CN115266966A - Method for detecting content of dissolved matter of polyvinyl alcohol film - Google Patents
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- 239000004372 Polyvinyl alcohol Substances 0.000 title claims abstract description 76
- 229920002451 polyvinyl alcohol Polymers 0.000 title claims abstract description 76
- 238000000034 method Methods 0.000 title claims abstract description 36
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims abstract description 115
- 239000000126 substance Substances 0.000 claims abstract description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000011259 mixed solution Substances 0.000 claims abstract description 23
- 238000004128 high performance liquid chromatography Methods 0.000 claims abstract description 14
- 238000002791 soaking Methods 0.000 claims abstract description 13
- 239000000463 material Substances 0.000 claims abstract description 7
- 230000035945 sensitivity Effects 0.000 claims description 7
- 238000000926 separation method Methods 0.000 claims description 6
- 238000005259 measurement Methods 0.000 abstract description 2
- 238000012360 testing method Methods 0.000 description 9
- 238000001514 detection method Methods 0.000 description 8
- 238000004090 dissolution Methods 0.000 description 7
- 238000001035 drying Methods 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000004043 dyeing Methods 0.000 description 3
- 238000009776 industrial production Methods 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 206010042674 Swelling Diseases 0.000 description 2
- 238000004364 calculation method Methods 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- 238000004811 liquid chromatography Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000008961 swelling Effects 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 241001391944 Commicarpus scandens Species 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 238000006136 alcoholysis reaction Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000010835 comparative analysis Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000004513 sizing Methods 0.000 description 1
- 238000004611 spectroscopical analysis Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/26—Conditioning of the fluid carrier; Flow patterns
- G01N30/28—Control of physical parameters of the fluid carrier
- G01N30/30—Control of physical parameters of the fluid carrier of temperature
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/26—Conditioning of the fluid carrier; Flow patterns
- G01N30/28—Control of physical parameters of the fluid carrier
- G01N30/32—Control of physical parameters of the fluid carrier of pressure or speed
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/62—Detectors specially adapted therefor
- G01N30/74—Optical detectors
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/86—Signal analysis
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N2030/042—Standards
- G01N2030/045—Standards internal
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/26—Conditioning of the fluid carrier; Flow patterns
- G01N30/28—Control of physical parameters of the fluid carrier
- G01N30/30—Control of physical parameters of the fluid carrier of temperature
- G01N2030/3007—Control of physical parameters of the fluid carrier of temperature same temperature for whole column
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/26—Conditioning of the fluid carrier; Flow patterns
- G01N30/28—Control of physical parameters of the fluid carrier
- G01N30/32—Control of physical parameters of the fluid carrier of pressure or speed
- G01N2030/324—Control of physical parameters of the fluid carrier of pressure or speed speed, flow rate
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Abstract
The invention relates to the field of polaroids, in particular to a method for detecting the content of a polyvinyl alcohol film dissolved matter. The method comprises the following steps: (1) Adding a polyvinyl alcohol film into water for soaking to obtain a mixed solution containing a polyvinyl alcohol film dissolved-out material and glycerol; (2) Detecting the mixed solution by adopting high performance liquid chromatography, wherein the mobile phase is pure water, and the concentration C of the glycerol in the mixed solution is detected1Performing measurement by using polyvinyl alcohol film dissolved matter in chromatogram andthe peak height or peak area ratio of the glycerol to obtain the concentration C of the glycerol1With the concentration C of the dissolved-out matter of the polyvinyl alcohol film in the mixed solution2The relation between them, then C is calculated2Followed by C2And calculating the content of the dissolved substance of the polyvinyl alcohol film. The invention adopts the glycerol as the internal standard substance, and can quickly and accurately detect the polyvinyl alcohol film product.
Description
Technical Field
The invention relates to the field of polaroids, in particular to a method for detecting the content of a polyvinyl alcohol film dissolved matter.
