A method for detecting the content of perfluorinated and polyfluorinated compounds in a textile

Abstract

The application discloses a method for detecting the content of perfluorinated and polyfluorinated compounds in textiles, and specifically comprises the following steps: reagent preparation, sample preparation, extraction of an extraction solution by an extraction device, rotary evaporation, nitrogen blowing, acetonitrile constant volume, filtration, and then obtaining a to-be-detected extraction solution; the to-be-detected extraction solution is detected by gas chromatography-mass spectrometry, so that the content of perfluorinated and polyfluorinated compounds in the to-be-detected sample is obtained. The detection method can realize one-time extraction and simultaneous analysis of 12 kinds of perfluorinated and polyfluorinated compounds including 4 fluorinated telomer alcohols, 3 fluorinated acrylates and 5 perfluorooctane sulfonamide compounds, is suitable for rapid detection of a large number of samples, and has the advantages of rapidness, low cost, high sensitivity, convenient operation, extraction efficiency of more than 95%, suitability for screening of textile complex matrix materials, filling of the deficiency of the existing method in simultaneous extraction of multiple types of PFASs in textiles, and good practicability and popularization value.

Description

Technical Field

[0001] This invention belongs to the field of textile testing technology, and in particular relates to a method for detecting the content of perfluorinated and polyfluorinated compounds in textiles. Background Technology

[0002] Per- and polyfluoroalkyl substances (PFAS) are organic compounds in which all or part of the hydrogen atoms in the straight or branched chains are replaced by fluorine. There are many types of PFAS, including perfluoroalkyl carboxylic acids, perfluoroalkyl sulfonic acids, perfluoroalkyl sulfonamides, fluorinated telomerols, and perfluoroalkyl phosphates. PFAS possess unique thermal stability and excellent hydrophobic / oleophobic surface activity. Perfluorooctane sulfonyl compounds are used as finishing agents in textiles such as clothing and carpets, as well as leather and leather products, providing excellent water and stain resistance. However, with advancements in analytical techniques, existing toxicological studies have shown that PFAS exhibit hepatotoxicity, developmental and reproductive toxicity, genetic and immunotoxicity, and carcinogenicity in experimental animals, posing a serious threat to human health.

[0003] Because textiles are composed of various fibers, which may be a single fiber or a mixture of two or more fibers, and these fibers come from a wide range of sources (natural, synthetic, man-made fibers, etc.), a variety of chemical substances are added during the production process, such as dyes, pigments, flame retardants, waterproofing and oil-repellent agents (such as PFASs), antibacterial agents, and wrinkle-resistant agents. Due to the material composition, the textile matrix itself introduces a large number of interfering substances during chemical analysis. Some literature clearly states that "textile sample matrices are complex and contain many interfering ions." These interfering substances can seriously affect the accuracy and sensitivity of detection, making the identification and quantification of target analytes difficult. Co-extracts can cause matrix interference such as ion suppression effects, severely affecting the accuracy of quantification.

[0004] Therefore, traditional textile testing methods (such as PFOA and PFOS) can no longer meet the requirements of the Oeko-Tex 100 standard for increasing the categories and limits of PFAS, and cannot effectively meet the needs of efficient separation and quantitative analysis of complex chemical components. Developing a simple and rapid analytical method capable of simultaneously detecting multiple volatile PFAS is urgently needed in current testing work. Summary of the Invention

[0005] The present invention provides a method for detecting the content of perfluorinated and polyfluorinated compounds in textiles.

[0006] This invention is achieved through the following technical solution:

[0007] A. Reagent preparation: Weigh a certain amount of each perfluorinated and polyfluorinated compound standard to prepare an independent standard stock solution (1000 mg / L). Then, mix the independent standard stock solutions together to prepare a mixed standard intermediate solution (50 mg / L). Finally, prepare standard working solutions of different concentrations (0.01 mg / L-25 mg / L) from the mixed standard intermediate solution for later use.

[0008] B. Sample preparation: Take a certain weight of textile and cut it into pieces. The size of the pieces should be less than 5mm×5mm to obtain the sample.

