L-arginine compound crystal and preparation method thereof
An arginine and compound technology, applied in the field of medicine, can solve problems such as no solution, and achieve the effects of low bulk density, low hygroscopicity and simple process
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Embodiment 1
[0036] [Example 1] Preparation of L-arginine crystals
[0037] 1) Prepare A solution: Sterile filter 600L of a mixed solvent of absolute ethanol and acetone (the volume ratio of absolute ethanol to acetone is 5:1) into a crystallization tank, and cool down to 12°C for use, which is A solution;
[0038] 2) Preparation of solution B: Add 60kg of water for injection into the dissolving tank, control the temperature at 70°C, add 30kg of crude L-arginine, add 0.45kg of activated carbon after dissolving, stir for 30min to decolorize, filter aseptically, and use 10kg of water for injection Washing, collecting filtrate and washing liquid, obtains B solution;
[0039] 3) Add solution B to solution A, lower the temperature to 15°C, precipitate crystals, grow crystals for 2 hours, filter, wash, and vacuum dry at 45°C until the water content is less than 0.5%.
[0040] The bulk density of the obtained L-arginine compound crystal is 0.36g / cm 3 , the X-ray powder diffraction of the cryst...
Embodiment 2-9
[0041] [Example 2-9] Preparation of L-arginine crystals according to the parameters shown in Table 1
[0042] Below is embodiment 2-9, and operating procedure is with embodiment 1, and concrete process parameter is shown in table 1:
[0043] Table 1, Embodiment 2-9
[0044]
[0045] The X-ray powder diffraction patterns obtained by measuring the L-arginine compound crystals obtained in Examples 2-9 using Cu-Kα rays are similar to those in Example 1.
Embodiment 10
[0046] [Example 10] Refining L-arginine according to the method of prior art
[0047] According to "Crystalization Process of Low Bulk Density Arginine as Cephradine Co-solvent for Injection" [Liang Baochen, Chen Hui, Dong Ying. Crystallization Process of Low Bulk Density Arginine as Cephradine Co-solvent for Injection [J]. Chinese Journal of Antibiotics, 2005, 30(11):693-694], the specific steps are as follows:
[0048] 1) Add 100ml of deionized water and 50g of crude L-arginine into a 250ml three-neck flask, heat the water bath to 55°C, and stir until dissolved;
[0049] 2) Put 0.50g of activated carbon into the bottle, stir for 10min, filter with suction, and transfer the filtrate to a 500ml three-necked bottle;
[0050] 3) Adjust the stirring speed (250-400r / min), and add 95% ethanol that has been pre-cooled to 5-10°C into the arginine solution;
[0051] 4) Suction filter the crystallization feed liquid, wash, and vacuum dry at 80°C until the water content is lower than ...
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