CN113368297A - Biomedical poly (4-hydroxybutyrate) absorbable surgical suture and preparation method thereof - Google Patents
Biomedical poly (4-hydroxybutyrate) absorbable surgical suture and preparation method thereof Download PDFInfo
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Abstract
A biomedical poly (4-hydroxybutyrate) absorbable surgical suture and a preparation method thereof. The invention belongs to the technical field of preparation of biomedical absorbable surgical sutures, and provides a method for preparing high-strength, functional and absorbable surgical sutures by using domestic independently-innovated biomedical raw materials and process technology. Solves the technical barriers that most of the biomedical materials in China depend on import and medical instrument preparation, and fundamentally breaks through foreign monopoly. The invention adopts the following raw materials: 90-95 parts of biomedical grade poly (4-hydroxybutyrate) (P4HB), 1-3 parts of nucleation inducer, 1-2 parts of natural antioxidant and 0-2 parts of chain extender. Firstly, preparing a P4HB modified material by adopting a proper process temperature and a proper shearing condition, and then preparing the surgical suture wires with different specifications by adopting a melt spinning method through secondary drawing and surface spraying coating. The invention has similar mechanical property with P4HB suture obtained by imported biological fermentation method, and has low cost, stable quality, more excellent human body compatibility and in vivo degradability.
Description
Technical Field
The invention relates to the technical field of preparation of biomedical materials, in particular to a novel bio-based poly (4-hydroxybutyrate) absorbable suture and a preparation method thereof.
Background
The surgical suture line applied clinically at present is divided into two major types, namely absorbable and non-absorbable, and the absorbable surgical suture line can provide a temporary support and a barrier for an organism, can avoid in-vivo rejection reaction, non-infectious inflammation and other adverse reactions through degradation and absorption, and simultaneously reduces the risk of secondary operation. The current absorbable polyester surgical suture material chemically synthesized in clinic includes Polyglycolide (PGA), copolymers of glycolide and caprolactone, copolymers of glycolide and lactide, Polydioxanone (PDO) and the like. The intellectual property patents and markets related to the products are mostly occupied by a few industrial countries such as the united states department of strength, the beram, germany, and the danek, australia. The absorbable suture line produced and sold in China is mainly made of catgut and collagen, the technology is relatively simple, but the problems of manufacturing process, antigenicity and high degradation rate are difficult to solve. The global surgical suture market in 2016 has a total revenue of $ 36 million, 60% absorbable sutures, and approximately 67% of absorbable suture revenue for absorbable surgical sutures, and is on the rise. However, at present, the demand of our country for absorbable surgical suture raw materials mainly depends on import, and the preparation technology of surgical sutures is difficult to solve at present. As a high-end biomedical material with rapid development, the development of technology and process with independent intellectual property rights is urgently needed to break through the monopoly abroad and realize independent innovation and industrialization.
Polyhydroxyalkanoates (PHAs) are aliphatic copolyester with different structures synthesized by microorganisms through fermentation of various carbon sources, and PHA has the characteristics of special biodegradability, gas separation, biological tissue compatibility, anticoagulation, hydrophobicity, optical isomerism and the like, and has unique advantages when being used as a high-end biomedical material to be applied to the fields of medical instruments, tissue engineering, drug carriers and the like. Poly (4-hydroxybutyrate) (P4HB) is the best comprehensive product of PHA materials, and can only be produced in small amount by microbial fermentation method from Tepha company in the United states. The new generation absorbable surgical suture prepared by taking the biological fermentation method P4HB as the raw material is approved by the United states Food and Drug Administration (FDA) to be used for clinical treatment, and compared with the common materials of the existing surgical sutures such as PGA, PLGA and PDO, the absorbable surgical suture has better biocompatibility, the degradation products are metabolized fast in vivo, and the degradation products can not cause the local high-acidity environment of tissues when degraded in vivo, so that the generation of non-bacterial tissue inflammation is avoided; meanwhile, the P4HB surgical suture has higher mechanical strength and elongation at break, better knotting (knotting) property, and higher mechanical strength in a longer time period compared with a PDO suture when the surgical suture is degraded in vivo. However, the biological fermentation method is unique in the United states, and has the defects of complex process flow, difficult purification of the obtained product, easy induction of organism immune reaction of residual biological substances and the like, so that the large-scale application of the biological fermentation method is limited.
