CN112147029A - Method for measuring swelling degree of cross-linked sodium hyaluronate gel - Google Patents
Method for measuring swelling degree of cross-linked sodium hyaluronate gel Download PDFInfo
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Abstract
The invention provides a method for measuring swelling degree of cross-linked sodium hyaluronate gel. According to the method for measuring the swelling degree of the cross-linked sodium hyaluronate gel, provided by the invention, through the use of the screen and the filter paper, the swelling time and the reagent addition amount are optimized, the influence of factors such as product character difference and artificial difference on experimental operation is reduced, and a calculation result with high accuracy and good reproducibility is obtained.
Description
Technical Field
The invention particularly relates to a method for measuring swelling degree of cross-linked sodium hyaluronate gel.
Background
Swelling refers to the phenomenon of a gel that absorbs liquid and then significantly increases its volume, which is an important characteristic of an elastic gel. The swelling degree is an important physical parameter for representing the hydrophilic property of the hydrogel. The water content of the crosslinked sodium hyaluronate saturated hydrogel is in positive correlation with the size of the three-dimensional grid of the crosslinked sodium hyaluronate. Therefore, the swelling degree is a quantitative index for evaluating the structure of the crosslinked sodium hyaluronate gel. The method for calculating the swelling degree of the cross-linked sodium hyaluronate in the existing industry standard YY/T0962-2014 has a large subjective influence due to factors such as different product character differences and the like in the step of removing excessive water. Experimental results show that the calculation result of the swelling degree is inaccurate.
Disclosure of Invention
The invention aims to provide a method for measuring the swelling degree of a cross-linked sodium hyaluronate gel, which has the advantages of high measurement accuracy, small artificial subjective error and good reproducibility. The technical scheme adopted by the invention comprises the following steps:
a method for measuring swelling degree of cross-linked sodium hyaluronate gel is characterized by comprising the following steps:
the method comprises the following steps: placing 500 mesh screen into drying oven, weighing at 80 deg.C to constant weight, and recording as m0；
Step two: weighing a crosslinked sodium hyaluronate gel sample, placing the crosslinked sodium hyaluronate gel sample on a 500-mesh sieve, placing the sieve in an evaporation dish, and adding a certain amount of sodium chloride solution to completely infiltrate the sample;
step three: swelling for a certain time, taking out the screen after the swelling is completely expanded, sucking the liquid around the screen by using filter paper, weighing the total mass of the sample and the screen, and recording the total mass as m1；
Step four: placing the screen in a drying oven, weighing the total mass of the sample and the screen after the weight is constant at 80 ℃, and recording the total mass as m2；
Step five: and (4) calculating a result: swelling degree (Q) ═ m1-m2)/(m2-m0)。
Preferably, in the step one, two screens with 500 meshes are parallelly taken and put into a drying oven, and the screens are respectively weighed after reaching the constant weight at the temperature of 80 ℃ and are respectively recorded as m0(ii) a Wherein, the parallel taking of the two screens refers to cutting two screens with 500 meshes in the same block or batch of screens with 500 meshes;
in the second step, two cross-linked sodium hyaluronate gel samples are weighed in parallel and respectively placed on the two 500-mesh sieves, the sieves are placed in an evaporation dish, and a certain amount of 0.9% sodium chloride solution is added to completely soak the samples; wherein the parallel weighing refers to randomly weighing two samples with the same mass in the same batch of the cross-linked sodium hyaluronate gel;
in the third step: swelling for a certain time, taking out the screen after the swelling is completely expanded, sucking the liquid around the screen by using filter paper, and respectively weighing the total mass of each group of samples and the total mass of the screen, and recording the total mass as m1；
In the fourth step: putting the screen mesh into the dryerIn a drying oven, after reaching a constant weight at 80 ℃, the total mass of each group of samples and the screen is weighed and recorded as m2；
In the fifth step: the swelling degree (Q) ═ m (m) of each sample was calculated1-m2)/(m2-m0) And taking the average value as the swelling degree measurement result.
Preferably, the mass of each sample in step one is 0.25-0.35 g, and 0.9% sodium chloride solution is preferably used in step two, and the addition amount is preferably 20-40 mL.
Preferably, the swelling time in step three is 20-40 min.
