CN105315330A - Cooling crystallization method for N-alpha-L-phthalein-L-phenylalanine 1-methyl aspartate - Google Patents
Cooling crystallization method for N-alpha-L-phthalein-L-phenylalanine 1-methyl aspartate Download PDFInfo
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- CN105315330A CN105315330A CN201410378512.1A CN201410378512A CN105315330A CN 105315330 A CN105315330 A CN 105315330A CN 201410378512 A CN201410378512 A CN 201410378512A CN 105315330 A CN105315330 A CN 105315330A
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- methyl esters
- asparagus fern
- phenylpropyl alcohol
- fern ammonia
- phthalein
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Abstract
The invention discloses a cooling crystallization method for N-alpha-L-phthalein-L-phenylalanine 1-methyl aspartate. The method comprises the following steps of preparing a solution, carrying out cooling, standing and crystallizing progressively and finally carrying out washing and baking. According to the cooling crystallization method for the N-alpha-L-phthalein-L-phenylalanine 1-methyl aspartate, disclosed by the invention, the N-alpha-L-phthalein-L-phenylalanine 1-methyl aspartate can be prepared by only pure water and carrying out cooling, standing and crystallizing progressively and carrying out washing and baking; and the method is simple and practical.
Description
Technical field
The invention belongs to chemical field, particularly a kind of crystallisation by cooling method of N-α-L-asparagus fern ammonia phthalein-L-phenylpropyl alcohol 1-propylhomoserin methyl esters.
Background technology
N-α-L-asparagus fern ammonia phthalein-L-phenylpropyl alcohol 1-propylhomoserin methyl esters (C
14h
18n
2o
5), be commonly called as aspartame, be a kind of artificial sweetner of non-carbohydrate class, its thermostability is poor, and less than 55 DEG C are relatively stable, and relatively stable between pH2 ~ 4, the solubleness of its hydrochloride is larger.
N-α-L-asparagus fern ammonia phthalein-L-phenylpropyl alcohol 1-propylhomoserin methyl esters (C
14h
18n
2o
5) in vivo rapid metabolization be aspartic acid, phenylalanine and methyl alcohol.N-α-L-asparagus fern ammonia phthalein-L-phenylpropyl alcohol 1-propylhomoserin methyl esters (C is taken in even if a large amount of
14h
18n
2o
5) (200 milligrams per kilogram of body weight), can not aspartame be detected in blood.
By N-α-L-asparagus fern ammonia phthalein-L-phenylpropyl alcohol 1-propylhomoserin methyl esters (C
14h
18n
2o
5) aspartic acid that provides only accounts for the 1-2% of human body institute's every day intake.Although aspartic acid and some amino acid (as L-glutamic acid) combined action may cause damage to neurocyte, research shows N-α-L-asparagus fern ammonia phthalein-L-phenylpropyl alcohol 1-propylhomoserin methyl esters (C
14h
18n
2o
5) there is no neurotoxicity, and by N-α-L-asparagus fern ammonia phthalein-L-phenylpropyl alcohol 1-propylhomoserin methyl esters (C
14h
18n
2o
5) aspartic acid taken in cannot reach enough toxigenous dosage.
Methyl alcohol in vivo metabolism is formaldehyde, and then is oxidized to formic acid, with formic acid form in vivo the residence time the longest, be therefore considered to the mechanism of action of methyl alcohol toxicity.But by N-α-L-asparagus fern ammonia phthalein-L-phenylpropyl alcohol 1-propylhomoserin methyl esters (C
14h
18n
2o
5) methyl alcohol that provides can not cause serious health problems.First, N-α-L-asparagus fern ammonia phthalein-L-phenylpropyl alcohol 1-propylhomoserin methyl esters (C
14h
18n
2o
5) methyl alcohol that provides is less than fruit juice and citrus fruit, and in the fermentation such as beer class drink, methanol content is higher.Then, N-α-L-asparagus fern ammonia phthalein-L-phenylpropyl alcohol 1-propylhomoserin methyl esters (C
14h
18n
2o
5) the formaldehyde amount that produces is far smaller than the formaldehyde amount that human normal diet produces, even take in aspartame with maximal dose, formaldehyde and formic acid concn there is no obvious rising in blood.
Therefore N-α-L-asparagus fern ammonia phthalein-L-phenylpropyl alcohol 1-propylhomoserin methyl esters (C
14h
18n
2o
5) be also a kind of sweeting agent of health.
