CN115266979B - Method for measuring azodicarbonamide in textile and artificial leather - Google Patents
Method for measuring azodicarbonamide in textile and artificial leather Download PDFInfo
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- XOZUGNYVDXMRKW-AATRIKPKSA-N azodicarbonamide Chemical compound NC(=O)\N=N\C(N)=O XOZUGNYVDXMRKW-AATRIKPKSA-N 0.000 title claims abstract description 51
- 235000019399 azodicarbonamide Nutrition 0.000 title claims abstract description 51
- 239000004156 Azodicarbonamide Substances 0.000 title claims abstract description 49
- 238000000034 method Methods 0.000 title claims abstract description 24
- 239000002649 leather substitute Substances 0.000 title claims abstract description 21
- 239000004753 textile Substances 0.000 title claims abstract description 20
- 238000000605 extraction Methods 0.000 claims abstract description 52
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 48
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-dimethylformamide Substances CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims abstract description 48
- 239000012046 mixed solvent Substances 0.000 claims abstract description 21
- 238000002137 ultrasound extraction Methods 0.000 claims abstract description 21
- 239000007788 liquid Substances 0.000 claims abstract description 16
- 239000006228 supernatant Substances 0.000 claims abstract description 13
- 239000002904 solvent Substances 0.000 claims abstract description 12
- 238000001914 filtration Methods 0.000 claims abstract description 8
- 239000012634 fragment Substances 0.000 claims description 12
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 7
- 238000004811 liquid chromatography Methods 0.000 claims description 7
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 7
- 239000012498 ultrapure water Substances 0.000 claims description 7
- 239000012528 membrane Substances 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 6
- 238000005303 weighing Methods 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 4
- 239000012224 working solution Substances 0.000 claims description 4
- 238000012360 testing method Methods 0.000 claims description 2
- 238000001514 detection method Methods 0.000 abstract description 15
- 239000000523 sample Substances 0.000 description 16
- 239000000126 substance Substances 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 238000004128 high performance liquid chromatography Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 238000010812 external standard method Methods 0.000 description 3
- 230000014759 maintenance of location Effects 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 239000013074 reference sample Substances 0.000 description 3
- 238000007789 sealing Methods 0.000 description 3
- 230000008859 change Effects 0.000 description 2
- 238000005187 foaming Methods 0.000 description 2
- 239000004088 foaming agent Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000012216 screening Methods 0.000 description 2
- 239000011550 stock solution Substances 0.000 description 2
- 238000002604 ultrasonography Methods 0.000 description 2
- 206010067484 Adverse reaction Diseases 0.000 description 1
- 239000004604 Blowing Agent Substances 0.000 description 1
- 206010020751 Hypersensitivity Diseases 0.000 description 1
- 230000006838 adverse reaction Effects 0.000 description 1
- 208000026935 allergic disease Diseases 0.000 description 1
- 230000007815 allergy Effects 0.000 description 1
- 238000010171 animal model Methods 0.000 description 1
- 208000006673 asthma Diseases 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000711 cancerogenic effect Effects 0.000 description 1
- 231100000357 carcinogen Toxicity 0.000 description 1
- 231100000315 carcinogenic Toxicity 0.000 description 1
- 239000003183 carcinogenic agent Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- -1 diazo dimethylformamide Chemical compound 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 235000013373 food additive Nutrition 0.000 description 1
- 239000002778 food additive Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000010985 leather Substances 0.000 description 1
- 239000002207 metabolite Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- DUIOPKIIICUYRZ-UHFFFAOYSA-N semicarbazide Chemical compound NNC(N)=O DUIOPKIIICUYRZ-UHFFFAOYSA-N 0.000 description 1
- 238000000527 sonication Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
Classifications
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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
-
- 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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
-
- 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
- G01N30/86—Signal analysis
- G01N30/8675—Evaluation, i.e. decoding of the signal into analytical information
- G01N30/8679—Target compound analysis, i.e. whereby a limited number of peaks is analysed
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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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N2030/042—Standards
- G01N2030/047—Standards external
-
- 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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N2030/062—Preparation extracting sample from raw material
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- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
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Abstract
The invention provides a method for measuring azodicarbonamide in textiles and artificial leather, which uses a mixed solvent of acetone and DMF as an extraction solvent, and adopts an ultrasonic extraction method to extract azodicarbonamide in a sample; and filtering to obtain supernatant, and detecting and analyzing the filtered sample liquid by using a high performance liquid chromatograph. The method is simple to operate, wide in application range, applicable to printed textiles and artificial leather, high in extraction efficiency, high in detection accuracy and not easy to cause damage to detection instruments.