[0009] C. Extraction: Take a certain amount of the sample obtained in step B into a container, add a certain amount of acetonitrile to the container to completely submerge the sample; place the container containing the sample into the extraction device, extract for 10-60 minutes at an extraction temperature of 40-80℃, let stand, and separate to obtain the extract. Then add a certain amount of acetonitrile to the same container to extract and separate the same sample. Repeat this operation to extract the same sample 1-3 times to obtain extracts. Combine the extracts obtained from each extraction, and dry the combined extract by rotary evaporation, nitrogen blowing, acetonitrile dilution, and filtration to obtain the extract to be tested.

[0010] D. Gas Chromatography-Mass Spectrometry: Take a certain amount of the standard working solution prepared in step A and put it into the gas chromatograph-mass spectrometer for detection. Prepare a working curve based on the data of the detection chromatogram. Put the test extract prepared in step C into the gas chromatograph-mass spectrometer for detection. Then compare the data of the detection chromatogram of the test extract with the working curve to obtain the content of perfluorinated and polyfluorinated compounds in the test sample.

[0011] The beneficial effects of this invention are: this detection method can achieve the determination of 12 perfluorinated and polyfluorinated compounds, including 4 fluorinated telomer alcohols, 3 fluorinated acrylates and 5 perfluorooctane sulfonyl compounds, in a single extraction and simultaneous analysis. It can also shorten the pretreatment time and reduce solvent consumption, making it suitable for rapid detection of large batches of samples.

[0012] This detection method is rapid, low-cost, highly sensitive, and easy to operate, with an extraction efficiency exceeding 95% and a wide coverage. It is particularly suitable for screening complex matrices in textiles, solving the problem of the large variety of PFASs, their significant differences in properties, and the incomplete extraction by traditional methods. This detection method fills the gap in existing methods for simultaneously extracting multiple types of PFASs from textiles, and has great practical value and potential for widespread application. Attached Figure Description

[0013] Figure 1 The SIM spectra were obtained for a mixed standard solution of 12 volatile perfluorinated and polyfluorinated compounds under established conditions.

[0014] Figure 2Chromatograms of 12 target analytes under different dilute solvents;

[0015] Figure 3 Extraction efficiency for different extraction solvents (n=3). Detailed Implementation

[0016] To enable those skilled in the art to better understand the technical solution of this invention, the following description is provided in conjunction with the appendix. Figures 1-3 The specific implementation method is described in detail.

[0017] A method for detecting the content of perfluorinated and polyfluorinated compounds in textiles, comprising the following steps:

[0018] A. Reagent preparation:

[0019] A1. Preparation of standard stock solutions (1000 mg / L): Accurately weigh a certain amount of each perfluorinated and polyfluorinated compound standard (accurate to 0.1 mg), place them in volumetric flasks, dilute with methanol to the mark, mix well, and obtain independent standard stock solutions for each perfluorinated and polyfluorinated compound. Store in brown stock bottles for later use.

[0020] A2. Preparation of mixed standard intermediate solution (50 mg / L): Accurately transfer a certain amount of each standard stock solution obtained in step A1 into the same volumetric flask, dilute with acetonitrile to the mark, mix well, and obtain a mixed standard intermediate solution of perfluorinated and polyfluorinated compounds. Store in a brown storage bottle for later use.

[0021] A3. Preparation of Standard Working Solutions (0.01 mg / L - 25 mg / L): According to the requirements of gas chromatography-mass spectrometry detection, accurately transfer a certain volume of the mixed standard intermediate solution obtained in step A2, dilute it with acetonitrile to prepare standard working solutions of different concentrations, and mix well to obtain standard working solutions of different concentrations for each perfluorinated and polyfluorinated compound. All prepared standard working solutions of different concentrations should be stored in brown storage bottles for later use; these standard working solutions of different concentrations will be used to subsequently prepare standard curves based on the sample conditions. The specific preparation methods for standard working solutions of different concentrations are as follows:

[0022] Based on the 0.01 mg / L and 25 mg / L standard working solutions prepared by the acetonitrile dilution method, several standard working solutions with different concentrations are prepared by taking a certain volume of mixed standard intermediate solution within the concentration range of 0.01 mg / L to 25 mg / L using the same acetonitrile dilution method. For ease of calculation, the subsequent concentration value is set to be n times the previous concentration value, where n is 5, 10, 15, 20 or other values ​​that are easy to calculate. However, in the same batch of standard working solutions, the multiple n between adjacent concentration values ​​is the same fixed value.

