Preparation method for S-adenosine-L-methionine disulfate tosylate

A technology of toluenesulfonic acid sulfuric acid and p-toluenesulfonic acid, which is applied to the preparation of sugar derivatives, chemical instruments and methods, sugar derivatives, etc., can solve the problems of reduced heating and cooling speed, increased heating unevenness, equipment and operation Require high-level problems, achieve the effect of less impurity adsorption, high product recovery rate, and low production cost

Active Publication Date: 2012-01-18
BEIJING UNIV OF CHEM TECH
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  • Abstract
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Problems solved by technology

Especially as the processing capacity increases, the degree of uneven heating increases, and the heating and cooling speed decreases, resulting in a large amount of degradation of bacteria, and a decrease in the extraction rate of SAM, resulting in a large loss of SAM
Therefore, in order to reduce the degradation rate of SAM and reduce the loss of SAM, the SAM extraction process requires strict control of the reaction temperature and reaction time, and requires the system to have a higher heating and cooling rate, higher requirements for equipment and operation, and higher costs. This method is limited to laboratory use and is not suitable for industrial application

Method used

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  • Preparation method for S-adenosine-L-methionine disulfate tosylate

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030](1) During the fermentation process for preparing SAM, Saccharomyces cerevisiae is used for high-density fermentation, and the precursor L-methionine is added to make the obtained fermentation broth have a higher SAM-rich bacterial cell content. After the fermentation, 30 L of fermentation broth was centrifuged at 6000 rpm for 10 min at 4° C. to obtain about 10 kg of wet bacteria.

[0031] (2) Take 8kg of wet bacteria prepared in step (1), add 24L of 50°C, 0.1M H 2 SO 4 The solution was homogenized at 50° C. for 1 hour, and the homogenizer rotated at 500 rpm. After the cells were crushed, the temperature was cooled with cold water, and the cells were centrifuged at 6000 rpm for 10 min at 4°C to remove the cell fragments to obtain the SAM extract. The yield, concentration and yield are shown in Table 1.

[0032] (3) Using an ultrafiltration membrane with a molecular weight cut-off of 10,000 to perform ultrafiltration on the SAM extract obtained in step (2) to remove pro...

Embodiment 2

[0038] Embodiment 2 is different from embodiment 1 in that:

[0039] (2) Take 1kg of the wet bacteria obtained in step (1), add 5L of 30°C, 0.2M H 2 SO 4 The solution was homogenized for 3 hours at 30° C., and the speed of the homogenizer was 300 rpm. The results are shown in Table 1.

[0040] (3) Using an ultrafiltration membrane with a molecular weight cut-off of 6000 to carry out ultrafiltration treatment on the SAM extract prepared in step (2).

[0041] (4) adjust the pH of the SAM filtrate prepared by step (3) to 7 with 20% NaOH solution, send into an ion exchange column with a column volume of about 0.3L for ion exchange treatment, and the exchange capacity of its resin is 90g / L resin, the feed concentration of SAM is 4.0g / L, the feed speed is 4.0BV / h, and the feed amount is 22.5BV; the consumption of deionized water is 5BV, and the flow rate is 1BV / h; the concentration of sulfuric acid solution is 0.05M, the flow rate is 1BV / h, the results are shown in Table 1.

[...

Embodiment 3

[0046] Embodiment 3 is different from embodiment 1 in that:

[0047] (2) Take 10kg of wet bacteria prepared in step (1), add 20L of 60°C, 0.5M H 2 SO 4 The solution was homogenized at 60°C for 0.5h, and the speed of the homogenizer was 600rpm. The results are shown in Table 1.

[0048] (3) Using an ultrafiltration membrane with a molecular weight cut-off of 6000 to carry out ultrafiltration treatment on the SAM extract prepared in step (2).

[0049] (4) adjust the pH of the SAM filtrate prepared by step (3) to 4 with 20% NaOH solution, send into an ion exchange column with a column volume of about 2.1L for ion exchange treatment, and the exchange capacity of its resin is 120g / L resin, the feed concentration of SAM is 10.0g / L, the feed rate is 1.0BV / h, and the feed amount is 12.0BV; the consumption of deionized water is 4BV, and the flow rate is 2BV / h; the concentration of sulfuric acid solution is 0.25M, the flow rate is 4BV / h, the results are shown in Table 1.

[0050] (...

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Abstract

The invention discloses a preparation method for S-adenosine-L-methionine disulfate tosylate. The method comprises the following steps of: precipitating S-adenosine-L-methionine (SAM) which is prepared through thallus collection, cell disruption of an acid heat method, extraction, and separation and purification; adjusting and controlling proportion of sulfate radial to para-toluenesulfonic acid radical; and drying to prepare the high-purity SAM disulfate tosylate. The method has the advantages of simple technological line, high processing capacity, product recovery rate of up to 75-80 percent, proportion of active ingredients in a product of more than 90 percent, product purity of up to 96-98 percent, corresponding indexes meeting pharmacopoeial requirements, low production cost and capability of realizing industrial production.

Description

technical field [0001] The invention relates to the field of biochemical separation of bioengineering, more specifically, the invention relates to a preparation method of S-adenosyl-L-methionine p-toluenesulfonic acid double salt. Background technique [0002] S-adenosyl-L-methionine (S-adenosyl-L-methionine, SAM, SAMe or AdoMet) is a sulfonyl compound of the organic tetravalent sulfur form (metal sulfonium) of methionine, known as " "Active methionine" is an important metabolic intermediate widely present in organisms, first discovered by Cantoni in 1952. SAM is a pair of chiral substances, with two isomers: (R, S)-SAM and (S, S)-SAM, only (S, S)-SAM has biological activity. In organisms, SAM is synthesized by L-methionine (L-Met) and adenosine triphosphate (ATP) through SAM synthetase (S-adenosylmethionine synthetase). Since SAM contains a high-energy sulfonium atom that can activate the nucleophilic attack reaction of adjacent carbon atoms, it has the functions of trans...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H19/167C07H1/00
Inventor 谭天伟李晓楠姚进孝孙龙王峥王杰鹏
Owner BEIJING UNIV OF CHEM TECH
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