CN107860788B - Collagen fiber biomaterial heat shrinkage performance detection equipment and application - Google Patents

Collagen fiber biomaterial heat shrinkage performance detection equipment and application Download PDF

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Publication number
CN107860788B
CN107860788B CN201711056629.8A CN201711056629A CN107860788B CN 107860788 B CN107860788 B CN 107860788B CN 201711056629 A CN201711056629 A CN 201711056629A CN 107860788 B CN107860788 B CN 107860788B
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collagen fiber
beaker
detecting
temperature
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CN107860788A (en
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马克·斯拜克
许和平
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Beijing Yh Biomax Biologic Technologies Co ltd
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Beijing Yh Biomax Biologic Technologies Co ltd
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N25/00Investigating or analyzing materials by the use of thermal means
    • G01N25/16Investigating or analyzing materials by the use of thermal means by investigating thermal coefficient of expansion

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Abstract

The invention provides detection equipment for detecting the heat shrinkage performance of a collagen fiber biomaterial after crosslinking and reinforcement, which is reasonable and precise in design and is suitable for detecting the heat shrinkage performance of a protein structure of the collagen fiber biomaterial after crosslinking and reinforcement by adopting different methods. After the collagen fiber is cross-linked by different methods, the macromolecular protein structure of the collagen fiber is instantaneously shrunk and cracked at different time according to the stability degree after being heated to a certain temperature, and the instantaneously changed temperature indirectly reflects the strength of cross-linking among molecules of the collagen fiber biological material, so that different degradation resistance of the material to collagenase is expressed. The detection equipment is used for representing the heat shrinkage performance of the collagen fiber biological material, has originality, high sensitivity, small size, simple composition and convenient use, and is suitable for detecting the heat shrinkage performance of the sheet, block, column, strip and tubular collagen fiber biological material with a three-dimensional structure.