P4HB can also be obtained by a chemical synthesis method, and has the advantages of simple process, few byproducts, high molecular weight of the synthesized product, controllable molecular weight and distribution thereof, and the like, and the used raw material gamma-butyrolactone (gamma-BL) is a common industrial solvent, and the succinic acid of the upstream product is listed first in twelve bio-based platform compounds proposed by the U.S. department of energy, and can be obtained from renewable biomass such as saccharides and the like. However, the ring-opening polymerization of five-membered ring lactones has been a major challenge in chemical synthesis, and γ -BL has long been recognized in both textbooks and literature as a non-polymerizable monomer. This is mainly because the five-membered ring structure of γ -butyrolactone and its derivatives has a small ring tension, and the enthalpy change during the ring-opening polymerization is small, plus a large entropy of polymerization, resulting in a tendency of a positive gibbs free energy during the polymerization under normal conditions. In recent years, my cooperation team of science and technology universities in Qingdao and Qingdao realizes breakthrough in the field, and the synthesis of high molecular weight poly (gamma-butyrolactone) is realized by utilizing an autonomously developed binary catalytic system, for example, the invention patent CN 107722250B, CN 109627429A has similar mechanical properties with P4HB obtained by a biological fermentation method, and provides a basis for developing a P4HB high-end absorbable surgical suture with completely independent intellectual property rights.
Disclosure of Invention
The present invention aims at overcoming the defects of the prior art and providing a novel biomedical absorbable surgical suture and a preparation method thereof. Aims to fundamentally break through foreign monopoly and realize independent innovation and industrialized application of biomedical materials.
The purpose of the invention can be realized by the following technical scheme:
a biomedical P4HB absorbable surgical suture is prepared from the following raw materials in parts by weight:
90-95 parts of biomedical grade P4HB 90, 1-3 parts of nucleating agent, 1-2 parts of antioxidant and 0-2 parts of chain extender.
The weight average molecular weight of the P4HB suitable for the invention is 10-20 ten thousand, the medical grade is, the melt index is 0.5-8, and the melting point is 58-60 ℃.
The nucleation inducing agent suitable for the invention is an absorbable material, preferably one or more of poly (3-hydroxybutyrate) (P3HB), Polyglycolide (PGA), copolymer of glycolide and caprolactone, copolymer of glycolide and lactide, Polydioxanone (PDO), starch and cellulose nanocrystal. Can effectively solve the defects of slow crystallization rate and difficult cooling and shaping of P4 HB.
The antioxidant suitable for the invention is an absorbable material, preferably one or more of vitamin C, vitamin E, licorice antioxidant, flavonoid, polysaccharide and derivatives thereof, unsaturated fatty acid, tea polyphenol, astaxanthin, lycopene and carotene.
The chain extender suitable for the invention is one or more of epoxy polymerization type chain extender, oxazoline chain extender, isocyanate chain extender and maleic anhydride grafting type chain extender. Has a key effect on maintaining the molecular weight, the melt viscosity and the strength of the polyester and the mechanical properties of the product.
The invention also provides a preparation method of the biomedical P4HB absorbable surgical suture, which comprises the following steps:
step one, weighing P4HB, a nucleation inducer, an antioxidant and a chain extender according to a formula, putting into a high-speed mixer, uniformly stirring to obtain a blend, and preparing modified P4HB by using a double-screw extruder;
and step two, spinning the modified material prepared in the step one by a melt spinning machine, and obtaining the surgical suture wires with different specifications after primary drawing, secondary heat drawing and heat setting after cooling and setting.
And step three, preparing the wire obtained in the step two into a coating by adopting a solution airless spraying method, wherein the coating film is firm in shaping, uniform in film thickness, good in smoothness and high in production efficiency.
Wherein, the processing temperature of the double-screw extruder applicable in the step one is 60-120 ℃, the rotating speed of the screw is 100-200rpm, and the screw combination selects high shear.
The processing temperature of the melt spinning extruder applicable in the second step is 80-150 ℃, the rotating speed of the screw is 20-40r/min, the rotating speed of the metering pump is 30-50r/min, the temperature of the cooling water tank is 3-10 ℃, the traction speed is 50-300r/min, the primary drawing speed ratio is 5-10 times, the secondary drawing speed ratio is 1.2-2 times, the secondary drawing temperature is 30-50 ℃, the heat setting temperature is 30-45 ℃, and the setting time is 12-36 hours.
