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Purification method of high-purity pyrroloquinoline quinone disodium salt

A technology of quinoline quinone disodium salt and purification method, which is applied in the field of purification of high-purity pyrroloquinoline quinone disodium salt, can solve the problems of low column chromatography load, high column pressure, and high production cost, and achieve purity High, large sample loading, high production efficiency

Active Publication Date: 2021-03-16
SUNRESIN NEW METERIALS CO LTD XIAN +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This patented purification process has the problems of low column chromatography load and high column pressure resulting in high production costs

Method used

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  • Purification method of high-purity pyrroloquinoline quinone disodium salt
  • Purification method of high-purity pyrroloquinoline quinone disodium salt
  • Purification method of high-purity pyrroloquinoline quinone disodium salt

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Experimental program
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Effect test

Embodiment 1

[0039] Prepare the mobile phase according to the following recipe:

[0040] Mobile phase A: 10g tetrabutylammonium chloride, 0.7g phosphoric acid, dissolve in 900ml water, add sodium hydroxide to adjust pH=6.0, then dilute to 1000ml with water;

[0041] Mobile phase B: mobile phase A: methanol = 60: 40 (V / V);

[0042] Mobile phase C: mobile phase A: methanol = 30:70 (V / V);

[0043] Weigh 0.9g PQQ crude product (purity 93% attached: crude product solution HPLC detection spectrum see figure 1 ) was dissolved in 450ml of solution A, stirred to dissolve the crude product, added phosphoric acid to adjust the pH of the solution to 6.0, and the concentration of the solution detected by HPLC external standard method was 1.85mg / ml for later use. Use ultra-highly cross-linked divinylbenzene polymer microspheres (LX-316 resin produced by Xi'an Lanxiao Technology New Materials Co., Ltd.) as chromatographic fillers, fill 10 × 600mm chromatographic columns with a wet method, and pack the ...

Embodiment 2

[0045] Prepare the mobile phase according to the following recipe:

[0046]Mobile phase A: 10g sodium lauryl sulfate, 0.7g carbonic acid, dissolve in 900ml water, add sodium hydroxide to adjust pH=3.0, then dilute to 1000ml with water;

[0047] Mobile phase B: mobile phase A: ethanol = 70: 30 (V / V);

[0048] Mobile phase C: mobile phase A: ethanol = 20:80 (V / V);

[0049] Weigh 1.8g PQQ crude product (purity 93% attached: crude product solution high performance liquid phase detection collection see figure 1 ) was dissolved in 450ml of A solution, stirred to dissolve the crude product, added carbonic acid to adjust the pH of the solution to 4.0, and the concentration of the solution detected by HPLC external standard method was 3.66mg / ml for later use. Use ultra-highly cross-linked divinylbenzene polymer microspheres (LX-316 resin produced by Xi'an Lanxiao Technology New Materials Co., Ltd.) as chromatographic fillers, fill 10 × 600mm chromatographic columns with a wet method,...

Embodiment 3

[0051] Prepare the mobile phase according to the following recipe:

[0052] Mobile phase A: 10g sodium dodecylbenzenesulfonate, 0.7g acetic acid, dissolve in 900ml water, add sodium hydroxide to adjust pH=3.2, then dilute to 1000ml with water;

[0053] Mobile phase B: mobile phase A: acetone = 90:10 (V / V);

[0054] Mobile phase C: mobile phase A: acetone = 40:60 (V / V);

[0055] Weigh 2.6g PQQ crude product (purity 93% attached: crude product solution high performance liquid phase detection collection see figure 1 ) was dissolved in 450ml of solution A, stirred to dissolve the crude product, added acetic acid to adjust the pH of the solution to 3.2, and the concentration of the solution detected by HPLC external standard method was 5.37mg / ml for later use. Use ultra-highly cross-linked divinylbenzene polymer microspheres (LX-261 resin produced by Xi'an Lanxiao Technology New Materials Co., Ltd.) as chromatographic fillers, fill 10 × 600mm chromatographic columns by wet method...

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Abstract

The invention discloses a purification method of high-purity pyrroloquinoline quinone disodium salt. The purification method comprises the following steps: dissolving pyrroloquinoline quinone disodiumsalt in a buffer salt solution containing a surfactant, and carrying out chromatographic separation by using a chromatographic column taking reversed-phase polymer microspheres as a filler to obtainthe purified pyrroloquinoline quinone salt solution, and then enabling the pyrroloquinoline quinone disodium salt to be subjected to the processes of concentration, crystallization and drying to obtain pyrroloquinoline quinone disodium salt. The pyrroloquinoline quinone disodium salt purified by the purification method is high in purity, the single impurity content is less than or equal to 0.1%, and the yield is high; the resin for purification is large in adsorption capacity, long in service life, capable of being repeatedly used and suitable for large-scale production.

Description

technical field [0001] The invention belongs to the field of medicine purification, in particular, the invention relates to a purification method of high-purity pyrroloquinoline quinone disodium salt. Background technique [0002] Pyrroloquinoline quinone (PQQ) disodium salt (hereinafter simply referred to as "PQQ"), chemical name: 4,5-dioxo-4,5-dihydro-1H-pyrrolo[2,3-F ] Quinoline-2,3,9-tricarboxylic acid disodium salt. It is a new type of water-soluble vitamin and an oxidoreductase prosthetic group. It has important physiological effects on microorganisms, animals and plants: it can improve the immunity of the human body, reduce the damage of free radicals to the human body, and regulate various nervous system diseases. , Promote the absorption of amino acids, promote the synthesis of growth factors, prevent Alzheimer's disease, and promote the synthesis of glutathione, etc. Its structure is as follows: [0003] [0004] At present, pyrroloquinoline quinone (PQQ) dis...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D471/04
CPCC07D471/04
Inventor 吴丹张赪贾晓妮刘琼寇晓康
Owner SUNRESIN NEW METERIALS CO LTD XIAN