Description
Technical Field
The invention relates to the field of textile detection, in particular to a method for measuring azodicarbonamide in textiles and artificial leather.
Background
Azodicarbonamide is widely used as a foaming agent, and can generate a plurality of tiny bubbles in the industrial production process, so that substances are in a foaming state, and the elasticity and the strength of products are improved. The foaming agent has the advantages of good foaming effect, high quality, good product elasticity, uniform cell diameter and good strength, and is widely applied. Many plastics, such as PVC, EVC, PP, PE, PS, etc., employ azodicarbonamide as a blowing agent. PVC coating, imitation leather artificial leather, bra pad and the like in the textile field can be foamed by using azodicarbonamide.
Although azodicarbonamide is not carcinogenic in itself, it and some of its metabolites have some toxic effects on experimental animals. Under certain conditions, azodicarbonamide may react to produce semicarbazide carcinogens, and if the human body ingests excessive azodicarbonamide, adverse reactions such as asthma, allergy and the like may occur.
Azodicarbonamide is used in limited amounts as a food additive in the united states and china; while the uk health and safety agency recognizes azodicarbonamide as a "breath-sensitive substance". In the 2020 Standard 100by OEKO-TEX annex 4 and 6, a limit value of <1000mg/kg is required for all product grades. The European chemical administration (ECHA) officially issued notification of year 2016, 6 and 20, and the SVHC highly focused substance contained azodicarbonamide.
At present, the detection of azodicarbonamide in textiles and artificial leather is usually carried out by using DMF as an extraction solvent to extract the azodicarbonamide and then using a detection instrument. However, research shows that DMF as an extraction solvent not only can dissolve azodicarbonamide in textiles and artificial leather, but also can dissolve other components, so that an extraction liquid is turbid, and further, instruments and equipment are blocked, and the precision of the instruments is influenced and even cannot be detected.
Disclosure of Invention
The invention provides a method for measuring azodicarbonamide in textiles and artificial leather, which is used for improving the extraction efficiency of azodicarbonamide in printed textiles and artificial leather and reducing the damage to detection equipment.
The technical scheme of the invention is as follows: a method for measuring azodicarbonamide in textiles and artificial leather comprises the steps of using a mixed solvent of acetone and DMF as an extraction solvent, extracting azodicarbonamide in a sample by an ultrasonic extraction method, filtering to obtain supernatant, and detecting and analyzing the filtered supernatant by a high performance liquid chromatograph.
The invention is further arranged that the volume ratio of the acetone to the DMF in the mixed solvent is 15:1-35:1.
The invention is further arranged to comprise the steps of:
(1) Preparing a standard working solution of azodicarbonamide, and drawing a standard curve;
(2) Crushing a sample to be detected into fragments with the particle size of less than 0.5mm, uniformly mixing, weighing a proper amount of the sample to be detected, and placing the fragment into an extraction bottle;
(3) Adding a mixed solvent of acetone and DMF into an extraction bottle;
(4) Placing the extraction bottle into an ultrasonic extraction instrument for ultrasonic extraction, and filtering to obtain supernatant;
(5) And detecting and analyzing the supernatant obtained by filtering by using a high performance liquid chromatograph.
The invention further provides that in the step (2), the mass of the weighed sample to be tested is 1-2 g, and the mass is accurate to 0.01g.
The invention further provides that in the step (3), the addition volume of the mixed solvent of the acetone and the DMF is 5-15 mL.
The invention further provides that in the step (3), the volume ratio of the acetone to the DMF in the mixed solvent is 15:1-35:1.
The invention is further configured that in the step (4), the ultrasonic extraction conditions are as follows: the ultrasonic extraction power is set to 400-500W, the ultrasonic extraction temperature is 35-45 ℃, and the ultrasonic extraction time is 25-35 min.
The invention further provides that in step (4), the filtration is carried out using an organic filter membrane having a specification of 0.45 μm.
