阅读说明：本技术 纽甜中粘性物质的去除方法 (Method for removing viscous substances in neotame ) 是由 王振东 陈良 刘传滨 于 2020-08-20 设计创作，主要内容包括：本发明属于食品添加剂技术领域,具体涉及一种纽甜中粘性物质的去除方法。本发明所述的纽甜中粘性物质的去除方法,使用混合有机溶剂溶解纽甜,经过滤、结晶、离心、重结晶、再离心、烘干后,得到高纯度的纽甜；所述的混合有机溶剂为异丙醚和甲醇的混合物。本发明所述的纽甜中粘性物质的去除方法,能够将杂质有效的去除,保证了结晶体系的纯净,提高了产品的应用性能。(The invention belongs to the technical field of food additives, and particularly relates to a method for removing viscous substances in neotame. According to the method for removing the sticky substances in the neotame, the neotame is dissolved by using a mixed organic solvent, and the high-purity neotame is obtained after filtration, crystallization, centrifugation, recrystallization, recentrifugation and drying; the mixed organic solvent is a mixture of isopropyl ether and methanol. The method for removing the sticky substances in the neotame can effectively remove impurities, ensure the purity of a crystalline system and improve the application performance of the product.)

1. A method for removing viscous substances in neotame is characterized by comprising the following steps: dissolving neotame by using a mixed organic solvent, and obtaining high-purity neotame after filtering, crystallizing, centrifuging, recrystallizing, re-centrifuging and drying;

the mixed organic solvent is a mixture of isopropyl ether and methanol.

2. The method of claim 1, further comprising the step of: the method comprises the following steps:

(1) dissolving neotame in a mixed solution of water and methanol, adding isopropyl ether, and stirring;

(2) after stirring, filtering to obtain filtrate;

(3) crystallizing the filtrate;

(4) carrying out centrifugal treatment to obtain neotame crystals;

(5) repeating the steps (1) to (4) for recrystallization;

(6) and (5) drying the neotame crystals obtained in the step (5) to obtain the high-purity neotame.

3. The method of claim 2, further comprising the step of: in the step (1), the mass ratio of the methanol to the neotame is 1: 2-1: 1.

4. The method of claim 2, further comprising the step of: in the step (1), the dissolving temperature is 30-80 ℃.

5. The method of claim 2, further comprising the step of: in the step (1), the stirring time is 30-180 min.

6. The method of claim 2, further comprising the step of: in the step (1), the mass ratio of the isopropyl ether to the neotame is 4: 25-1: 25.

7. The method of claim 2, further comprising the step of: in the step (3), slowly cooling crystallization is adopted, the filtrate is added into a crystallization kettle and stirred for 3-5 hours, then standing crystallization is carried out, and the temperature in the crystallization kettle is reduced by 2 ℃ per hour.

8. The method of claim 2, further comprising the step of: and (4) recovering and recycling the centrifugal mother liquor obtained by the centrifugal treatment.

9. The method of claim 2, further comprising the step of: in the step (6), the drying temperature is 50-65 ℃, and the drying time is 6-8 hours.

Technical Field

The invention belongs to the technical field of food additives, and particularly relates to a method for removing viscous substances in neotame.

Background

Neotame, chemical name is: n- [ N- (3, 3-dimethylbutyl) -L-alpha-aspartyl ] -L-phenylalanine-1-methyl ester, which is a white crystalline powder containing about 4.5% of crystal water, is a functional sweetener. Has pure sweet taste, synergistic sweet taste, close to aspartame, and no bitter taste and metallic taste of other intense sweeteners. The sweetness is 7000-13000 times that of cane sugar and 30-60 times that of aspartame, and the energy value is almost zero.

Currently, neotame (N- [ N- (3, 3-dimethylbutyl) -L-alpha-aspartic acid ] -L-phenylalanine-1-methyl ester) is a high-potency sweetener developed by Neutravist, USA, which has the advantages of high sweetness, low calorie, high stability and the like, and the potential of neotame as a good sweetener is gradually discovered along with the application depth.

However, in the application process, the by-product is easily generated in the hydrogenation reaction process, so that the quality problems of stickiness, caking, poor solubility and the like of the product occur in the use process.

Disclosure of Invention

The technical problem to be solved by the invention is as follows: the method for removing the sticky substances in the neotame overcomes the defects of the prior art, can effectively remove impurities, ensures the purity of a crystalline system, and improves the application performance of the product.

According to the method for removing the sticky substances in the neotame, the neotame is dissolved by using a mixed organic solvent, and the high-purity neotame is obtained after filtration, crystallization, centrifugation, recrystallization, recentrifugation and drying;

the mixed organic solvent is a mixture of isopropyl ether and methanol.

Specifically, the method comprises the following steps:

(1) dissolving neotame in a mixed solution of water and methanol, adding isopropyl ether, and stirring;

(2) after stirring, filtering to obtain filtrate;

(3) crystallizing the filtrate;

(4) carrying out centrifugal treatment to obtain neotame crystals;

(5) repeating the steps (1) to (4) for recrystallization;

(6) and (5) drying the neotame crystals obtained in the step (5) to obtain the high-purity neotame.

In the step (1), the mass ratio of the methanol to the neotame is 1: 2-1: 1.

In the step (1), the dissolution temperature is 30 to 80 ℃, preferably 40 ℃.

In the step (1), the stirring time is 30-180 min.

In the step (1), the mass ratio of the isopropyl ether to the neotame is 1: 25-4: 25.

In the step (3), slowly cooling crystallization is adopted, the filtrate is added into a crystallization kettle and stirred for 3-5 hours, then standing crystallization is carried out, the temperature in the crystallization kettle is reduced by 2 ℃ per hour, and the temperature is reduced to 5-10 ℃.

In the step (4), the centrifugal mother liquor obtained by centrifugal treatment is recycled and reused, and the solvent for reuse can be recycled after the centrifugal mother liquor is distilled and filtered, so that the cost is saved and the pollution is reduced.

In the step (5), the drying temperature is 50-65 ℃, preferably 58 ℃, and the drying time is 6-8 hours, preferably 7 hours. The drying is mainly to remove moisture and solvent, because neotame has a small amount of methanol solvent in the synthesis process, the methanol solvent is volatile, and no residue is left after drying.

The filtration is carried out by using a filter element with 0.1-0.3 μm, preferably a filter element with 0.2 μm.

According to the invention, the neotame is effectively dissolved by using purified water and methanol, the isopropyl ether is added to dissolve the neotame, then crystallization is carried out, and secondary crystallization is carried out, so that the purity of the neotame is obviously improved.

The invention adopts a drying process after centrifugation to effectively remove volatile organic solvent.

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

the treatment method disclosed by the invention is simple and efficient, is energy-saving and environment-friendly, can effectively remove organic impurity components in the neotame, ensures the purity of a crystal system, prolongs the storage performance of a product, and improves the application performance of the product.

Detailed Description

The present invention will be further described with reference to the following examples.