Description

Collagen fiber biomaterial heat shrinkage performance detection equipment and application
Technical Field
The invention relates to the technical fields of biomaterials, mechanical engineering and the like, in particular to collagen fiber biomaterial heat shrinkage performance detection equipment, and provides precise heat shrinkage detection equipment and an application method for collagen fiber biomaterial substances.
Background
With the rapid development of medical technology, tissue engineering and biological materials are also rapidly advanced and developed. According to clinical needs, various biomaterial products have been researched on the market to be suitable for clinical patients, and the physicochemical properties of some polymer biomaterial products cannot completely meet the requirements of clinical use, so that the materials need to be treated by some physical or chemical methods, for example, collagen fiber materials are very easily degraded by collagenase in vivo and cannot play the role of extracellular scaffolds if the collagen fiber materials are not crosslinked after being formed into products.
In order to adapt the physical, chemical and biological performance of the product to the needs of the organism, it is very important to strengthen the cross-linking of the product. Taking a biological membrane made of a collagen fiber material I as an example, collagen is homogenized, freeze-dried to form a compact three-dimensional pore structure, and then crosslinked by a physical method, single collagen peptide chains are removed by certain ions to form point-mutual combination (crosslinking) among chains, so that the biological membrane has better degradation resistance. The collagen fiber has the phenomenon that the collagen molecules in the peptide chain can be instantaneously shrunk and broken at a specific temperature in the heating process, and the temperature of the material which is heated and shrunk is the thermal shrinkage temperature of the material. The thermal shrinkage performance (temperature) of the same collagen material after being crosslinked by different methods is different, and the thermal shrinkage performance of the collagen fiber biomaterial can be detected by proper and professional precision equipment. Because no precise equipment for detecting the heat shrinkage performance of the collagen fiber biological material completely conforms to the state of China, the equipment which has high specificity and is suitable for detecting the heat shrinkage performance of the sheet, block, column, strip and tubular collagen fiber biological material with a three-dimensional structure is needed and provided.
The working principle of the equipment for detecting the thermal shrinkage performance of the collagen fiber biological material is that the molecules are instantaneously shrunk and broken when the protein molecules of a sample to be detected are heated to reach a certain temperature, and the specific temperature can represent that the material has different degrees of sensitivity to temperature shrinkage after the crosslinking reinforcement under different conditions, so that the strength of the degradation resistance of the material is indirectly reflected.
The heat shrinkage change amplifies the micro shrinkage force to the instrument panel through the instrument pointer through the pulley transmission device, so that the temperature of the sample to be measured at the moment of heat shrinkage is obtained, and the temperature indirectly indicates the degradation resistance degree of the sample to be measured in a living body.
Disclosure of Invention
The invention provides a detection device with reasonable and precise heat shrinkage performance, which is suitable for detecting the temperature of the molecular structure of a collagen fiber biological material when the molecular structure is instantaneously shrunk and broken after being heated to a certain temperature.
The invention is realized by the following technical scheme:
a collagen fiber biomaterial heat shrinkage performance detection device is characterized in that a main body is made of 304 steel materials, the length of the main body is 30-90 cm, the width of the main body is 20-45 cm, the height of the main body is 30-50 cm, and the main body structurally comprises a material preheating portion, a sample fixing portion, a mechanical conduction portion and a temperature indicating portion.
Preferably, the preheating part of the device consists of a heating power supply, a beaker and a heating chassis and is used for continuously heating the sample device to be tested, the diameter of the heating chassis is 10-30 cm, and the diameter of the beaker is matched with that of the heating chassis.
Preferably, the diameter of the fixing base with the threaded structure at the sample fixing part of the device is 2-6 cm.
Preferably, the clamp of the sample fixing part of the device is made of 304 steel, the width of the clamp is matched with the size of a sample to be detected, the clamp at one side is fixed at the bottom of the beaker with the base after clamping the sample, and the clamp at the other side is connected with the thin wire after clamping the sample.
Preferably, the beaker with the base of the sample fixing part of the device is placed on the heating plate, the required liquid is added into the beaker with the sample to be detected, the liquid is required to completely cover the top end of the sample to be detected, and the temperature of the liquid in the beaker is 20-70 ℃.
Preferably, the temperature indicator probe of the sample holding portion of the apparatus is inserted into the liquid, placed in the vicinity of the sample to be measured, and constantly detects the temperature at the instant of contraction of the sample during heating.