The invention further provides that the test conditions of the high performance liquid chromatograph are as follows: ZORBAX SB-Aq (4.6mm. Times.250 mm,5 μm) was a liquid chromatography column; the column temperature is 30+/-5 ℃; the mobile phase is ultrapure water with 100 percent; the flow rate is 0.8mL/min; the DAD detector wavelength was set to 275±5nm.
Compared with the prior art, the invention has the following beneficial effects:
(1) According to the determination method, the mixed solvent of acetone and DMF is used as the extraction solvent, so that the high-efficiency extraction of the azodicarbonamide in textiles and artificial leather is realized, and the damage of a high-performance liquid chromatograph is not easy to cause.
(2) The determination method provided by the invention has the advantages of simple operation and wide application range, and is suitable for textiles and artificial leather.
(3) The measuring method provided by the invention has the advantages of low detection limit and high accuracy.
Drawings
FIG. 1 is a standard graph of azodicarbonamide.
FIG. 2 is a chromatogram of azodicarbonamide in example 4.
Detailed Description
The invention will be further illustrated with reference to specific examples. It should be understood that the examples are illustrative of the present invention and are not intended to limit the scope of the present invention. Further, it is understood that various changes and modifications may be made by those skilled in the art after reading the teachings of the present invention, and such equivalents are intended to fall within the scope of the claims appended hereto.
Example 1 Standard Curve was plotted
Accurately weighing a certain amount of azodicarbonamide standard substance, wherein the volume ratio of acetone to DMF is 20:1 is taken as an extraction solvent, transferred into a volumetric flask to be diluted to a certain volume, and then prepared into an azodicarbonamide standard stock solution with the mass concentration of 1000mg/L for standby.
The volume ratio of acetone to DMF is 20:1, preparing 10.0mg/L, 20.0mg/L, 30.0mg/L, 40.0mg/L and 50.0mg/L standard working solutions by gradient dilution of the azo dicarboxamide standard stock solution by using the mixed solvent, and detecting the standard working solutions by using a high performance liquid chromatograph.
The high performance liquid chromatograph instrument conditions are as follows: ZORBAX SB-Aq (4.6mm. Times.250 mm,5 μm) was selected as the liquid chromatography column; the mobile phase was 100% ultrapure water. The column temperature is 30 ℃; the flow rate was 0.8mL/min. The DAD detector wavelength was set to 275nm.
Plotting the peak area of the chromatographic peak as an ordinate and the corresponding concentration as an abscissa, and drawing a standard working curve, wherein the standard curve is shown in figure 1; a standard curve linear equation is established, the result is shown in table 1, y= 8.536079x-6.9770, azodicarbonamide is in the range of 10.0mg/L to 50.0mg/L, and the correlation coefficient R is more than 0.999. The detection limit of the method is determined to be 1.0mg/kg, and the quantitative limit is determined to be 4.0mg/kg.
TABLE 1 Linear equation and correlation coefficient for azodicarbonamide
Example 2 screening of extraction solvent
The method comprises the steps of respectively adding standard sample of the artificial leather with the standard content of 30mg/kg of azodicarbonamide into fragments with the particle size of less than 0.5mm, uniformly mixing, accurately weighing 4 parts of 1+/-0.01 g, respectively marking the fragments as a, b, c, d, and respectively putting the weighed samples into an extraction bottle. Wherein, a, adding acetone: 10mL of mixed solvent with the volume ratio of DMF being 15:1, and sealing; b, adding acetone: 10mL of mixed solvent with the volume ratio of DMF being 20:1, and sealing; c, adding acetone: : 10mL of mixed solvent with the volume ratio of DMF being 35:1, and sealing; d, adding acetone: the mixed solvent with the DMF volume ratio of 10:1 is 10mL, and the mixture is sealed. The extraction bottle filled with the sample and the solvent is put into an ultrasonic extraction instrument for extraction, the extraction power is 450W, the extraction temperature is 40 ℃, and the extraction time is 30min. The supernatant was filtered through a 0.45 μm organic filter membrane and tested by high performance liquid chromatography. The high performance liquid chromatograph instrument conditions are as follows: ZORBAX SB-Aq (4.6mm. Times.250 mm,5 μm) was selected as the liquid chromatography column; the mobile phase was 100% ultrapure water. The column temperature is 30 ℃; the flow rate was 0.8mL/min. The DAD detector wavelength was set to 275nm.