Compared with the prior art, the invention has the following beneficial effects:
the invention improves the analysis method on the calculation method of the swelling degree of the cross-linked sodium hyaluronate gel in the existing industry standard YY/T0962-2014. The conventional standard swelling capacity measuring method comprises placing about 0.2g of crosslinked sodium hyaluronate gel on two culture dishes, placing the two culture dishes in a drying oven, weighing at 80 deg.C until constant weight, and recording as m1. Dropping water until swelling, removing excessive water, weighing, and recording as m2. Swelling degree (Q) ═ m2-m1)/m1. The existing standard method has no regulation on the water adding amount and the swelling time, and the water adding amount and the swelling time influence the swelling degree result. And finally, the step of removing the excessive water causes poor repeatability of the calculation result of the swelling degree due to factors such as different product character differences, manual operation differences and the like. The method selects 0.9 percent sodium chloride solution as a swelling medium of the cross-linked sodium hyaluronate, fully considers the preparation of the cross-linked sodium hyaluronate gel as physiological balanced salt, and eliminates the expansion influence caused by the difference of internal and external osmotic pressures of the sample. Through the use of a screen and filter paper, the swelling time and the preferable determination of the addition amount of 0.9 percent sodium chloride solution reduce the influence of factors such as product character difference, artificial difference and the like on experimental operation. Compared with the measurement results of the existing standard method and the method of the invention, and the comparison of the measurement results of different analysts shows that the swelling degree of the crosslinked sodium hyaluronate gel measured by the method of the invention is more excellent than that measured by the standard method. The method of the invention is accurateHigh degree, good reproducibility, small artificial subjective error and simple operation.
Detailed Description
The following invention is further illustrated with reference to examples in order to better illustrate the procedures and protocols of the present invention. The specific examples described herein are intended to be illustrative only and are not intended to be limiting.
Firstly, the method comprises the following steps: cross-linked sodium hyaluronate gel swelling degree determination process
Example 1
Two 500-mesh sieves are parallelly placed in a drying oven, weighed respectively after reaching constant weight at 80 ℃, and respectively recorded as m0. Approximately 0.2g of crosslinked sodium hyaluronate gel was weighed in parallel and placed on two 500 mesh sieves, respectively, the sieves were placed in an evaporation dish, and 40ml of 0.9% sodium chloride solution was added to completely infiltrate the sample. After swelling for 40min, the screen was removed, the liquid around the screen was removed by suction with filter paper, and the total mass of each set of samples and screen was weighed separately and recorded as m1. Then, the sieve was placed in a drying oven at 80 ℃ until the weight became constant, and the total mass of each set of the sample and the sieve was measured and recorded as m2. The swelling degree (Q) ═ m (m) of each sample was calculated1-m2)/(m2-m0) Then, the average value thereof was taken as the measurement result.
Example 2
Two 500-mesh sieves are parallelly placed in a drying oven, weighed respectively after reaching constant weight at 80 ℃, and recorded as m0. Approximately 0.2g of crosslinked sodium hyaluronate gel was weighed in parallel onto two 500 mesh sieves, placed in an evaporation dish and allowed to completely infiltrate the sample by adding 20ml of 0.9% sodium chloride solution. After swelling for 40min, the screen was taken out, the liquid around the screen was removed by suction with filter paper, and the total mass of each set of samples and screen was weighed separately and recorded as m1. Then, the sieve is put into a drying oven, the total mass of each group of samples and the sieve is weighed after the temperature is 80 ℃ to constant weight and is recorded as m2. The swelling degree (Q) ═ m (m) of each sample was calculated1-m2)/(m2-m0) Then, the average value thereof was taken as the measurement result.
Example 3
Two 500-mesh sieves are parallelly placed in a drying oven, weighed respectively after reaching constant weight at 80 ℃, and recorded as m0. Approximately 0.2g of crosslinked sodium hyaluronate gel was weighed in parallel onto two 500 mesh sieves, placed in an evaporation dish and allowed to completely infiltrate the sample by adding 20ml of 0.9% sodium chloride solution. After swelling for 20min, the screen was taken out, the liquid around the screen was removed by suction with filter paper, and the total mass of each set of samples and screen was weighed separately and recorded as m1. Then, the sieve is put into a drying oven, the total mass of each group of samples and the sieve is weighed after the temperature is 80 ℃ to constant weight and is recorded as m2. The swelling degree (Q) ═ m (m) of each sample was calculated1-m2)/(m2-m0) Then, the average value thereof was taken as the measurement result.
Example 4
Two 500-mesh sieves are parallelly placed in a drying oven, weighed respectively after reaching constant weight at 80 ℃, and recorded as m0. Approximately 0.2g of crosslinked sodium hyaluronate gel was weighed in parallel onto two 500 mesh sieves, placed in an evaporation dish and 30ml of 0.9% sodium chloride solution was added to completely infiltrate the sample. After swelling for 20min, the screen was taken out, the liquid around the screen was removed by suction with filter paper, and the total mass of each set of samples and screen was weighed separately and recorded as m1. Then, the sieve is put into a drying oven, the total mass of each group of samples and the sieve is weighed after the temperature is 80 ℃ to constant weight and is recorded as m2. The swelling degree (Q) ═ m (m) of each sample was calculated1-m2)/(m2-m0) Then, the average value thereof was taken as the measurement result.