The dye suitable for the third step is preferably alkanna tinctoria color and gallic acid, and has no toxicity, and has antibacterial, antiinflammatory and antioxidant effects.
Compared with the prior art, the invention has the beneficial effects that:
1. the material and the formula are optimized, and the raw materials have independent intellectual property rights, so that the foreign monopoly is broken. P4HB has good physical and chemical properties, biocompatibility and biodegradability. The degradation rate is slow (8-52 weeks), and the degradation is mainly surface degradation, so that the mechanical properties of the material can be maintained to the maximum extent.
2. The raw materials are produced by adopting the nonmetal alkaline catalyst with independent intellectual property rights, and the method has the advantages of no metal residue, easy removal of the catalyst and the like. The polymer has narrow distribution and uniform performance, can meet the spinning requirement and can realize industrialized production.
3. The surgical suture in the invention is of a monofilament structure, and the coating is additionally arranged, so that the surface of the suture is lubricated, the wound on tissue cells is small, and the firm connection of needles and threads is facilitated. The monofilament structure and the coating not only delay degradation and control absorption period, but also avoid inhabitation of foreign matters and bacteria.
4. The novel coating design creates preferable gromwell color, gallic acid and the like at home and abroad, belongs to additive dyes for traditional Chinese medicines and foods, and has no toxicity, sterilization, anti-inflammation and antioxidation effects.
In general, the research and development and production of the biomedical absorbable surgical suture prepared by adopting P4HB at home are not reported at present, so that the invention can fill the blank of preparing the absorbable surgical suture by adopting P4HB in China, and has very important promotion effect on the independent innovation of biomedical materials in China.
Drawings
FIG. 1 illustrates poly (4-hydroxybutyrate) absorbable surgical suture products of varying sizes.
Detailed Description
The following examples are given to illustrate the present invention in more detail, and it should be noted that the following examples are not to be construed as limiting the scope of the present invention, and that the skilled person in the art may make modifications and adaptations of the present invention in accordance with the above disclosure without departing from the essential scope thereof.
Example 1
A biomedical P4HB absorbable surgical suture is prepared from the following raw materials in parts by weight:
96 parts of biomedical grade P4HB (molecular weight is 15.8 ten thousand, and melt index is 2.5), 1.5 parts of P3HB 1.5, 2 parts of VC and 44680.5 parts of epoxy polymerization type chain extender ADR-44680.5.
The preparation method of the absorbable surgical suture line P4HB comprises the following steps:
step one, weighing P4HB, P3HB, ADR-4468 and VC according to a formula, putting into a high-speed mixer, stirring and blending uniformly to obtain a blend, and preparing modified P4HB by using a double-screw extruder. The processing temperature of the double-screw extruder is 80 ℃, 100 ℃, 120 ℃, 100 ℃, the rotating speed of the screw is 150rpm, the high shear is selected by the combination of the screws, and the cooling water temperature is 7 ℃.
And step two, adding the modified P4HB particles into melt spinning, wherein the processing temperature is 80 ℃, 100 ℃, 120 ℃, 150 ℃, the screw rotation speed is 30rpm, the cooling water temperature is 3 ℃, the metering pump rotation speed is 60r/min, the traction speed is 100r/min, the primary drawing speed ratio is 5 times, the secondary drawing speed ratio is 1.2 times, the secondary drawing temperature is 35 ℃, the heat setting temperature is 40 ℃, and the setting time is 12 hours. The diameter of the prepared surgical suture is 0.33mm, and the prepared surgical suture belongs to the specification of 3-0.
And step three, preparing the wire obtained in the step two into a coating by adopting a gallic acid solution airless spraying method, so that the surface of the suture is lubricated, the wound on tissue cells is small, and the firm connection of the needle and the thread is facilitated.
Example 2
A biomedical P4HB absorbable surgical suture is prepared from the following raw materials in parts by weight:
96 parts of biomedical grade P4HB (molecular weight is 15.8 ten thousand, melt index is 2.5), 1 part of PDO, 2 parts of VE and ADR-44681 parts of epoxy polymerization type chain extender.
The preparation method of the absorbable surgical suture line P4HB comprises the following steps:
step one, weighing P4HB, PDO, ADR-4468 and VE according to a formula, putting the weighed materials into a high-speed mixer, stirring and blending the materials uniformly to obtain a blend, and preparing modified P4HB by using a double-screw extruder. The processing temperature of the double-screw extruder is 80 ℃, 100 ℃, 120 ℃, 130 ℃ and 120 ℃, the rotating speed of the screw is 150rpm, the high shear is selected by the combination of the screws, and the cooling water temperature is 7 ℃.
