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Separation and purification method of gibberellins A7 (GA7)

A purification method and technology of gibberellin, which are applied in the field of separation and purification of gibberellin GA7, can solve the problems of low crystal purity and difficult problems of gibberellin, and achieve the advantages of improving crystal powder yield, good environmental protection conditions and expanding processing capacity. Effect

Active Publication Date: 2016-07-20
ZHEJIANG QIANJIANG BIOCHEMICAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The purity of crystals obtained from the above purification is relatively low, and currently domestic manufacturers are unable to directly produce high-purity GA 7 products, only get GA 7 with GA 4 mixture, which makes high-purity gibberellin A 7 Product becomes a bigger problem

Method used

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  • Separation and purification method of gibberellins A7 (GA7)

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Such as figure 1 As shown, weigh 1000gGA 4 / 7 solid powder (GA 4 :GA 7 =60:40), added to 20L methyl tert-butyl ether, heated to 50-60°C until completely dissolved, cooled to 0-5°C to crystallize. Suction filtration or centrifugation, obtain wet powder 897.3g (dry=627.9g), after testing (GA 4 :GA 7 =42:58), dissolved in 12.5L (MTBE) by heating at 50g / L, cooled to 0-5°C to crystallize. Suction filtration, obtain wet powder 503.5g (dry=352.5g), after testing (GA 4 :GA 7 =27:73), dissolved in 8.8L (MTBE) by heating at 40g / L, cooled to 0-5°C to crystallize. Suction filtration, obtain wet powder 187.6g (dry=131.3g), after testing (GA 4 :GA 7 =12:88), dissolved in 4.4L (MTBE) by heating at 30g / L, cooled to 0-5°C to crystallize. Suction filtration, obtain wet powder 103.8g, after testing (GA 4 :GA 7 =5:95), oven vacuum dried to obtain crystal powder 67.4g, GA 7 The content is 95.4%.

Embodiment 2

[0027] Such as figure 1 As shown, weigh 1000gGA 4 / 7 solid powder (GA 4 :GA 7 =61:39), added to 20L methyl tert-butyl ether, heated to 50-60°C until completely dissolved, cooled to 0-5°C to crystallize. Suction filtration or centrifugation, obtain wet powder 887.1g (dry=620.9g), after testing (GA 4 :GA 7 =44:56), dissolved in 12.4L (MTBE) by heating at 50g / L, cooled to 0-5°C to crystallize. Suction filtration, obtain wet powder 486.5g (dry=340.5g), after testing (GA 4 :GA 7 =28:72), dissolved in 8.5L (MTBE) by heating at 40g / L, cooled to 0-5°C to crystallize. Suction filtration, obtain wet powder 181.3g (dry=126.9g), after testing (GA 4 :GA 7 =12:88), dissolved in 4.2L (MTBE) by heating at 30g / L, cooled to 0-5°C to crystallize. Suction filtration, obtain wet powder 98.8g, after testing (GA 4 :GA 7 =6:94), oven vacuum drying to obtain crystal powder 64.4g, GA7 content is 95.1%.

Embodiment 3

[0029] Such as figure 1 As shown, weigh 1000gGA 4 / 7 solid powder (GA 4 :GA 7 =62:38), added to 20L methyl tert-butyl ether, heated to 50-60°C until completely dissolved, cooled to 0-5°C to crystallize. Suction filtration or centrifugation, obtain wet powder 887.3g (dry=621.1g), after testing (GA4:GA 7 =45:55), dissolved in 15.5L (MTBE) by heating at 40g / L, cooled to 0-5°C to crystallize. Suction filtration, obtain wet powder 390.5g (dry=273.3g), after testing (GA4:GA 7 =27:73), dissolved in 6.8L (MTBE) by heating at 40g / L, cooled to 0-5°C to crystallize. Suction filtration, obtain wet powder 160.6g (dry=112.4g), after testing (GA4:GA 7 =12:88), dissolved in 3.7L (MTBE) by heating at 30g / L, cooled to 0-5°C to crystallize. Suction filtration, obtain wet powder 85.9g, after testing (GA 4 :GA 7 =6:94), oven vacuum drying to obtain crystal powder 55.8g, GA 7 The content is 94.9%.

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Abstract

The invention provides a separation and purification method of gibberellins A7 (GA7). The method comprises the following steps: dissolving a mixture of gibberellins A4 / 7 (GA4 / 7) with methyl tertiary butyl ether (MTBE) at the ratio of GA4 / 7 to MTBE being (30-50) to 1,000 (g / L ratio); heating the solution to 50-60 DEG C for dissolving; cooling the solution to 0-5 DEG C for crystallization treatment for 6-12 hours; carrying out suction filtration or centrifugation on the crystallized solution for solid-liquid separation, wherein the separated crystal is crystal powder and the separated solution is a mother liquid; concentrating the mother liquid at 60 DEG C and in a vacuum environment, and recovering MTBE; and carrying out re-crystallization and solid-liquid separation for 3-5 times, and carrying out vacuum drying on the crystal powder at 45 DEG C for 4-5 hours to obtain a qualified product GA7. The GA7 recovery rate is high, and the products with different GA7 content can be obtained by adjusting the re-crystallization frequency; the GA4 in the first re-crystallized mother liquid is relatively high in content and can be used as a starting raw material for producing high-purity GA4; and the later crystallized mother liquids can be used as the starting raw materials of the previous step for recycling.

Description

technical field [0001] The present invention relates to a kind of purification method of plant growth regulator, particularly relate to a kind of gibberellin GA 7 separation and purification method. Background technique [0002] Gibberellin is a plant growth regulator widely used internationally and domestically, and it plays a regulating role in preserving flowers and fruits of fruits, rice and other plants. GA 7 with GA 4 It is a pair of substances with similar polarities that exist in gibberellin at the same time. During the fermentation process of gibberellin, due to the difference in medium composition and fermentation conditions, it will lead to GA 7 with GA 4 Ratio variation, but difficult to produce single-component GA 7 . Neither the traditional solvent extraction method nor the macroporous adsorption resin separation method can make GA 7 with GA 4 separate. [0003] For example, a domestic patent [Application No.: 201510864578.6] discloses a method of sepa...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/00
CPCC07D307/00
Inventor 冯偑杰祝金山陆建卫常宏
Owner ZHEJIANG QIANJIANG BIOCHEMICAL CO LTD
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