Example 5
Two 500-mesh sieves are parallelly placed in a drying oven, weighed respectively after reaching constant weight at 80 ℃, and recorded as m0. Approximately 0.2g of crosslinked sodium hyaluronate gel was weighed in parallel onto two 500 mesh sieves, placed in an evaporation dish and 30ml of 0.9% sodium chloride solution was added to completely infiltrate the sample. After swelling for 30min, the screen was taken out, the liquid around the screen was removed by suction with filter paper, and the total mass of each set of samples and screen was weighed separately and recorded as m1. Then, the screen was placed in a drying oven at 80 deg.CWeighing the total mass of each group of samples and the screen after the weight is constant, and recording the total mass as m2. The swelling degree (Q) ═ m (m) of each sample was calculated1-m2)/(m2-m0) Then, the average value thereof was taken as the measurement result.
II, secondly: measurement result of swelling degree of crosslinked sodium hyaluronate gel
Table 1: results of swelling measurement of various examples
And (4) conclusion: the same samples were used, and the same person conducted the same procedures as in examples 1 to 5 above, and the measurement results are shown in Table 1. In the method, the addition amount of 0.9 percent sodium chloride solution is between 20 and 40mL, the swelling time is between 20 and 40min, the relative deviation of the swelling degree measurement result is small, the result is accurate, and the method has wide application range.
Table 2: comparison of swelling degree method of industry standard YY/T0962-
And (4) conclusion: the crosslinked sodium hyaluronate gel was subjected to 3 measurements (two parallel samples per measurement) according to the method described in example 5 and the bar method, and the results are shown in Table 2, where the RSD of the method of the present invention is much lower than that of the bar method. The line marking method has poor reproducibility and is easily influenced by other factors. The method can effectively avoid the defect, and has the advantages of high accuracy of the measured result, small error and good repeatability.
Table 3: results of swelling measurement according to example 5 (results of two measurements in parallel)
And (4) conclusion: the results of the swelling degree measurement of the same sample by different analysts in accordance with example 5 are shown in table 3. The method has the advantages of small human error, high accuracy and good repeatability.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and any modification, improvement, etc. made within the spirit and principle of the present invention are within the protection scope of the present invention.
Claims (4)
1. A method for measuring swelling degree of cross-linked sodium hyaluronate gel is characterized by comprising the following steps:
the method comprises the following steps: placing 500 mesh screen into drying oven, weighing at 80 deg.C to constant weight, and recording as m0；
Step two: weighing a crosslinked sodium hyaluronate gel sample, placing the crosslinked sodium hyaluronate gel sample on a 500-mesh sieve, placing the sieve in an evaporation dish, and adding a certain amount of 0.9% sodium chloride solution to completely infiltrate the sample;
step three: swelling for a certain time, taking out the screen after the swelling is completely expanded, sucking the liquid around the screen by using filter paper, weighing the total mass of the sample and the screen, and weighing the total mass as m1；
Step four: placing the screen in a drying oven, weighing the total mass of the sample and the screen after the weight is constant at 80 ℃, and recording the total mass as m2；
Step five: and (4) calculating a result: swelling degree (Q) ═ m1-m2)/(m2-m0)。
2. The method for measuring the swelling capacity of the crosslinked sodium hyaluronate gel according to claim 1, wherein: in the first step, two 500-mesh sieves are parallelly placed in a drying oven, weighed respectively after reaching constant weight at 80 ℃, and respectively recorded as m0；
In the second step, two cross-linked sodium hyaluronate gel samples with the same mass are weighed in parallel and respectively placed on the two 500-mesh sieves, the sieves are placed in an evaporation dish, and a certain amount of 0.9% sodium chloride solution is added to completely soak the samples;
in the third step: swelling for a certain time, taking out the screen after the swelling is completely expanded, sucking the liquid around the screen by using filter paper, and respectively weighing the total mass of each group of samples and the total mass of the screen, and recording the total mass as m1；
In the fourth step: placing the screen in a drying oven, weighing the total mass of each group of samples and the screen after the weight of the samples is constant at 80 ℃, and recording the total mass as m2；
In the fifth step: the swelling degree (Q) ═ m (m) of each sample was calculated1-m2)/(m2-m0) And taking the average value as the swelling degree measurement result.