And step two, adding the modified P4HB particles into melt spinning, wherein the processing temperature is 80 ℃, 100 ℃, 120 ℃, 150 ℃, the screw rotation speed is 30rpm, the cooling water temperature is 3 ℃, the metering pump rotation speed is 60r/min, the traction speed is 150r/min, the primary drawing speed ratio is 6 times, the secondary drawing speed ratio is 1.2 times, the secondary drawing temperature is 40 ℃, the heat setting temperature is 40 ℃, and the setting time is 12 hours. The diameter of the prepared surgical suture is 0.22mm, and the prepared surgical suture belongs to the specification of 4-0.
And step three, preparing the wire obtained in the step two into a coating by adopting a gallic acid solution airless spraying method, so that the surface of the suture is lubricated, the wound on tissue cells is small, and the firm connection of the needle and the thread is facilitated.
Example 3
A biomedical P4HB absorbable surgical suture is prepared from the following raw materials in parts by weight:
96.5 parts of biomedical grade P4HB (molecular weight is 15.8 ten thousand, and melt index is 2.5), 1 part of cellulose nanocrystal, 2 parts of carotene and 0.5 part of maleic anhydride.
The preparation method of the absorbable surgical suture line P4HB comprises the following steps:
step one, weighing P4HB, cellulose nanocrystalline, carotene and maleic anhydride according to a formula, putting into a high-speed mixer, stirring and blending uniformly to obtain a blend, and preparing modified P4HB by using a double-screw extruder. The processing temperature of the double-screw extruder is 80 ℃, 100 ℃, 120 ℃, 100 ℃, the rotating speed of the screw is 150rpm, the high shear is selected by the combination of the screws, and the cooling water temperature is 7 ℃.
And step two, adding the modified P4HB particles into melt spinning, wherein the processing temperature is 80 ℃, 100 ℃, 120 ℃, 150 ℃, the screw rotation speed is 30rpm, the cooling water temperature is 3 ℃, the metering pump rotation speed is 40r/min, the traction speed is 100r/min, the primary drawing speed ratio is 5 times, the secondary drawing speed ratio is 1.5 times, the secondary drawing temperature is 40 ℃, and the setting time is 12 hours. . The diameter of the prepared surgical suture is 0.16mm, and the prepared surgical suture belongs to the specification of 5-0.
And step three, preparing the wire obtained in the step two into a coating by adopting a gallic acid solution airless spraying method, so that the surface of the suture is lubricated, the wound on tissue cells is small, and the firm connection of the needle and the thread is facilitated.
Example 4
A biomedical P4HB absorbable surgical suture is prepared from the following raw materials in parts by weight:
96 parts of biomedical grade P4HB (molecular weight is 15.8 ten thousand, and melt index is 2.5), 1.5 parts of PGA, 2 parts of astaxanthin and 0.5 part of maleic anhydride.
The preparation method of the absorbable surgical suture line P4HB comprises the following steps:
step one, weighing P4HB, PGA, astaxanthin and maleic anhydride according to a formula, putting into a high-speed mixer, stirring and blending uniformly to obtain a blend, and preparing modified P4HB by using a double-screw extruder. The processing temperature of the double-screw extruder is 80 ℃, 100 ℃, 120 ℃, 130 ℃ and 120 ℃, the rotating speed of the screw is 150rpm, the high shear is selected by the combination of the screws, and the cooling water temperature is 7 ℃.
And step two, adding the modified P4HB particles into melt spinning, wherein the processing temperature is 80 ℃, 100 ℃, 120 ℃, 150 ℃, the screw rotation speed is 30rpm, the cooling water temperature is 3 ℃, the metering pump rotation speed is 40r/min, the traction speed is 200r/min, the primary drawing speed ratio is 7 times, the secondary drawing speed ratio is 1.2 times, the secondary drawing temperature is 40 ℃, the heat setting temperature is 40 ℃, and the setting time is 12 hours. The diameter of the prepared surgical suture is 0.14mm, and the prepared surgical suture belongs to the specification of 6-0.
And step three, preparing the wire obtained in the step two into a coating by adopting a gallic acid solution airless spraying method, so that the surface of the suture is lubricated, the wound on tissue cells is small, and the firm connection of the needle and the thread is facilitated.