Background
Polyvinyl alcohol is a high molecular material and is widely applied to the industries of medical treatment, construction, textile and the like. Polyvinyl alcohol is soluble in water, and its solubility in water is mainly influenced by the degree of polymerization and alcoholysis. The preparation of the polyvinyl alcohol film is based on a solution method, the polyvinyl alcohol is dissolved and then cast into a film, and the polyvinyl alcohol film is obtained after drying, can be used for manufacturing the polaroid and is mainly applied to the industries of liquid crystal displays, sunglasses and the like. When the polyvinyl alcohol film is used for manufacturing the polaroid, the film is required to be placed in water for swelling, then soaked in a medicine for dyeing, stretching and sizing, and finally the polaroid is formed after the polyvinyl alcohol film is attached to a protective film.
Because the production process and raw materials of the polyvinyl alcohol film are different, the dissolution time and dissolution amount of dissolution materials of different polyvinyl alcohol films are different. When the amount of the dissolved substances is too high, the elongation of the polyvinyl alcohol film is too low, the polyvinyl alcohol film is easy to break during processing, and the optical performance of the polarizer after molding is influenced. When the dissolution time of the dissolved substances is longer, the film is not completely dissolved in the swelling stage, so that a large amount of substances are remained on the film, and partial dissolved substances can be continuously dissolved in the dyeing medicine, so that the dyeing effect is seriously influenced. Because the dissolution in the polyvinyl alcohol film not only affects the production process of the whole polaroid, but also has a large influence on the performance of the polaroid, a related method must be established to detect the content of the dissolution in the polyvinyl alcohol film so as to achieve the purposes of improving the product quality and promoting the process improvement.
The traditional dissolved substance test needs to consume a large amount of samples to dry and weigh the dissolved substance after washing, so that the test period is too long, and the dissolved substance volatilizes in the drying process, so that the test parallelism is too poor and the data is inaccurate.
Disclosure of Invention
The invention aims to overcome the problems of poor detection accuracy of the dissolved matter and no related accurate detection method of the dissolved matter of the polyvinyl alcohol film in the prior art, and provides a method for detecting the content of the dissolved matter of the polyvinyl alcohol film.
In order to achieve the above object, the present invention provides a method for detecting the content of an eluted polyvinyl alcohol film, comprising:
(1) Adding a polyvinyl alcohol film into water for soaking to obtain a mixed solution containing a polyvinyl alcohol film dissolved-out material and glycerol;
(2) Detecting the mixed solution by adopting high performance liquid chromatography, wherein the mobile phase is pure water, and the concentration C of the glycerol in the mixed solution is detected1Measuring, and obtaining the concentration C of glycerol by the peak height or peak area ratio of the peak of the polyvinyl alcohol film eluate to the glycerol in the chromatogram1With the concentration C of the dissolved matter of the polyvinyl alcohol film in the mixed solution2In relation to each other, and then calculate C2Then use C2And calculating the content of the dissolved substance of the polyvinyl alcohol film.
Preferably, in the step (1), the weight ratio of the polyvinyl alcohol film to water is 1: (1-100).
Preferably, in step (1), the soaking time in step (1) is 1-240min.
Preferably, in step (1), the temperature of the soaking is 20-30 ℃.
Preferably, in step (2), the flow rate of the mobile phase is 0.5-2mL/min.
Preferably, in the step (2), a C18 chromatographic column is used as a separation column, and the column temperature is 30-50 ℃.
Preferably, in step (2), the sample amount is 5-50 μ L, and the collection time is 5-60min.
Preferably, in step (2), the detector of the high performance liquid chromatography is a refractive index detector.
Preferably, in step (2), the sensitivity of the differential refractive detector is 4 to 32.
Preferably, in step (2), the temperature of the differential refractive detector is 30 to 50 ℃.
The method has the advantages of less sample consumption, convenient detection, short detection time and accurate result, can quickly and accurately detect the polyvinyl alcohol film products and samples in industrial production, is convenient for guiding the improvement of the process technology, and improves the quality of the products.
Drawings
FIG. 1 is a standard curve of glycerol concentration in the present invention;
FIG. 2 is a liquid chromatography spectrum of a mixed solution in example 1 of the present invention;
FIG. 3 is a comparison of the results of the present method and the prior art method for determining the content of the dissolved matter in the polyvinyl alcohol film.
Detailed Description
The following detailed description of embodiments of the invention refers to the accompanying drawings. It should be understood that the detailed description and specific examples, while indicating the preferred embodiment of the invention, are given by way of illustration and explanation only, not limitation.