N-α-L-asparagus fern ammonia phthalein-L-phenylpropyl alcohol 1-propylhomoserin methyl esters (C
14h
18n
2o
5) in current production technique and in production process, all can there is the phenomenon that alkali local is excessive, the N-α-L-asparagus fern ammonia phthalein-L-phenylpropyl alcohol 1-propylhomoserin methyl esters (C of each manufacturer
14h
18n
2o
5) all contain impurity 2-(5-benzyl-3 in finished product, 6-diketopiperazine-2-base) acetic acid, some producers control well, foreign matter content is lower, some producer controls weaker, foreign matter content is higher, impurity 2-(5-benzyl-3,6-diketopiperazine-2-base) removal is very difficult afterwards in acetic acid generation, a part can be removed by the mode of washing, but overall yield is also affected, impurity 2-(5-benzyl-3,6-diketopiperazine-2-base) existence of acetic acid can have influence on N-α-L-asparagus fern ammonia phthalein-L-phenylpropyl alcohol 1-propylhomoserin methyl esters (C
14h
18n
2o
5) quality and yield.
Summary of the invention
The object of this invention is to provide one, to solve the problems of the prior art.
For achieving the above object, the present invention is by the following technical solutions:
A crystallisation by cooling method for N-α-L-asparagus fern ammonia phthalein-L-phenylpropyl alcohol 1-propylhomoserin methyl esters, comprises the steps:
A, obtain solution, be mixed with the aqueous solution by N-α-L-asparagus fern ammonia phthalein-L-phenylpropyl alcohol 1-propylhomoserin methyl esters;
B, cooling, prepare mother liquor cooling, have sub-fraction N-α-L-asparagus fern ammonia phthalein-L-phenylpropyl alcohol 1-propylhomoserin methyl esters crude crystalline to separate out by steps A;
C, leave standstill, have more N-α-L-asparagus fern ammonia phthalein-L-phenylpropyl alcohol 1-propylhomoserin methyl esters crude crystalline to separate out;
D, crystallization, most of N-α-L-asparagus fern ammonia phthalein-L-phenylpropyl alcohol 1-propylhomoserin methyl esters crude crystalline is separated out;
E, repeating step B and D;
F, washing and drying, then N-α-L-asparagus fern ammonia phthalein-L-phenylpropyl alcohol 1-propylhomoserin methyl esters crude product washing and drying is obtained N-α-L-asparagus fern ammonia phthalein-L-phenylpropyl alcohol 1-propylhomoserin methyl esters sterling.
Further, during described steps A obtained aqueous solution, adopt pure water.
Preferably, described step B is cooled to 50 degree.
Further, described step C leaves standstill 30min.
Preferably, described step e, at least repeating step B and D twice.
Further, described step e, during repeating step B and D, each cooling temperature reduces by 10 degree, and time of repose extends 1 times.
Beneficial effect of the present invention: the crystallisation by cooling method of a kind of N-α of the present invention-L-asparagus fern ammonia phthalein-L-phenylpropyl alcohol 1-propylhomoserin methyl esters, only need pure water to add to cool step by step, leave standstill and crystallization, the method is simple and practical.
Embodiment
In order to make object of the present invention, technical scheme and advantage clearly understand, below in conjunction with embodiment, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, be not intended to limit the present invention.
A crystallisation by cooling method for N-α-L-asparagus fern ammonia phthalein-L-phenylpropyl alcohol 1-propylhomoserin methyl esters, comprises the steps:
A, obtain solution, be mixed with the aqueous solution by N-α-L-asparagus fern ammonia phthalein-L-phenylpropyl alcohol 1-propylhomoserin methyl esters;
B, cooling, prepare mother liquor cooling, have sub-fraction N-α-L-asparagus fern ammonia phthalein-L-phenylpropyl alcohol 1-propylhomoserin methyl esters crude crystalline to separate out by steps A;
C, leave standstill, have more N-α-L-asparagus fern ammonia phthalein-L-phenylpropyl alcohol 1-propylhomoserin methyl esters crude crystalline to separate out;
D, crystallization, most of N-α-L-asparagus fern ammonia phthalein-L-phenylpropyl alcohol 1-propylhomoserin methyl esters crude crystalline is separated out;
E, repeating step B and D;
F, washing and drying, then N-α-L-asparagus fern ammonia phthalein-L-phenylpropyl alcohol 1-propylhomoserin methyl esters crude product washing and drying is obtained N-α-L-asparagus fern ammonia phthalein-L-phenylpropyl alcohol 1-propylhomoserin methyl esters sterling.
During described steps A obtained aqueous solution, adopt pure water.
Described step B is cooled to 50 degree.
Described step C leaves standstill 30min.
Described step e, at least repeating step B and D twice.
Described step e, during repeating step B and D, each cooling temperature reduces by 10 degree, and time of repose extends 1 times.
