CN105175772A - Preparation method of solid-phase carrier material easy-functionalization reactive resin for polypeptide/nucleotide synthesis - Google Patents
Preparation method of solid-phase carrier material easy-functionalization reactive resin for polypeptide/nucleotide synthesis Download PDFInfo
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- CN105175772A CN105175772A CN201510687267.7A CN201510687267A CN105175772A CN 105175772 A CN105175772 A CN 105175772A CN 201510687267 A CN201510687267 A CN 201510687267A CN 105175772 A CN105175772 A CN 105175772A
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Abstract
The invention discloses a preparation method of a solid-phase carrier material easy-functionalization reactive resin for polypeptide/nucleotide synthesis, which comprises the following steps: mixing cellulose, starch and a dimethylacetamide (DMAC) solution, adding into a reaction bulb, stirring at 140 DEG C for 2 hours, transferring the reaction bulb into an 80-DEG C oil bath, adding LiCl into the reaction bulb at such temperature, stirring for 24 hours, continuing stirring at room temperature until the cellulose is completely dissolved, dropwisely adding the obtained fiber/starch DMAC/LiCl solution into ethanol to obtain pellets, immersing the cellulose pellets with ethanol many times, drying in a vacuum drying oven, extracting with hot water, washing with ethanol after 48 hours, and carrying out vacuum drying. The preparation method is simple and convenient to operate. The prepared solid-phase carrier material reactive resin for polypeptide/nucleotide synthesis can be easily functionalized.
Description
Technical field
The present invention relates to bio-pharmaceuticals solid support material technical field, the preparation method of the easy functionalized living resin of specifically one peptide species/Nucleotide synthesis solid support material.
Background technology
Along with brand-new chemical structure new drug development difficulty strengthens, Meteorological increases year by year, and the exploitation of polypeptide drug becomes the new focus of field of medicaments gradually.Micromolecule polypeptide class and nucleotide drug are strictly said and are referred to that with micromolecule polypeptide hormone and base be the general designation that the medicine produced prepared by raw material, have been found that bioactive polypeptide is thousands of, ripe product reaches more or less a hundred, in the general widespread use of American-European countries for many years, be 21 century pharmaceutical industry development and the field of cut-throat competition.
Polypeptide drug synthetic technology is complicated, and purge process is loaded down with trivial details, and starting material, carrier and processing requirement are harsh, and cause polypeptide series products price high, tempo of development is slow.Although polypeptide and Nucleotide are found there be more than 100 year so far, its real develop rapidly occurs in nearest twenty or thirty year.Along with the revolutionary character of the life science such as molecular biology and biological chemistry is in progress, especially utilize the appearance of solid-phase synthesis improvement on synthesis and nucleic acid technique, the Quality and yield of artificial synthetic polypeptide and Nucleotide is significantly improved.
Along with market is to the sharp increase of polypeptide class and nucleotide drug demand, pharmaceutical industry also creates huge demand to porous solid phase carrier necessary in production process.Develop there is different size, shape is regular, functional group is diversified and functionality much higher hole solid phase carrier is produced most important for polypeptide and Nucleotide, be directly connected to molecular weight distribution and the productive rate of the finished product, determine purity and the output of medicine further.
Mierocrystalline cellulose by D-dewater Glucopyranose acid anhydride (AGU) unit by β-Isosorbide-5-Nitrae-glycosidic link be formed by connecting (, each AGU unit, containing 3 oh groups, utilizes hydroxyl to carry out functionalized to it easily.If Mierocrystalline cellulose is prepared into porous small ball, and its surface is carried out functionalized accordingly, have broad application prospects at solid-phase synthesis improvement on synthesis and nucleic acid technique field.
Summary of the invention
The object of the present invention is to provide the preparation method of the easy functionalized living resin of one peptide species/Nucleotide synthesis solid support material, to solve the problem proposed in above-mentioned background technology.
For achieving the above object, the invention provides following technical scheme:
The preparation method of the easy functionalized living resin of one peptide species/Nucleotide synthesis solid support material, concrete operation step is as follows: Mierocrystalline cellulose, starch are mixed to join in reaction flask with the massfraction of 4:1 and N,N-DIMETHYLACETAMIDE DMAC solution by (1), and 140
o2h is stirred under C,
(2) reaction flask is transferred to 80
oin C oil bath, in this temperature downhill reaction bottle, add LiCl, after stirring 24h, continue under room temperature to stir, until Mierocrystalline cellulose dissolves completely,
(3) by the fiber obtained/starch N,N-DIMETHYLACETAMIDE DMAC/LiCl dropwise is added dropwise in ethanol, obtains bead,
(4) utilize ethanol repeatedly to soak above-mentioned cellulose pellets, vacuum drying oven is dry,
(5) extracting is carried out with hot water, with washing with alcohol after 48h, vacuum-drying.
Compared with prior art, the invention has the beneficial effects as follows: preparation method of the present invention is simple to operation, the polypeptide made/Nucleotide synthesis solid support material reactive resin can carry out functionalized to it easily.
Accompanying drawing explanation
Fig. 1 is Mierocrystalline cellulose (comprising 20Wt% starch) bead figure
The SEM image of Fig. 2 cellulose pellets
Fig. 3 comparative fibers element of the present invention bead figure.
Embodiment
Below in conjunction with the embodiment of the present invention, be clearly and completely described the technical scheme in the embodiment of the present invention, obviously, described embodiment is only the present invention's part embodiment, instead of whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art, not making the every other embodiment obtained under creative work prerequisite, belong to the scope of protection of the invention.