The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and such ranges or values should be understood to encompass values close to those ranges or values. For ranges of values, between the endpoints of each of the ranges and the individual points, and between the individual points may be combined with each other to give one or more new ranges of values, and these ranges of values should be considered as specifically disclosed herein.
The invention provides a method for detecting the content of dissolved substances of a polyvinyl alcohol film, which comprises the following steps:
(1) Adding a polyvinyl alcohol film into water for soaking to obtain a mixed solution containing a polyvinyl alcohol film dissolved-out material and glycerol;
(2) Detecting the mixed solution by adopting high performance liquid chromatography, wherein the mobile phase is pure water, and the concentration C of glycerol in the mixed solution is detected1Measuring, and obtaining the concentration C of glycerol by the peak height or peak area ratio of the peak of the polyvinyl alcohol film eluate to the peak of glycerol in the chromatogram1With the concentration C of the dissolved-out matter of the polyvinyl alcohol film in the mixed solution2The relation between them, then C is calculated2Followed by C2And calculating the content of the dissolved substance of the polyvinyl alcohol film.
The polyvinyl alcohol film extract in the invention refers to: when the polyvinyl alcohol film swells in water, the polyvinyl alcohol film is dissolved in other polyvinyl alcohol substances except the additive glycerol.
Preferably, in the step (1), the weight ratio of the polyvinyl alcohol film to the water is 1: (1-100). Specifically, the weight ratio of the polyvinyl alcohol film to water may be 1: 1. 1: 10. 1: 20. 1: 30. 1: 40. 1: 50. 1: 60. 1: 70. 1: 80. 1:90 or 1:100.
preferably, in step (1), the soaking time is 1-240min. Specifically, the soaking time may be 1min, 30min, 60min, 90min, 120min, 150min, 180min, 210min or 240min.
In the present invention, in the step (1), the temperature of the soaking is 20 to 30 ℃. Specifically, the temperature of the soaking may be 20 ℃, 21 ℃, 22 ℃, 23 ℃, 24 ℃, 25 ℃, 26 ℃, 27 ℃, 28 ℃, 29 ℃ or 30 ℃.
In the present invention, in the step (2), the flow rate of the mobile phase is 0.5 to 2mL/min. Specifically, the flow rate of the mobile phase may be 0.5 to 2mL/min. Preferably, the flow rate of the mobile phase is 1mL/min.
In the invention, in the step (2), a C18 chromatographic column is used as a separation column, and the column temperature is 30-50 ℃. In specific cases, the column temperature can be 30 ℃, 31 ℃, 32 ℃, 33 ℃, 34 ℃, 35 ℃, 36 ℃, 37 ℃, 38 ℃, 39 ℃, 40 ℃, 41 ℃, 42 ℃, 43 ℃, 44 ℃, 45 ℃, 46 ℃, 47 ℃, 48 ℃, 49 ℃ or 50 ℃.
In the invention, in the step (2), when the mixed solution is detected by adopting high performance liquid chromatography, the sample injection amount is 5-50 mu L, and the collection time is 5-60min. Specifically, the sample amount may be 5 μ L, 10 μ L, 20 μ L, 30 μ L, 40 μ L, or 50 μ L, and the collection time may be 5min, 10min, 15min, 20min, 25min, 30min, 35min, 40min, 45min, 50min, 55min, 60min. Preferably, the sample amount is 10 μ L, and the collection time is 10min.
In the present invention, in the step (2), the detector of the high performance liquid chromatography is a refractive index detector.
Preferably, in step (2), the sensitivity of the refractive index detector is 4 to 32. In particular, the sensitivity of the differential refractive detector may be 4, 8, 16 or 32. Preferably, the sensitivity of the differential refractive detector is 4.
Preferably, in step (2), the temperature of the refractive index detector is 30 to 50 ℃. Specifically, the temperature of the differential refractive index detector may be 30 ℃, 31 ℃, 32 ℃, 33 ℃, 34 ℃, 35 ℃, 36 ℃, 37 ℃, 38 ℃, 39 ℃, 40 ℃, 41 ℃, 42 ℃, 43 ℃, 44 ℃, 45 ℃, 46 ℃, 47 ℃, 48 ℃, 49 ℃ or 50 ℃.