[0023] B. Sample preparation: Take a certain weight of textile and cut it into pieces. The size of the pieces should be less than 5mm×5mm to obtain the sample.

[0024] C. Extraction: Take a certain amount of the sample obtained in step B into a container, add 20-30 ml of acetonitrile per gram (g) of sample in the container to completely submerge the sample; place the container containing the sample in an extraction device, and use any one of ultrasonic extraction, Soxhlet extraction, or mechanical oscillation extraction. Extract for 10-60 min at an extraction temperature of 40-80℃, allow to stand and precipitate, and separate to obtain the first extract; then, add 20-30 ml of acetonitrile to the container again to extract the sample residue a second time, and repeat this operation to extract the sample residue 1-3 times; then combine the extracts, and dry the combined extract by rotary evaporation, nitrogen blowing, acetonitrile dilution (volume ratio of the two is 0.8-1:1), and filter through a microporous membrane (pore size less than 0.22µm) to obtain the extract to be tested.

[0025] D. Gas Chromatography-Mass Spectrometry (GC-MS): The extract to be tested is analyzed using a gas chromatograph-mass spectrometer. A certain amount of the standard working solution prepared in step A3 is placed into the GC-MS instrument to prepare a working curve. The extract to be tested, prepared in step C, is then placed into the GC-MS instrument for analysis to obtain the content of perfluorinated and polyfluorinated compounds in the sample. The specific operating procedure is as follows:

[0026] D1. In the same batch of standard working solutions prepared in step A3, standard working solutions of different concentrations are selected and injected sequentially into a gas chromatograph-mass spectrometer for detection to obtain chromatograms of the content of perfluorinated and polyfluorinated compounds in each concentration of standard working solutions. Subsequently, based on the detection peak data in the detection chromatograms, a standard curve is established with concentration as the abscissa (X-axis) and peak area (or peak height) as the ordinate (Y-axis). The curve equation is: y=ax+b.

[0027] D2. Under identical gas chromatography-mass spectrometry (GC-MS) conditions, the sample to be tested is injected into the GC-MS instrument for detection. The chromatogram of the content of perfluorinated and polyfluorinated compounds in the sample to be tested is obtained. The chromatogram shows the peak data (peak area or peak height) of perfluorinated and polyfluorinated compounds in the sample to be tested.

[0028] D3. Substitute the peak data (peak area or peak height) of perfluorinated and polyfluorinated compounds obtained from the chromatogram in step D2 into the equation y=ax+b of the standard curve to calculate the accurate concentration of the target (perfluorinated and polyfluorinated compounds) in the extract to be tested, and finally achieve the purpose of obtaining the content of perfluorinated and polyfluorinated compounds in the sample to be tested.

[0029] D4. In the detection of the extract to be tested in step D2, multiple peaks may appear, representing different perfluorinated and polyfluorinated compounds. By comparing the peak retention time and mass spectrometry information, the specific substance can be determined. Then, the content can be determined by comparing it with the peak area and standard curve in step D2.

[0030] D5. Gas chromatography-mass spectrometry determination shall be performed under the following conditions:

[0031] a) Chromatographic column: DB-5MS capillary column (30m×0.25mm×0.25µm) or its equivalent;

[0032] b) The heating program is as follows: initial temperature 40℃ (hold for 0 min), increase to 100℃ at 5℃ / min (hold for 0 min), and then rapidly increase to 280℃ at 20℃ / min (hold for 3 min).

[0033] c) Carrier gas: Helium, purity ≥ 99.999%, flow rate 1.2 mL / min;

[0034] d) Inlet temperature: 280℃;

[0035] e) Injection volume: 1 μL;

[0036] f) Mass spectrometry interface temperature: 260℃;

[0037] g) Ion source: Electron impact ionization source (EI), temperature 250℃;

[0038] h) Transmission line temperature: 280℃;

[0039] i) Detection method: Select Ion Scan (SIM) mode.