Embodiment
0.8g Mierocrystalline cellulose, 0.2g starch, 30ml N,N-DIMETHYLACETAMIDE DMAC solution are mixed to join in reaction flask, 140
ostir 2h under C, reaction flask is transferred to 80
oin C oil bath, add 2.0gLiCl in this temperature downhill reaction bottle, after stirring 24h, continue under room temperature to stir, until Mierocrystalline cellulose dissolves completely, by the fiber obtained/starch N,N-DIMETHYLACETAMIDE DMAC/LiCl dropwise is added dropwise in ethanol, obtains bead, (as shown in Figure 1) utilizes ethanol repeatedly to soak above-mentioned cellulose pellets, vacuum drying oven is dry, extracting is carried out with hot water, with washing with alcohol after 48h, vacuum-drying.SEM tests its microtexture, and as shown in Figure 2, a is its overall picture, and b, c are its surface, and d is its section (namely it is inner).From these pictures, bead surface is comparatively smooth, also has pore-forming place, and it is inner in cellular, and space is more, is vesicular structure.
comparative example
Keep other each component constant, same dissolution mechanism will be taked, 0.8g Mierocrystalline cellulose, 0.2g starch dissolution are contained 3.3gLiCl in 50mLDMAC/LiCl() in, this dropwise is added dropwise in ethanol, obtain bead, but bead broken (as shown in Figure 3) after stirring, illustrates when DMAc/LiCl strength of solution is lower for Mierocrystalline cellulose (comprising 20Wt% starch), cannot obtain complete cellulose pellets (comprising 20Wt% starch).
To those skilled in the art, obviously the invention is not restricted to the details of above-mentioned one exemplary embodiment, and when not deviating from spirit of the present invention or essential characteristic, the present invention can be realized in other specific forms.Therefore, no matter from which point, all should embodiment be regarded as exemplary, and be nonrestrictive, scope of the present invention is limited by claims instead of above-mentioned explanation, and all changes be therefore intended in the implication of the equivalency by dropping on claim and scope are included in the present invention.
Claims (2)
1. the preparation method of the easy functionalized living resin of one peptide species/Nucleotide synthesis solid support material, it is characterized in that, concrete operation step is as follows:
(1) Mierocrystalline cellulose, starch are mixed to join in reaction flask with the massfraction of 4:1 and N,N-DIMETHYLACETAMIDE DMAC solution, 140
o2h is stirred under C,
(2) reaction flask is transferred to 80
oin C oil bath, in this temperature downhill reaction bottle, add LiCl, after stirring 24h, continue under room temperature to stir, until Mierocrystalline cellulose dissolves completely,
(3) by the fiber obtained/starch N,N-DIMETHYLACETAMIDE DMAC/LiCl dropwise is added dropwise in ethanol, obtains bead,
(4) utilize ethanol repeatedly to soak above-mentioned cellulose pellets, vacuum drying oven is dry,
(5) extracting is carried out with hot water, with washing with alcohol after 48h, vacuum-drying.
2. the preparation method of the easy functionalized living resin of polypeptide according to claim 1/Nucleotide synthesis solid support material, is characterized in that, is mixed to join in reaction flask by 0.8g Mierocrystalline cellulose, 0.2g starch, 30ml N,N-DIMETHYLACETAMIDE DMAC solution, 140
ostir 2h under C, reaction flask is transferred to 80
oin C oil bath, add 2.0gLiCl in this temperature downhill reaction bottle, after stirring 24h, continue under room temperature to stir, until Mierocrystalline cellulose dissolves completely, by the fiber obtained/starch N,N-DIMETHYLACETAMIDE DMAC/LiCl dropwise is added dropwise in ethanol, obtains bead, utilizes ethanol repeatedly to soak above-mentioned cellulose pellets, vacuum drying oven is dry, extracting is carried out with hot water, with washing with alcohol after 48h, vacuum-drying.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201510687267.7A CN105175772A (en) | 2015-10-22 | 2015-10-22 | Preparation method of solid-phase carrier material easy-functionalization reactive resin for polypeptide/nucleotide synthesis |
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| CN201510687267.7A CN105175772A (en) | 2015-10-22 | 2015-10-22 | Preparation method of solid-phase carrier material easy-functionalization reactive resin for polypeptide/nucleotide synthesis |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1248274A (en) * | 1997-12-14 | 2000-03-22 | 纺织品和合成材料研究协会图林根研究所 | Method for producing regular porous cellulose pearls, corresponding cellulose pearls and use thereof |
| WO2004058794A1 (en) * | 2002-12-31 | 2004-07-15 | Proligo Llc | Methods and compositions for the tandem synthesis of two or more oligonuleotides on the same solid support |
| CN101591409A (en) * | 2008-05-26 | 2009-12-02 | 日东电工株式会社 | Be used for nucleic acid synthetic solid phase carrier |
| CN102143996A (en) * | 2008-10-30 | 2011-08-03 | 大卫·刘 | Micro-spherical porous biocompatible scaffolds and methods and apparatus for fabricating same |
-
2015
- 2015-10-22 CN CN201510687267.7A patent/CN105175772A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1248274A (en) * | 1997-12-14 | 2000-03-22 | 纺织品和合成材料研究协会图林根研究所 | Method for producing regular porous cellulose pearls, corresponding cellulose pearls and use thereof |
| WO2004058794A1 (en) * | 2002-12-31 | 2004-07-15 | Proligo Llc | Methods and compositions for the tandem synthesis of two or more oligonuleotides on the same solid support |
| CN101591409A (en) * | 2008-05-26 | 2009-12-02 | 日东电工株式会社 | Be used for nucleic acid synthetic solid phase carrier |
| CN102143996A (en) * | 2008-10-30 | 2011-08-03 | 大卫·刘 | Micro-spherical porous biocompatible scaffolds and methods and apparatus for fabricating same |
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Application publication date: 20151223 |
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