In the invention, the concentration C of the glycerol in the mixed solution is measured by adopting a standard curve method1And (4) carrying out measurement.
The method disclosed by the invention has the advantages of less sample consumption, convenience in detection, short detection time and accurate result, and can be used for quickly and accurately detecting the polyvinyl alcohol film products and the samples in industrial production by adopting the glycerol as the internal standard substance, so that the improvement of the process technology is facilitated, and the quality of the products is improved.
The present invention will be described in detail below by way of examples, but the method of the present invention is not limited thereto.
In the following examples, the polyvinyl alcohol film used was obtained from Chongqing New Spectroscopy materials science and technology Co., ltd under the designation SG-01; the high performance liquid chromatography is waters2514, C18 column is used as separation column, differential refraction detector waters2918 is used as detector, and pure water is used as mobile phase.
The detection method of the standard curve of the concentration and the peak area of the glycerol comprises the following steps: the mass fractions are respectively prepared as follows: 0.1%,0.25%,0.5%,0.75%,1%,1.25%,1.5% of a standard aqueous solution of glycerol (glycerol is available from HPLC purity, cromet chemicals ltd, tianjin). Respectively making a liquid chromatography standard curve for the prepared solution, taking pure water as a mobile phase, and setting high performance liquid chromatography parameters: the flow rate of the mobile phase is 1mL/min, the column temperature of the separation column is 40 ℃, the temperature of the detector is 40 ℃, the sensitivity of the differential refraction detector is 4, the sample amount is 10uL, the acquisition time is 10min, and the peak areas of glycerol in the liquid chromatogram under different concentrations are obtained, so that a standard curve of the concentration of the glycerol and the peak area is obtained, as shown in FIG. 1, and the linear correlation coefficient r =0.9999.
Example 1
(1) Adding 25.173g of a polyvinyl alcohol film 1223 sample into 500.879g of water, soaking at 25 ℃ for 10min, fully shaking up to obtain a mixed solution containing a polyvinyl alcohol film eluate and glycerol, detecting the mixed solution by adopting a high performance liquid chromatography, wherein a mobile phase is pure water, and setting high performance liquid chromatography parameters: the flow rate of the mobile phase is 1mL/min, the column temperature of the separation column is 40 ℃, the temperature of the detector is 40 ℃, the sensitivity of the differential refraction detector is 4, the sample injection amount is 10uL, the acquisition time is 10min, and the concentration C of glycerol in the mixed solution is obtained by adopting a standard curve detection10.476 wt%;
(2) By the peak area ratio of the peak areas of the polyvinyl alcohol film eluate and the glycerol in the chromatogram,to obtain the concentration C of glycerol1With the concentration C of the dissolved-out matter of the polyvinyl alcohol film in the mixed solution2The relation between them, then C is calculated2Followed by C2And calculating the content of the dissolved substance of the polyvinyl alcohol film.
The HPLC chromatogram of example 1 is shown in FIG. 2, which shows that the PVA film eluate is well separated from glycerol and has a symmetrical peak shape.
The results of example 1 are shown in table 1.
The calculation method of the content of the glycerol in the polyvinyl alcohol film comprises the following steps: c1X (weight of polyvinyl alcohol film + weight of water)/weight of polyvinyl alcohol film;
the calculation method of the content of the dissolved substance of the polyvinyl alcohol film in the polyvinyl alcohol film comprises the following steps: c2X (weight of polyvinyl alcohol film + weight of water)/weight of polyvinyl alcohol film.
TABLE 1
Example 2
(1) 5 parts of a polyvinyl alcohol film 1225 sample, each part of which is 25g in weight, are added with 500g of water, which is respectively marked as No. 1-5 and No. 1-5 samples, and the obtained results are detected according to the method of the example 1 and are shown in the table 2.
TABLE 2
As can be seen from Table 2, the results obtained by performing 5 parallel experiments by using the method are between 0.097% and 0.104%, the results are stable, and the parallelism is good.