Preferably, pulleys of the mechanical transmission part of the equipment are made of polytetrafluoroethylene, the diameter of an inner groove is 1-2.5 cm, the diameter of an outer groove is 1.5-3.0 cm, the width of the inner groove is 1-4 mm, and the width of the outer groove is 3-7 mm; the surface smoothness grade of the pulley is better than that of No. 2D.
Preferably, the diameter of the threaded rod of the mechanical transmission part of the device is 1.5-4 cm, the length of the threaded rod is 15-25 cm, and the threaded rod is used for adjusting the horizontal height of the pulley, so that the stretching state of the sample to be tested is controlled, and the sample to be tested is kept in a natural stretching state.
Preferably, the length of a horizontal rod of the pulley of the mechanical transmission part of the equipment is 10-25 cm.
Preferably, the thin line of the mechanical conducting part of the device adopts a fishing line with the diameter of 0.1-0.4 mm to connect the pointer and the sample clamp, the fishing line is made of ultra-high molecular weight polyethylene fiber, and the micro-shrinkage state of the sample is transmitted to the pointer through the thin line to be amplified.
Preferably, the weight of the temperature indicating part of the equipment is 0.5-2.5 g, the weight is connected to the tail end of the pointer, and the length of the pointer is based on reaching the scale of the dial.
The equipment application mode is as follows: the contraction of the sample is transmitted to the top end of the pointer through a conducting wire and a pulley for magnified observation. In the testing process, use 2 fixation clamps will examine the sample and be fixed in the beaker, link to each other through conducting wire and instrument pointer, slowly add corresponding liquid in the beaker, guarantee that liquid does not too the sample top of awaiting measuring, through threaded rod adjusting pulley, make the sample that awaits measuring keep the natural state of stretching out. The sample is heated by the heating device, the micro-motion condition of the top end of the indicating needle of the instrument is observed at any time, once the pointer is micro-moved, the shrinkage reaction of the internal sub-structure of the sample to be detected is shown, and meanwhile, the temperature displayed by the instantaneous micro-motion thermometer of the indicating needle of the instrument is recorded, namely the thermal shrinkage temperature of the sample.
Description of the drawings:
FIG. 1 is a schematic structural view of the present invention;
FIG. 2 is a top view of the present invention;
Detailed Description
As shown in fig. 1, the biomaterial heat shrinkage detecting apparatus includes: heating plate 1, thermometer 2, beaker 3 with base, bracket 4, clamp 5, thin line 6, pulley 7, pulley lever 8, threaded rod 9, instrument pointer 10, weight 11, instrument 12.
The clip is with sample centre gripping after-fixing to the beaker of taking the base, fine rule one end links to each other with the clip, the other end passes through pulley and pulley lever and links to each other with the instrument pointer, place on the heating plate after adding liquid in the beaker of taking the base, the probe of thermometer passes through the support of support and places near (contactless) the sample and be used for real-time supervision sample temperature of being heated, adjusting threaded rod and weight through the weight messenger sample and weight reach balanced state, the top of instrument pointer shows certain angle on the panel board this moment, it heats to open heating power supply and carries out the continuous heating to liquid in the beaker. The dynamic state of the pointer in the dial is carefully observed and recorded, and when the pointer starts to slightly move downwards, the value of the micro-motion instantaneous thermometer is recorded, and the value is the heat shrinkage temperature of the biological material.
Example (b): detection of thermal shrinkage performance of I type collagen dura mater repair material
The device of the invention is adopted to detect the thermal shrinkage performance of the I type collagen dura mater repair material with the specification of 5mm multiplied by 10mm multiplied by 50 mm.
Get a 5mm x 10mm x 50 mm's I type collagen dura mater repair material and soak in different liquid, one end is got by the fixed clamp that has the fine rule and is got, the other end is got by the clamp and is got and be fixed in the beaker of taking the base, confirm the fine rule and walk around the pulley, and the other end links to each other with the pointer, the pointer tail end hangs the weight of certain weight, add 1L purified water in the beaker, make the liquid level not too completely at I type collagen dura mater repair material top, adjust the pulley lever height through the threaded rod, make I type collagen dura mater repair material be in the nature state of extending, the record pointer is in the calibrated scale position, place the thermometer probe near I type collagen dura mater repair material (contactless). And opening a heating power supply to enable the heating plate to continuously heat the liquid in the beaker. Carefully observing and recording the dynamic state of the pointer in the dial, and recording the numerical value of the micro-motion instant thermometer when the pointer starts to micro-motion downwards, wherein the numerical value range is between 39 and 60 ℃, and the numerical value is the heat shrinkage temperature of the I type collagen dura mater repair material.