The peak of azodicarbonamide appears at the corresponding retention time of the sample to be tested and the standard reference sample, the content of azodicarbonamide is calculated according to an external standard method, and the result is shown in Table 2.
TABLE 2 detection results of azodicarbonamide in different volume ratios of extraction solvents
| Numbering device | Acetone: DMF (V: V) | Azodicarbonamide (mg/kg) |
| a | 15:1 | 30.1 |
| b | 20:1 | 29.7 |
| c | 35:1 | 27.3 |
| d | 10:1 | Instrument blockage failure |
As can be seen from the results in table 2, the volume ratio of acetone to DMF was 20: the mixed solvent of 1 is used as the extraction solvent of azodicarbonamide, the extraction efficiency is better, and the instrument blockage can not occur, therefore, the subsequent detection of the sample adopts the volume ratio of acetone and DMF as 20:1 as an extraction solvent.
EXAMPLE 3 screening of ultrasonic extraction parameters
3.1 determination of ultrasound temperature
In order to determine the optimal sonication temperature, azodicarbonamide was extracted at 30℃40℃50℃60℃and 70℃respectively. The method comprises the following steps: respectively adding 120mg/kg sample into artificial leather, pulverizing into pieces with particle diameter below 0.5mm, uniformly mixing, accurately weighing 5 parts of 1+/-0.01 g, placing the weighed samples into an extraction bottle, and respectively adding acetone: and the mixed solvent with the DMF volume ratio of 20:1 is 10mL, and the mixture is sealed. The extraction bottle with the sample is put into an ultrasonic extraction instrument for extraction, and the extraction temperatures are respectively 30 ℃,40 ℃, 50 ℃, 60 ℃ and 70 ℃ and the extraction power is 450W, and the extraction time is 30min. The supernatant was filtered through a 0.45 μm organic filter membrane and tested by high performance liquid chromatography. The high performance liquid chromatograph instrument conditions are as follows: ZORBAX SB-Aq (4.6mm. Times.250 mm,5 μm) was selected as the liquid chromatography column; the mobile phase was 100% ultrapure water. The column temperature is 30 ℃; the flow rate was 0.8mL/min. The DAD detector wavelength was set to 275nm. The results are shown in Table 3.
TABLE 3 ultrasonic temperature and extraction Effect relationship
As is clear from the results in Table 3, the detected content of azodicarbonamide increases with increasing extraction temperature, and the maximum value is substantially reached when the extraction temperature increases to 40℃and the change after 40℃is not large, so that the extraction temperature is preferably 40 ℃.
3.2 determination of ultrasound Power
The experimental process is the same as the process for determining the ultrasonic temperature, and the difference is that under the condition that the ultrasonic extraction temperature is 40 ℃ and the extraction time is 30min, the extraction effects of the diazo dimethylformamide are detected under the conditions of different extraction powers of 300W, 350W, 400W, 450W and 500W. The results are shown in Table 4.
TABLE 4 relationship between ultrasonic power and extraction effect
As is clear from the results in Table 4, the content of azodicarbonamide increased with the increase of ultrasonic power, and the change was not substantially large after the power was increased to 450W, and the influence factor was relatively small. Thus, it is preferable that 450W be the ultrasonic power of the pretreatment.
Example 4 detection of azodicarbonamide content in textiles
The textile standard sample is crushed into fragments with the particle size of less than 0.5mm, the fragments are uniformly mixed, 1+/-0.01 g of the fragments are accurately weighed, and the standard adding content of the textile azodicarbonamide is 20mg/kg respectively. Putting the weighed samples into an extraction bottle, and respectively adding acetone: and the mixed solvent with the DMF volume ratio of 20:1 is 10mL, and the mixture is sealed. The extraction bottle with the sample is put into an ultrasonic extraction bottle for extraction with the extraction power of 450W and the extraction temperature of 40 ℃ for 30min. The supernatant was filtered through a 0.45 μm organic filter membrane and tested by high performance liquid chromatography. The high performance liquid chromatograph instrument conditions are as follows: ZORBAX SB-Aq (4.6mm. Times.250 mm,5 μm) was selected as the liquid chromatography column; the mobile phase was 100% ultrapure water. The column temperature is 30 ℃; the flow rate was 0.8mL/min. The DAD detector wavelength was set to 275nm.