Comparative example 1
Taking 5 parts of the same polyvinyl alcohol film 1225 sample as in example 2, respectively marking as 6-10#, and respectively detecting the content of the polyvinyl alcohol film dissolved-out substance in the sample 6-10# by using a traditional method, wherein the concrete steps are as follows:
(1) Drying the sample in an oven (the drying temperature is 80 ℃) to constant weight, recording the initial mass m1, then putting the sample into pure water for washing, fully removing dissolved components in the sample, drying the washed sample in the oven again to constant weight, recording m2, wherein m1-m2 is the total amount of the dissolved substance of the polyvinyl alcohol film and glycerol in the sample, and thus obtaining the loss w1= (m 1-m 2)/m 1 of the sample.
(2) And (3) testing the content of the glycerol in the sample by using a method for testing the content of 5.3 glycerol in the chemical reagent of GB/T687-2011 in the national standard to obtain the content w2 of the glycerol in the sample, and obtaining the content w3 of the dissolved substance of the polyvinyl alcohol film by the difference value of the sample loss w1 and the content w2 of the glycerol.
The specific results of the dissolution using the conventional drying method are shown in Table 3.
TABLE 3
| Sample(s) | 6# | 7# | 8# | 9# | 10# |
| |
10.82 | 10.65 | 10.37 | 10.58 | 10.62 |
| |
10.12 | 10.20 | 10.42 | 9.91 | 10.46 |
| Polyvinyl alcohol film extract content w 3/wt% | 0.70 | 0.45 | -0.05 | 0.67 | 0.16 |
FIG. 3 is a comparative analysis chart of the test results of two different methods of example 2 and comparative example 1, and it can be seen that the test results of the conventional method have large deviation and even have negative values due to the complicated whole operation process and the low proportion of the dissolved-out substance of the polyvinyl alcohol film in the whole loss amount, and the introduced error has a great influence on the test results, resulting in inaccurate test data and poor parallelism.
The results show that the method of the invention adopts glycerol as the internal standard substance, and can quickly and accurately detect polyvinyl alcohol film products and samples in industrial production.
The preferred embodiments of the present invention have been described above in detail, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, many simple modifications can be made to the technical solution of the invention, including combinations of various technical features in any other suitable way, and these simple modifications and combinations should also be regarded as the disclosure of the invention, and all fall within the scope of the invention.
Claims (10)
1. A method for detecting the content of dissolved substances in a polyvinyl alcohol film, which comprises the following steps:
(1) Adding a polyvinyl alcohol film into water for soaking to obtain a mixed solution containing a polyvinyl alcohol film dissolved-out material and glycerol;
(2) Detecting the mixed solution by adopting high performance liquid chromatography, wherein the mobile phase is pure water, and the concentration C of the glycerol in the mixed solution is detected1Measuring, and obtaining the concentration C of glycerol by the peak height or peak area ratio of the peak of the polyvinyl alcohol film eluate to the glycerol in the chromatogram1With the concentration C of the dissolved matter of the polyvinyl alcohol film in the mixed solution2The relation between them, then C is calculated2Followed by C2And calculating the content of the dissolved substance of the polyvinyl alcohol film.
2. The method according to claim 1, wherein in step (1), the weight ratio of the polyvinyl alcohol film to water is 1: (1-100).
3. The method according to claim 1 or 2, wherein in step (1), the soaking time is 1-240min.
4. The method according to claim 3, wherein the temperature of the soaking in the step (1) is 20-30 ℃.
5. The method according to claim 1, wherein in step (2), the flow rate of the mobile phase is 0.5-2mL/min.
6. The method according to claim 1 or 5, wherein in step (2), a C18 chromatographic column is used as the separation column, and the column temperature is 30-50 ℃.
7. The method according to claim 1, wherein in the step (2), the sample amount is 5 to 50 μ L, and the collection time is 5 to 60min.
8. The method of claim 1, wherein in step (2), the detector of the high performance liquid chromatography is a differential refractive detector.
9. The method of claim 8, wherein in step (2), the sensitivity of the refractive index detector is 4-32.
10. The method according to claim 8 or 9, wherein in step (2), the temperature of the differential refractive detector is 30-50 ℃.
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