powder according to claim 1, characterized in that: 4. The dust suppressing substance is added by dissolving or dispersing it in the minimum amount of volatile organic solvent that can permeate the entire enzyme bulk powder, mixing it with the enzyme bulk powder, and then vacuum drying it by a conventional method. A method for producing a dust-free enzyme powder according to claim 1. 5. Claim 1, wherein the volatile organic solvent is one commonly used for enzyme purification, such as ethanol, methanol, isopropanol, acetone, etc.
A method for producing dust-free enzyme powder.