As shown in fig. 2, the peak of azodicarbonamide appears at the corresponding retention time of the sample to be measured and the standard reference sample, and the content of azodicarbonamide in the textile is calculated according to an external standard method: 19.6mg/kg.
Example 5 detection of azodicarbonamide content in Artificial leather
The artificial leather is crushed into fragments with the particle size of less than 0.5mm by adding a standard sample, the fragments are uniformly mixed, 1+/-0.01 g of the fragments are accurately weighed, and the standard adding content of the azo dicarboxamide of the artificial leather is 30mg/kg respectively. Putting the weighed samples into an extraction bottle, and respectively adding acetone: and the mixed solvent with the DMF volume ratio of 20:1 is 10mL, and the mixture is sealed. The extraction bottle with the sample is put into an ultrasonic extraction bottle for extraction with the extraction power of 450W and the extraction temperature of 40 ℃ for 30min. The supernatant was filtered through a 0.45 μm organic filter membrane and tested by high performance liquid chromatography. The high performance liquid chromatograph instrument conditions are as follows: ZORBAX SB-Aq (4.6mm. Times.250 mm,5 μm) was selected as the liquid chromatography column; the mobile phase was 100% ultrapure water. The column temperature is 30 ℃; the flow rate was 0.8mL/min. The DAD detector wavelength was set to 275nm.
The peak of azodicarbonamide appears at the corresponding retention time of the sample to be tested and the standard reference sample, and the content of azodicarbonamide in the artificial leather is 28.9mg/kg according to the calculation of an external standard method.
From the results of the above examples, the detection method of azodicarbonamide in textiles and artificial leather is simple in pretreatment, low in detection limit, high in accuracy and small in damage to detection equipment.
The above examples illustrate only a few embodiments of the invention, which are described in detail and are not to be construed as limiting the scope of the invention. It should be noted that it will be apparent to those skilled in the art that several variations and modifications can be made without departing from the spirit of the invention, which are all within the scope of the invention.
Claims (6)
1. The method for determining azodicarbonamide in textiles and artificial leather is characterized in that a mixed solvent of acetone and DMF is used as an extraction solvent, azodicarbonamide in a sample is extracted by adopting an ultrasonic extraction method, supernatant is filtered and obtained, and the filtered supernatant is detected and analyzed by using a high performance liquid chromatograph;
in the mixed solvent, the volume ratio of the acetone to the DMF is 15:1-20:1;
the ultrasonic extraction conditions are as follows: the ultrasonic extraction power is set to 400-450W, the ultrasonic extraction temperature is 40-45 ℃, and the ultrasonic extraction time is 25-35 min;
the test conditions of the high performance liquid chromatograph are as follows: ZORBAX SB-Aq (4.6mm. Times.250 mm,5 μm) was a liquid chromatography column; the column temperature is 30+/-5 ℃; the mobile phase is ultrapure water with 100 percent; the flow rate is 0.8mL/min; the DAD detector wavelength was set to 275±5nm.
2. The method of measuring according to claim 1, comprising the steps of:
(1) Preparing a standard working solution of azodicarbonamide, and drawing a standard curve;
(2) Crushing a sample to be detected into fragments with the particle size of less than 0.5mm, uniformly mixing, weighing a proper amount of the sample to be detected, and placing the fragment into an extraction bottle;
(3) Adding a mixed solvent of acetone and DMF into an extraction bottle;
(4) Placing the extraction bottle into an ultrasonic extraction instrument for ultrasonic extraction, and filtering to obtain supernatant;
(5) And detecting and analyzing the supernatant obtained by filtering by using a high performance liquid chromatograph.
3. The method according to claim 2, wherein in the step (2), the mass of the sample to be measured is 1 to 2g, to the nearest 0.01g.
4. The method according to claim 2, wherein in the step (3), the mixed solvent of acetone and DMF is added in a volume of 5 to 15mL.
5. The method according to claim 2, wherein in the step (3), the volume ratio of acetone to DMF in the mixed solvent is 15:1 to 20:1.
6. The method according to claim 2, wherein in the step (4), the filtration is performed using an organic filter membrane having a size of 0.45 μm.
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