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A method for purifying vitamin B2
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A vitamin and 2SO4 technology, which is applied in the field of separation and purification, can solve the problems of low purity of vitamin B2 and achieve the effects of avoiding sample loss, high separation efficiency and large preparation volume
Active Publication Date: 2021-03-23
BEIJING HARMONY HEALTH MEDICAL DIAGNOSTICS CO LTD +1
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Problems solved by technology
[0004] At present, the production methods of vitamin B2 mainly include plant extraction, chemical synthesis, microbial fermentation and semi-microbial fermentation. The extraction methods mainly include heavy metal salt precipitation, acid dissolution, alkali dissolution, etc. However, the above-mentioned The purity of vitamin B2 obtained by the method is low (<98%)
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Embodiment 1
[0033] Butanol, acetonitrile, 50% (NH4) 2 SO 4 , Water is configured into a two-phase solvent system ((NH4) according to the volume ratio of 3:1:2.4:2 2 SO 4 The concentration is 50%), placed in a separatory funnel, shake well, after standing for stratification, divided into upper phase stationary phase and lower phase mobile phase, ultrasonic degassing 10min before use, remove air bubbles for later use.
[0034] Take 100 mg of vitamin B2 with a purity of 90% from Shanghai Yuanye Biotechnology Co., Ltd., and dissolve the sample with 10 ml of the lower phase and 10 ml of the upper phase.
[0035] Pump the upper phase that has been ultrasonically degassed in the two-phase solvent system into the separation tube of the high-speed countercurrent chromatograph at a speed of 20ml / min until the upper phase flows out to ensure that the stationary phase fills the entire separation spiral tube, and then adjust the speed of the host to 850rpm, the helical column of the chromatographic...
Embodiment 2
[0041] Butanol, acetonitrile, 40% (NH4) 2 SO 4 , Water is configured into a two-phase solvent system according to the volume ratio of 3.5:0.8:2:2.5, placed in a separatory funnel, shaken well, after standing for stratification, it is divided into an upper phase stationary phase and a lower phase mobile phase, before use Ultrasonic degassing for 12 minutes, remove air bubbles and set aside.
[0042] Take 100 mg of vitamin B2 with a purity of 90% (same as the sample in Example 1) sold by Shanghai Yuanye Biotechnology Co., Ltd., and dissolve the sample with 10 ml of the lower phase and 10 ml of the upper phase.
[0043] Pump the upper phase that has been ultrasonically degassed in the two-phase solvent system into the separation tube of the high-speed countercurrent chromatograph at a speed of 20ml / min until the upper phase flows out to ensure that the stationary phase fills the entire separation spiral tube, and then adjust the speed of the host to 850rpm, the helical column o...
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Abstract
The invention relates to a method for rapidly purifying vitamin B2, which comprises the following steps: a step of mixing n-butyl alcohol, acetonitrile, (NH4)2SO4 and water to obtain a two-phase solvent system, and performing separation to obtain an upper-phase stationary phase and a lower-phase mobile phase after the solvent system is layered; a step of respectively dissolving a sample by using the upper-phase stationary phase and the lower-phase mobile phase to respectively obtain an upper-phase liquid and a lower-phase liquid; a step of introducing the obtained upper-phase liquid and the lower-phase liquid into a high-speed counter-current chromatograph, namely a step of injecting the obtained upper-phase liquid into a separation tube of the high-speed counter-current chromatograph, then injecting the lower-phase liquid, monitoring the dissolved solution in the separation tube by using the high-speed counter-current chromatograph, collecting fractions, and combining the same components to obtain a purified product. The purity of the vitamin B2 in the purified product is greater than 98%.
Description
technical field [0001] The invention belongs to the technical field of separation and purification, and in particular relates to a method for quickly purifying vitamin B2. Background technique [0002] The information disclosed in this background section is only intended to increase the understanding of the general background of the present invention, and is not necessarily taken as an acknowledgment or any form of suggestion that the information constitutes the prior art already known to those skilled in the art. [0003] Vitamin B2, also known as riboflavin, is a component of the prosthetic group of flavin enzymes in the body (flavor enzymes play the role of hydrogen transfer in biological redox). When lacking, it will affect the biological oxidation of the body and cause metabolic disorders. The lesions are often manifested as inflammation of the mouth, eyes and external genitalia, such as angular cheilitis, cheilitis, glossitis, conjunctivitis and scrotal inflammation, s...
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Patent Type & Authority Patents(China)
IPC IPC(8): C07D475/14
CPCC07D475/14
Inventor 段文娟翟瑞雪倪君君王晓李月董红敬马天宇
Owner BEIJING HARMONY HEALTH MEDICAL DIAGNOSTICS CO LTD
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