[0040] The perfluorinated and polyfluorinated compounds include at least one of fluorinated telomer alcohols, fluorinated acrylates, and perfluorooctane sulfonamides, wherein,

[0041] The fluorinated telomer alcohol includes at least one of 1H,1H,2H,2H-perfluorohexanol, 1H,1H,2H,2H-perfluorooctanol, 1H,1H,2H,2H-perfluorodecanol, and 1H,1H,2H,2H-perfluorododecylol.

[0042] The fluorinated acrylates include at least one of 1H,1H,2H,2H-perfluorohexanol acrylate, 1H,1H,2H,2H-perfluorooctanol acrylate, and 1H,1H,2H,2H-perfluorododecyl acrylate.

[0043] The perfluorooctane sulfonamide compounds include at least one of N-methylperfluorooctane sulfonamide ethanol, N-ethylperfluorooctane sulfonamide ethanol, perfluorooctane sulfonamide, perfluoro-N-methyloctane sulfonamide, and perfluoro-N-ethyloctane sulfonamide.

[0044] Furthermore, the LogP values ​​of the perfluorinated and polyfluorinated compounds, including fluoropolymers (FTOHs), fluoropolymer polyacrylates (FTAs), perfluorooctyl sulfonamides (FOSAs), and perfluorooctyl sulfonamide ethanol (FOSEs), differ significantly, and their boiling points and polarities vary. Therefore, a chromatographic column with a wider range of applications is required. Thus, a DB-5 (30m × 0.25mm × 0.25µm) chromatographic column was used for separation.

[0045] Example 1

[0046] Experimental methods

[0047] A1. Reagents

[0048] A1.1 Methanol: chromatographic grade.

[0049] A1.2 Acetonitrile: chromatographic grade.

[0050] A1.3, 12 perfluorinated and polyfluorinated compound standards: see Table 1, purity ≥98%.

[0051] A1.4 Standard stock solutions (1000 mg / L): Accurately weigh 0.025 g (accurate to 0.1 mg) of each perfluorinated and polyfluorinated compound standard, place them in 25 mL volumetric flasks, dilute to the mark with methanol, mix well, and obtain standard stock solutions of each perfluorinated and polyfluorinated compound. Store in brown stock bottles.

[0052] A1.5 Mixed standard intermediate solution (50 mg / L): Accurately transfer 1.25 mL of the standard stock solutions of each perfluorinated and polyfluorinated compound prepared in step A1.4 into a 25 mL volumetric flask, dilute to the mark with acetonitrile, mix well, and obtain the mixed standard intermediate solution of each perfluorinated and polyfluorinated compound in a brown storage bottle.

[0053] A1.6 Standard working solutions (0.01 mg / L-25 mg / L): When performing the detection, according to the requirements of gas chromatography-mass spectrometry, accurately transfer a certain volume of the mixed standard intermediate solution prepared in step A1.5, dilute it with acetonitrile to prepare a mixed standard working solution, mix well, and you will get the standard working solutions of each perfluorinated and polyfluorinated compound. This mixed standard working solution is the sample reagent, and it is stored in a brown storage bottle.

[0054] A1.61. The specific preparation method for standard working solutions of different concentrations is as follows: Accurately transfer a certain volume of mixed standard intermediate solution and dilute it with acetonitrile to obtain standard working solutions with concentrations of 0.01 mg / L and 25 mg / L respectively. Then, within the concentration range of 0.01 mg / L to 25 mg / L, use the same acetonitrile dilution method to take a certain volume of mixed standard intermediate solution to prepare several standard working solutions with different concentration values. Store them in brown storage bottles for later use. For ease of calculation, the subsequent concentration value is set to be n times the previous concentration value, where n is 5, 10, 15, 20 or other values ​​that are easy to calculate. However, in the same batch of standard working solutions, the multiple n between adjacent concentration values ​​is the same fixed value.

