Molecular weight grading and purifying method of polyhydroxyalkanoate

A polyhydroxyalkanoate and purification method technology, applied in the field of biomedicine, can solve the problems of complex chemical composition of polyester, wide molecular weight distribution, difficult purification and other problems, and achieve the effects of narrow molecular weight distribution, uniform and accurate molecular weight, and convenient operation.

Active Publication Date: 2021-08-24
THE SIXTH AFFILIATED HOSPITAL OF SUN YAT SEN UNIV +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The technical difficulty in obtaining polyester with high purity and narrow molecular weight distribution is that the chemical composition of polyester obtained by biological fermentation is relatively complex, the molecular weight distribution is wide, and the purification is difficult. The biggest challenge is how to obtain different Molecular Weight and Molecular Weight Distribution of PHA Molecules

Method used

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  • Molecular weight grading and purifying method of polyhydroxyalkanoate
  • Molecular weight grading and purifying method of polyhydroxyalkanoate
  • Molecular weight grading and purifying method of polyhydroxyalkanoate

Examples

Experimental program
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Embodiment 1

[0051] This embodiment provides a method for molecular weight classification and purification of polyhydroxyalkanoate, poly 3-hydroxybutyrate-co-4 hydroxybutyrate is used as raw material for molecular weight classification and purification, and its 3-hydroxybutyric acid monomer and The ratio of 4-hydroxybutyric acid monomer is (4 ~ 1): (1 ~ 4), using liquid phase permeation gel chromatography (GPC), hydrogen nuclear magnetic resonance spectrum (H-NMR) and thermogravimetry (TGA) on The purity of the poly 3-hydroxybutyrate-co-4 hydroxybutyrate obtained is characterized, and the characterization method of the specific initial poly 3-hydroxybutyrate-co-4 hydroxybutyrate in H-NMR is that 3 mg of poly-3 -Hydroxybutyric acid-co-4 hydroxybutyrate raw material is dissolved in 0.6 ~ 1mL deuterated chloroform, under the strong madness of scanning 32 ~ 64 times, there is no impurity peak in the hydrogen spectrum, indicating that the purity of the screened product is greater than 85%. Poly...

Embodiment 2

[0057] This embodiment provides a method for molecular weight classification and purification of polyhydroxyalkanoate, poly 3-hydroxybutyrate-co-4 hydroxybutyrate is used as raw material for molecular weight classification and purification, and its 3-hydroxybutyric acid monomer and The ratio of 4-hydroxybutyric acid monomer is (4 ~ 1): (1 ~ 4), using liquid phase permeation gel chromatography (GPC), hydrogen nuclear magnetic resonance spectrum (H-NMR) and thermogravimetry (TGA) on The purity of the poly 3-hydroxybutyrate-co-4 hydroxybutyrate obtained is characterized, and the characterization method of the specific initial poly 3-hydroxybutyrate-co-4 hydroxybutyrate in H-NMR is that 3 mg of poly-3 -Hydroxybutyric acid-co-4 hydroxybutyrate raw material is dissolved in 0.6 ~ 1mL deuterated chloroform, under the strong madness of scanning 32 ~ 64 times, there is no impurity peak in the hydrogen spectrum, indicating that the purity of the screened product is greater than 85%. Poly...

Embodiment 3

[0063] This embodiment analyzes the molecular weight of poly-3-hydroxybutyrate-co-4 hydroxybutyrate through molecular weight fractionation and purification in Example 1:

[0064] Take 5 mg of the poly-3-hydroxybutyrate-co-4 hydroxybutyrate and 5 mg of poly-3-hydroxybutyrate-co-4 hydroxybutyrate raw materials that have undergone molecular weight fractionation and purification in Example 1, and add 1 ml of DMF respectively to fully dissolve , placed in the liquid phase permeation gel chromatography (GPC) of DMF mobile phase to test the molecular weight of the polymer.

[0065] Analysis results such as image 3 , Curve d-P34HB corresponds to the polymer molecular weight of poly 3-hydroxybutyrate-co-4 hydroxybutyrate in Example 1 after molecular weight fractionation and purification, and curve P34HB corresponds to poly 3-hydroxybutyrate-co-4 hydroxybutyrate co-4 hydroxybutyrate base polymer molecular weight, given by image 3 It can be seen that the abscissa value corresponding ...

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Abstract

The invention relates to the field of biological medicine, in particular to a molecular weight grading and purifying method of polyhydroxyalkanoate, which comprises the following steps: S1, dissolving a polyhydroxyalkanoate raw material in a good solvent, and adding a catalyst for heating degradation; S2, cooling the solution heated and degraded in the step S1 to room temperature, conducting mixing with a poor solvent, precipitating and separating out a degradation product, and collecting the degradation product after sedimentation; and S3, centrifuging the degradation product collected in the step S2, and washing and drying the degradation product to finish molecular weight grading and purification of the polyhydroxyalkanoate. The method is simple in step and convenient to operate, molecular weight grading can be carried out on polyhydroxyalkanoate while the polyhydroxyalkanoate is purified, and the polyhydroxyalkanoate obtained after grading and purification through the method is high in purity, uniform and accurate in molecular weight and narrow in molecular weight distribution and has a higher active terminal.

Description

technical field [0001] The invention relates to the field of biomedicine, in particular to a molecular weight fractionation and purification method of polyhydroxyalkanoate. Background technique [0002] Biopolymer materials obtained by biological fermentation are one of the most rapidly developed biomedical friendly materials in recent years. Among these biological materials, polyhydroxyalkanoate (PHA) is particularly excellent because of its excellent performance. There are many reports on nerve guides made of it, cartilage-promoting materials and esophageal regeneration auxiliary functional materials, which also proves its good biological properties. Compatibility and excellent physical, chemical and mechanical properties, poly 4-hydroxybutyrate (P4HB) in the PHA family has been used as a patch for the repair of human abdominal wall defects. Compared with traditional polypropylene ( PP) patch has better biocompatibility, but the disadvantage is that it is very expensive, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/90C08J11/14C08J11/16C08L67/04
CPCC08G63/90C08J11/14C08J11/16C08J2367/04Y02W30/62
Inventor 杜杨王辉王怀明吕金艳余柳松
Owner THE SIXTH AFFILIATED HOSPITAL OF SUN YAT SEN UNIV
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