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A kind of refining method of neotame
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A refining method, neotame technology, applied in the preparation method of peptides, chemical instruments and methods, peptides, etc., can solve the problem of not specifically removing impurity A, etc., to improve quality and safety requirements, meet quality and safety requirements, and improve quality Effect
Active Publication Date: 2021-06-22
JINAN CHENGHUI SHUANGDA CHEM +1
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Problems solved by technology
The patent CN1784418A only involves the synthesis method, and the liquid phase purity of the final product is required to be more than 97%, and there is no specific method for removing impurity A. From the perspective of technology, the impurity A is unavoidable, and the impurity A is the main impurity
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Embodiment 1
[0039] Put 400kg of methanol and 1200kg of water in a 2000L reaction kettle, add 300kg of neotame (liquid phase purity 95.4%, impurity A4.2%) under stirring, heat to 40°C to dissolve, then add 6kg of sodium bicarbonate, pay attention to slow addition to prevent A large amount of gas is released violently, filtered to remove insoluble impurities, then passed through ice salt water to cool down and crystallize, when the temperature drops to 5-10°C, the material is shaken, the solid material is washed with 150kg of cold water, and then filtered to obtain neotame wet product, dried under reduced pressure Material obtains dry product 270kg, refining yield 90.0%, liquid phase purity 99.950%, impurity A0.013%.
Embodiment 2
[0041] Put 150kg of methanol and 600kg of water in a 1000L reaction kettle and add 300kg of neotame (liquid phase purity 95.4%, impurity A4.2%) under stirring, heat to 60°C to dissolve, then add potassium bicarbonate 7.2kg, pay attention to adding slowly To prevent a large amount of gas from being released violently, remove insoluble impurities by filtration, then pass ice salt water to cool down and stir to crystallize, when the temperature drops to 0-5°C, shake off the material, wash the solid material with 150kg of cold water, and then filter to obtain neotame wet product, reduce The dry product obtained by pressing and drying was 277.8kg, the refined yield was 92.6%, the liquid phase purity was 99.942%, and the impurity A was 0.038%.
Embodiment 3
[0043] Put 150kg of methanol and 600kg of water in a 1000L reaction kettle and add 300kg of neotame (liquid phase purity 95.4%, impurity A4.2%) under stirring, heat to 30°C to dissolve, then add 4.5kg of sodium carbonate, pay attention to slow addition, Remove insoluble impurities by filtration, then pass through ice salt water to cool down and stir to crystallize, when the temperature drops to -5-0°C, shake off the material, wash the solid material with 150kg of cold water, filter to obtain neotame wet product, dry the material under reduced pressure to obtain dry Product 281.1kg, refined yield 93.7%, liquid phase purity 99.936%, impurity A0.051%.
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Abstract
The invention belongs to the field of chemically synthesized food additives, in particular to a method for refining neotame, namely N-[N-(3,3-dimethylbutyl)-L-α-aspartyl]-L-benzene The impurity N‑[N‑(3,3‑dimethylbutyl)‑L‑α‑aspartyl]‑L‑phenylalanine ( Impurity A) removal method. It is characterized in that: the neotame containing the hydrolyzed impurity A is heated and dissolved in a mixed solvent of methanol and water, and sodium bicarbonate is added for treatment, followed by crystallization to obtain a product, which can effectively remove the impurity A. The beneficial effect produced by the present invention is that the fine neotame is obtained by using the refined neotame of the present invention, and the refining yield is over 90%. The liquid-phase purity of refined neotame can reach over 99.9%, and impurity A can be reduced to less than 0.1%, which is more conducive to improving the quality of neotame in production, thereby further improving and meeting the quality and safety requirements of pharmaceutical excipients and food additives.
Description
technical field [0001] The invention belongs to the technical field of chemical synthesis of food additives, in particular to a method for refining neotame, which can remove the impurity N-[N-(3,3-dimethylbutyl)-L-α- Aspartyl]-L-Phenylalanine. Background technique [0002] Neotame chemical name: N-[N-(3,3-dimethylbutyl)-L-α-aspartyl]-L-phenylalanine-1-methyl ester, white crystalline powder, containing About 4.5% crystal water, is a functional sweetener. The structural formula of neotame is as follows: [0003] . [0004] Neotame has a pure sweetness, a harmonious sweetness, very close to aspartame, without the bitterness and metallic taste often associated with other strong sweeteners. The sweetness is 7000~13000 times sweeter than sucrose, 30~60 times sweeter than aspartame, and the energy value is almost zero, which is more conducive to the use of special groups of people. [0005] Neotame is not only widely used in daily life, but also widely used in pharmaceutical...
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