[0055] Note: When stored in a refrigerator at -18°C away from light, the standard stock solution has a shelf life of 12 months, while the mixed standard intermediate solution and standard working solution have a shelf life of 3 months.

[0056] Table 1. List of 12 perfluorinated and polyfluorinated compounds

[0057]

[0058] A2. Instruments and Equipment

[0059] A2.1 Gas Chromatography-Mass Spectrometer: Equipped with an electron impact ionization source (EI source).

[0060] A2.2 Analytical balance: sensitivity 0.1 mg.

[0061] A2.3 Ultrasonic generator: frequency 40kHz.

[0062] A2.4 Vacuum rotary evaporator.

[0063] A2.5 Centrifuge tubes: 50mL, polypropylene.

[0064] A2.6, Heart-shaped bottle: 150mL.

[0065] A2.7 Disposable syringe: 2mL.

[0066] A2.8 Organic microporous filter membrane: Nylon, 0.22μm.

[0067] B1. Sample Preparation

[0068] Take 5.0g~10.0g of textiles as a representative sample, cut the textiles into pieces with a size of less than 5mm×5mm, and that is the sample.

[0069] C1, Extraction

[0070] Accurately weigh 1 g (accurate to 0.01 g) of the sample obtained in step B into a 50 mL centrifuge tube, add 20-30 mL of acetonitrile until the sample is completely submerged, and place the centrifuge tube in an ultrasonic generator at 60 °C for 30 min. After standing, remove all the extract, and then add another 20-30 mL of acetonitrile to the centrifuge tube for a second extraction of the sample residue. Combine the two extracts in a pistol flask, rotary evaporate at least 1 mL, purge with nitrogen until the solvent is basically removed, add 1 mL of acetonitrile to make up to volume, and use a disposable syringe to extract and filter through a 0.22 µm microporous membrane to obtain the extract to be tested.

[0071] D. Gas Chromatography-Mass Spectrometry (GC-MS): The extract to be tested is analyzed using a gas chromatograph-mass spectrometer. A certain amount of the standard working solution prepared in step A is placed into the GC-MS instrument to prepare a working curve. The extract to be tested, prepared in step C, is then placed into the GC-MS instrument for analysis to obtain the content of perfluorinated and polyfluorinated compounds in the sample. The specific operation method is as follows:

[0072] D1. In the same batch of standard working solutions prepared in step A1.6, standard working solutions of different concentrations are sequentially injected into a gas chromatograph-mass spectrometer for detection to obtain chromatograms of the content of perfluorinated and polyfluorinated compounds in each concentration of standard working solutions. Subsequently, based on the peak data of each detection peak in the chromatogram, a standard curve is established with concentration as the abscissa (X-axis) and peak area (or peak height) as the ordinate (Y-axis). The curve equation is: y=ax+b;

[0073] D2. Under identical gas chromatography-mass spectrometry (GC-MS) conditions, the sample to be tested is injected into the GC-MS instrument for detection. The chromatogram of the content of perfluorinated and polyfluorinated compounds in the sample to be tested is obtained. The chromatogram shows the peak data (peak area or peak height) of perfluorinated and polyfluorinated compounds in the sample to be tested.

[0074] D3. Substitute the peak data (peak area or peak height) of perfluorinated and polyfluorinated compounds obtained from the chromatogram in step D2 into the equation y=ax+b of the standard curve to calculate the accurate concentration of the target (perfluorinated and polyfluorinated compounds) in the extract to be tested, and finally achieve the purpose of obtaining the content of perfluorinated and polyfluorinated compounds in the sample to be tested.

[0075] D4. In the detection of the extract to be tested in step D2, multiple peaks may appear, representing different perfluorinated and polyfluorinated compounds. By comparing the peak retention time and mass spectrometry information, the specific substance can be determined. Then, the content can be determined by comparing it with the peak area and standard curve in step D2.