Claims (11)

1. A device for detecting the thermal shrinkage performance of collagen fiber biomaterials is characterized in that the device is suitable for detecting the performance that the macromolecular protein structure of a material with the macromolecular protein structure of collagen fibers is instantaneously subjected to shrinkage fracture after the material is heated to a certain temperature,
the collagen fiber type biomaterial is type I collagen, and is a sheet-shaped, block-shaped, columnar, strip-shaped or tubular biomaterial with a three-dimensional structure;
the device structure comprises a material preheating part, a sample fixing part, a mechanical conduction part and a temperature indicating part:
1) the material preheating part consists of a heating device consisting of a heating power supply, a beaker and a heating chassis and is used for continuously heating the sample device to be tested;
2) the sample fixing part comprises a clamp which is positioned at the bottom of the beaker and provided with a thread structure and is fixed on a sawtooth opening sample of the base of the beaker, and the other end of the sample fixing part is provided with a clamp which is provided with a free sawtooth opening sample of the same type and provided with a thin line and is used for connecting and fixing the other side of the sample to be detected;
the width of a clamp of the sample fixing part is consistent with the size of a sample to be detected, the clamp at one side clamps the sample and then is fixed at the bottom of the beaker with the base, and the clamp at the other side clamps the sample and then is connected with the thin wire;
3) the mechanical conduction part is composed of an ultra-high molecular weight polyethylene fiber fishing line, one end of which is connected with a free fixing clamp, and a horizontal support with adjustable height and a precise conduction pulley, so that the extension state of a horizontal adjustment and conduction sample is ensured, and the far end of the conduction line is connected with an instrument pointer and is used for conducting micro-shrinkage of a material caused by temperature change, thereby causing the change of the instrument pointer on an observation instrument panel;
the mechanical conduction part is also provided with a threaded rod for adjusting the horizontal height of the pulley, so that the stretching state of the sample to be tested is controlled, and the sample to be tested is kept in a natural stretching state;
4) the temperature indicating part consists of an instrument panel and an instrument indicating needle which moves precisely, a certain volume of liquid is filled in the beaker, and the temperature indicating part is used for ensuring that a sample to be detected keeps a natural state and is heated uniformly under an infiltration state; the thermometer probe is placed near the sample to be detected so as to ensure that the temperature of the detection position is consistent with the heated temperature of the sample.
2. The apparatus for detecting thermal shrinkage performance of collagen fiber biomaterial according to claim 1, wherein the main body is made of 304 steel, and has a length of 30-90 cm, a width of 20-45 cm and a height of 30-50 cm.
3. The equipment for detecting the thermal shrinkage performance of the collagen fiber biomaterial according to claim 1, wherein the diameter of the heating base plate is 10-30 cm, and the diameter of the beaker is matched with the diameter of the heating base plate.
4. The apparatus for detecting thermal shrinkage of collagen fiber-based biomaterial according to claim 1, wherein the diameter of the fixing base of the sample fixing portion with the screw structure is 2-6 cm.
5. The apparatus for detecting thermal contraction properties of collagen fiber-based biomaterial according to claim 1, wherein the clamp of the sample fixing part is made of 304 steel.
6. The apparatus for detecting thermal shrinkage performance of collagen fiber-based biomaterial according to claim 1, wherein the pulleys of the mechanical conduction part are made of polytetrafluoroethylene, the inner groove diameter is 1-2.5 cm, the outer groove diameter is 1.5-3.0 cm, the inner groove width is 1-4 mm, and the outer groove width is 3-7 mm; the surface smoothness grade of the pulley is better than that of No. 2D.
7. The apparatus for detecting thermal shrinkage performance of collagen fiber-based biomaterial according to claim 1, wherein the threaded rod of the mechanical conduction part has a diameter of 1.5-4 cm and a length of 15-25 cm.
8. The apparatus for detecting thermal shrinkage of collagen fiber-based biomaterial according to claim 1, wherein the length of the horizontal rod of the pulley of the mechanical conduction part is 10-25 cm.
9. The apparatus for detecting thermal shrinkage performance of collagen fiber-based biomaterial according to claim 1, wherein the thin line of the mechanical conduction part is a fishing line with a diameter of 0.1-0.4 mm for connecting the pointer and the sample clamp, the fishing line is made of ultra-high molecular weight polyethylene fiber, and the micro shrinkage state of the sample is transmitted to the pointer through the thin line for amplification.
10. The apparatus for detecting thermal shrinkage of collagen fiber type biomaterial as claimed in claim 1, wherein the weight of the temperature indicating part is 0.5-2.5 g, and the weight is connected to the end of the pointer, and the length of the pointer is based on the scale of the dial.
11. The method for detecting the thermal shrinkage performance of the collagen fiber type biomaterial by using the detection device according to any one of claims 1 to 10, wherein a beaker with a base for fixing the sample is placed on a heating plate, a required liquid is added into the beaker with the sample to be detected, the liquid is required to be completely not over the top end of the sample to be detected, the temperature of the liquid in the beaker is between 20 and 70 ℃, a thermometer probe of the sample fixing part is inserted into the liquid and placed near the sample to be detected, and the temperature at the instant of the shrinkage of the sample during the heating process is detected at any time.
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CN1542438A (en) * 2003-11-08 2004-11-03 陕西科技大学 Precise determination analysis method and device for leather contraction temperature
CN2862023Y (en) * 2006-01-05 2007-01-24 中国石化仪征化纤股份有限公司 Heat shrinkage testing device for chemical fabrics filament
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