TABLE 1 Performance parameters of absorbable surgical sutures prepared in examples 1-4
Remarking: comparative example is an inlet
The study product.
Claims (6)
1. A biomedical poly (4-hydroxybutyrate) (P4HB) absorbable surgical suture is mainly prepared from the following raw materials in parts by weight: 90-95 parts of biomedical grade P4HB 90, 1-3 parts of nucleation inducer, 1-2 parts of antioxidant and 0-2 parts of chain extender.
2. The biomedical P4HB absorbable surgical suture of claim 1, wherein: the weight average molecular weight of the P4HB is 10-20 ten thousand, the weight average molecular weight is medical grade, the melt index is 0.5-8, and the melting point is 58-60 ℃.
3. The biomedical P4HB absorbable surgical suture of claim 1, wherein: the nucleation inducer should be absorbable material, preferably one or more of poly (3-hydroxybutyrate) (P3HB), Polyglycolide (PGA), copolymer of glycolide and caprolactone, copolymer of glycolide and lactide, Polydioxanone (PDO), starch, and cellulose nanocrystal.
4. The biomedical P4HB absorbable surgical suture of claim 1, wherein: the antioxidant is absorbable material, preferably one or more of vitamin C, vitamin E, Glycyrrhrizae radix antioxidant, flavonoids, polysaccharide and its derivatives, unsaturated fatty acid, tea polyphenols, astaxanthin, lycopene, and carotene.
5. The biomedical P4HB absorbable surgical suture of claim 1, wherein: the chain extender is one or more of epoxy polymerization type chain extender, oxazoline chain extender, isocyanate chain extender and maleic anhydride grafting type chain extender.
6. The method for preparing the biomedical P4HB absorbable surgical suture according to claim 1 comprises the following steps:
step one, weighing P4HB, a nucleation inducer, an antioxidant and a chain extender according to a formula, putting into a high-speed mixer, uniformly stirring to obtain a blend, and preparing modified P4HB by using a double-screw extruder;
and step two, spinning the modified material prepared in the step one by a melt spinning machine, and obtaining the surgical suture wires with different specifications after primary drawing, secondary heat drawing and heat setting after cooling and setting.
And step three, preparing the wire obtained in the step two into a coating by adopting a solution airless spraying method, wherein the coating film is firm in shaping, uniform in film thickness, good in smoothness and high in production efficiency.
Preferably, in the step one, the processing temperature of the double-screw extruder is 60-120 ℃, the screw rotating speed is 100-200rpm, and the screw combination selects high shear.
Preferably, in the second step, the processing temperature of the melt spinning extruder is 80-150 ℃, the rotating speed of a screw is 20-40r/min, the rotating speed of a metering pump is 30-50r/min, the temperature of a cooling water tank is 3-10 ℃, the traction speed is 50-300r/min, the primary drawing speed ratio is 5-10 times, the secondary drawing speed ratio is 1.2-2 times, the secondary drawing temperature is 30-50 ℃, the heat setting temperature is 30-45 ℃, and the setting time is 12-36 hours.
Preferably, the dyes used in step three are alkannin and gallic acid, which have no toxicity, and have the effects of sterilization, inflammation diminishing and oxidation resistance.
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| CN202110709335.0A Pending CN113368297A (en) | 2021-06-25 | 2021-06-25 | Biomedical poly (4-hydroxybutyrate) absorbable surgical suture and preparation method thereof |
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| US4024871A (en) * | 1975-07-23 | 1977-05-24 | Ethicon, Inc. | Antimicrobial sutures |
| US20160045636A1 (en) * | 2014-08-15 | 2016-02-18 | Tepha, Inc. | Self-retaining sutures of poly-4-hydroxybutyrate and copolymers thereof |
| CN111961322A (en) * | 2020-08-21 | 2020-11-20 | 青岛科技大学 | Poly (4-hydroxybutyrate) biodegradable packaging film and preparation method thereof |
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| US4024871A (en) * | 1975-07-23 | 1977-05-24 | Ethicon, Inc. | Antimicrobial sutures |
| US20160045636A1 (en) * | 2014-08-15 | 2016-02-18 | Tepha, Inc. | Self-retaining sutures of poly-4-hydroxybutyrate and copolymers thereof |
| CN111961322A (en) * | 2020-08-21 | 2020-11-20 | 青岛科技大学 | Poly (4-hydroxybutyrate) biodegradable packaging film and preparation method thereof |
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