3. The method for measuring the swelling capacity of the crosslinked sodium hyaluronate gel according to claim 1 or 2, which comprises the following steps: in the first step, the mass of each sample is preferably 0.25-0.35 g, and the addition amount of the 0.9% sodium chloride solution in the second step is preferably 20-40 mL.
4. The method for measuring the swelling capacity of the crosslinked sodium hyaluronate gel according to claim 1 or 2, which comprises the following steps: the swelling time in the third step is preferably 20-40 min.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116124754A (en) * | 2023-04-17 | 2023-05-16 | 山东省中源联科生物工程集团有限公司 | Method for detecting residual quantity of cross-linking agent in sodium hyaluronate gel through image analysis |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5057574A (en) * | 1984-12-28 | 1991-10-15 | Mitsubishi Rayon Company, Ltd. | Process for producing an α-alkyl-substituted aromatic vinyl copolymer and a thermoplastic resin composition comprising the copolymer |
| EP0608949A1 (en) * | 1993-01-25 | 1994-08-03 | Shell Internationale Researchmaatschappij B.V. | Process for the preparation of moisture resistant vegetable fibres |
| US5496890A (en) * | 1994-03-03 | 1996-03-05 | Bayer Aktiengesellschaft | Super-absorbent polymers |
| US20150328123A1 (en) * | 2012-09-29 | 2015-11-19 | Hangzhou Gallop Biological Products Co., Ltd. | Cross-linked sodium hyaluronate gel for tissue filler for plastic surgery and preparation method thereof |
| US20160145357A1 (en) * | 2013-06-28 | 2016-05-26 | Galderma S.A. | Method for manufacturing a shaped crosslinked hyaluronic acid product |
| WO2016167229A1 (en) * | 2015-04-15 | 2016-10-20 | キユーピー 株式会社 | Cross-linked product of carboxymethyl group-containing modified hyaluronic acid and/or salt of same, and method for producing same |
| CN108774329A (en) * | 2018-06-13 | 2018-11-09 | 浙江景嘉医疗科技有限公司 | A kind of preparation method of medical cross-linking sodium hyaluronate gel |
| US20190062461A1 (en) * | 2013-06-28 | 2019-02-28 | Galderma S.A. | Process for preparing a cross-linked hyaluronic acid product |
-
2019
- 2019-06-28 CN CN201910572767.4A patent/CN112147029A/en active Pending
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5057574A (en) * | 1984-12-28 | 1991-10-15 | Mitsubishi Rayon Company, Ltd. | Process for producing an α-alkyl-substituted aromatic vinyl copolymer and a thermoplastic resin composition comprising the copolymer |
| EP0608949A1 (en) * | 1993-01-25 | 1994-08-03 | Shell Internationale Researchmaatschappij B.V. | Process for the preparation of moisture resistant vegetable fibres |
| US5496890A (en) * | 1994-03-03 | 1996-03-05 | Bayer Aktiengesellschaft | Super-absorbent polymers |
| US20150328123A1 (en) * | 2012-09-29 | 2015-11-19 | Hangzhou Gallop Biological Products Co., Ltd. | Cross-linked sodium hyaluronate gel for tissue filler for plastic surgery and preparation method thereof |
| US20160145357A1 (en) * | 2013-06-28 | 2016-05-26 | Galderma S.A. | Method for manufacturing a shaped crosslinked hyaluronic acid product |
| US20190062461A1 (en) * | 2013-06-28 | 2019-02-28 | Galderma S.A. | Process for preparing a cross-linked hyaluronic acid product |
| US20200247913A1 (en) * | 2013-06-28 | 2020-08-06 | Galderma S.A. | Method for manufacturing a shaped cross-linked hyaluronic acid product |
| WO2016167229A1 (en) * | 2015-04-15 | 2016-10-20 | キユーピー 株式会社 | Cross-linked product of carboxymethyl group-containing modified hyaluronic acid and/or salt of same, and method for producing same |
| CN108774329A (en) * | 2018-06-13 | 2018-11-09 | 浙江景嘉医疗科技有限公司 | A kind of preparation method of medical cross-linking sodium hyaluronate gel |
Non-Patent Citations (2)
| Title |
|---|
| 王召旭等: "整形手术用交联透明质酸钠凝胶", 《中华人民共和国医药行业标准YY/T 0962-2014》 * |
| 谢水祥等: "有机硅吸水膨胀型选择性堵水剂的合成与性能评价", 《石油钻探技术》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116124754A (en) * | 2023-04-17 | 2023-05-16 | 山东省中源联科生物工程集团有限公司 | Method for detecting residual quantity of cross-linking agent in sodium hyaluronate gel through image analysis |
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