The specific embodiment of the present invention is described although above-mentioned in conjunction with the embodiments; but not limiting the scope of the invention; one of ordinary skill in the art should be understood that; on the basis of technical scheme of the present invention, those skilled in the art do not need to pay various amendment or distortion that performing creative labour can make still within protection scope of the present invention.
Claims (6)
1. a crystallisation by cooling method for N-α-L-asparagus fern ammonia phthalein-L-phenylpropyl alcohol 1-propylhomoserin methyl esters, is characterized in that, comprise the steps:
A, obtain solution, be mixed with the aqueous solution by N-α-L-asparagus fern ammonia phthalein-L-phenylpropyl alcohol 1-propylhomoserin methyl esters;
B, cooling, prepare mother liquor cooling, have sub-fraction N-α-L-asparagus fern ammonia phthalein-L-phenylpropyl alcohol 1-propylhomoserin methyl esters crude crystalline to separate out by steps A;
C, leave standstill, have more N-α-L-asparagus fern ammonia phthalein-L-phenylpropyl alcohol 1-propylhomoserin methyl esters crude crystalline to separate out;
D, crystallization, most of N-α-L-asparagus fern ammonia phthalein-L-phenylpropyl alcohol 1-propylhomoserin methyl esters crude crystalline is separated out;
E, repeating step B and D;
F, washing and drying, then N-α-L-asparagus fern ammonia phthalein-L-phenylpropyl alcohol 1-propylhomoserin methyl esters crude product washing and drying is obtained N-α-L-asparagus fern ammonia phthalein-L-phenylpropyl alcohol 1-propylhomoserin methyl esters sterling.
2. the crystallisation by cooling method of N-α-L-asparagus fern ammonia phthalein-L-phenylpropyl alcohol 1-propylhomoserin methyl esters according to claim 1, is characterized in that, during described steps A obtained aqueous solution, adopts pure water.
3. the crystallisation by cooling method of N-α-L-asparagus fern ammonia phthalein-L-phenylpropyl alcohol 1-propylhomoserin methyl esters according to claim 1, it is characterized in that, described step B is cooled to 50 degree.
4. the crystallisation by cooling method of N-α-L-asparagus fern ammonia phthalein-L-phenylpropyl alcohol 1-propylhomoserin methyl esters according to claim 1, it is characterized in that, described step C leaves standstill 30min.
5. the crystallisation by cooling method of N-α-L-asparagus fern ammonia phthalein-L-phenylpropyl alcohol 1-propylhomoserin methyl esters according to claim 1, is characterized in that, described step e, at least repeating step B and D twice.
6. the crystallisation by cooling method of N-α-L-asparagus fern ammonia phthalein-L-phenylpropyl alcohol 1-propylhomoserin methyl esters according to claim 1, is characterized in that, described step e, and during repeating step B and D, each cooling temperature reduces by 10 degree, and time of repose extends 1 times.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410378512.1A CN105315330A (en) | 2014-08-04 | 2014-08-04 | Cooling crystallization method for N-alpha-L-phthalein-L-phenylalanine 1-methyl aspartate |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410378512.1A CN105315330A (en) | 2014-08-04 | 2014-08-04 | Cooling crystallization method for N-alpha-L-phthalein-L-phenylalanine 1-methyl aspartate |
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| Publication Number | Publication Date |
|---|---|
| CN105315330A true CN105315330A (en) | 2016-02-10 |
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| CN201410378512.1A Pending CN105315330A (en) | 2014-08-04 | 2014-08-04 | Cooling crystallization method for N-alpha-L-phthalein-L-phenylalanine 1-methyl aspartate |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0091787A1 (en) * | 1982-04-12 | 1983-10-19 | Ajinomoto Co., Inc. | Process for crystallizing alpha-L-aspartyl-L-phenylalanine-methyl ester |
| CN102584938A (en) * | 2012-03-02 | 2012-07-18 | 孟州市华兴生物化工有限责任公司 | Crystallizing method of aspartame |
| CN103626843A (en) * | 2012-08-21 | 2014-03-12 | 常州光辉生物科技有限公司 | Impurity control method for production of aspartame |
-
2014
- 2014-08-04 CN CN201410378512.1A patent/CN105315330A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0091787A1 (en) * | 1982-04-12 | 1983-10-19 | Ajinomoto Co., Inc. | Process for crystallizing alpha-L-aspartyl-L-phenylalanine-methyl ester |
| CN102584938A (en) * | 2012-03-02 | 2012-07-18 | 孟州市华兴生物化工有限责任公司 | Crystallizing method of aspartame |
| CN103626843A (en) * | 2012-08-21 | 2014-03-12 | 常州光辉生物科技有限公司 | Impurity control method for production of aspartame |
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Application publication date: 20160210 |