[0076] D5. Gas chromatography-mass spectrometry determination shall be performed under the following conditions:

[0077] a) Chromatographic column: DB-5MS capillary column (30m×0.25mm×0.25µm) or its equivalent; it should be noted that when determining fluoropolymers (FTOHs), fluoropolymer polyacrylates (FTAs), perfluorooctyl sulfonamides (FOSAs), and perfluorooctyl sulfonamide ethanol (FOSEs), the determination conditions in steps b to i remain unchanged, and step a uses a DB-5 (30m×0.25mm×0.25µm) chromatographic column for separation;

[0078] b) The heating program is as follows: Initial temperature 40℃, hold for 0 min, increase to 100℃ at 5℃ / min, hold for 0 min, then rapidly increase to 280℃ at 20℃ / min, hold for 3 min;

[0079] c) Carrier gas: Helium, purity ≥ 99.999%, flow rate 1.2 mL / min;

[0080] d) Inlet temperature: 280℃;

[0081] e) Injection volume: 1 μL;

[0082] f) Mass spectrometry interface temperature: 260℃;

[0083] g) Ion source: Electron impact ionization source (EI), temperature 250℃;

[0084] h) Transmission line temperature: 280℃;

[0085] i) Detection method: Select Ion Scan (SIM) mode.

[0086] Optimization of chromatographic conditions

[0087] The detection method of this invention involves 12 volatile perfluorinated and polyfluorinated compounds, including fluoropolymers (FTOHs), fluoropolymer polyacrylates (FTAs), perfluorooctyl sulfonamides (FOSAs), and perfluorooctyl sulfonamide ethanol (FOSEs). These compounds exhibit significant differences in LogP values, boiling points, and polarities. Therefore, a chromatographic column with a wider range of applications is required. A comparison of DB-5, DB-35, and DB-WAX columns revealed that DB-5 effectively separated all 12 target compounds, producing sharp and symmetrical peaks, significantly superior to the other two columns. Therefore, the DB-5 column (30 m × 0.25 mm × 0.25 µm) was selected for separation. Figure 1 The SIM spectrum is obtained under established conditions from a mixed standard solution of 12 volatile perfluorinated and polyfluorinated compounds.

[0088] Optimization of mass spectrometry conditions

[0089] This standard uses a single quadrupole mass spectrometer as the detector to detect 12 volatile perfluorinated and polyfluorinated compounds in electron impact ionization (EI) mode. Each target compound showed a good response. The 12 target compounds were measured in full-scan SCAN mode, and the characteristic ions of each compound were identified. In the fragmentation fragments of perfluorinated and polyfluorinated compounds, characteristic ions with lower mass-to-charge ratios showed higher responses. Furthermore, due to the similar chemical structures of the target compounds, the same characteristic ion fragments, such as 69, 55, and 99 m / z ions, are easily generated under the same bombardment energy. Therefore, most perfluorinated and polyfluorinated compounds share the same characteristic ion fragments. Specific parameters are shown in Table 2.

[0090] Table 2. Mass Spectrometry Conditions for 12 Perfluorinated and Polyfluorinated Compounds

[0091]

[0092] like Figure 2 , 3 As shown, the volume-fixing solvent has a significant impact on the response and peak shape of the target compounds. This method compares four solvents: methanol, acetonitrile, ethyl acetate, and n-hexane. When methanol is used as the volume-fixing solvent, some target compounds exhibit significant tailing of peaks, resulting in poor separation and making it unsuitable as a volume-fixing solvent. When ethyl acetate and n-hexane are used as volume-fixing solvents, obvious impurity peaks appear in the spectrum, and there are very high solvent peaks before 4 min, which severely interfere with the early-eluting 4:2FTOH compounds (RT: 3.12 min). Even SIM-selective ionization cannot eliminate this interference, making them unsuitable as volume-fixing solvents. In contrast, the detection method of this invention uses acetonitrile as the volume-fixing solvent, resulting in high target analyte response, sharp and symmetrical peak shapes, high separation, more accurate qualitative and quantitative analysis, and higher extraction efficiency. It eliminates the drawbacks of methanol, ethyl acetate, and n-hexane detection, making it a very suitable volume-fixing solvent.

Claims

1. A method for detecting the content of perfluorinated and polyfluorinated compounds in textiles, comprising sample preparation, extraction, and determination steps, characterized in that, The specific steps are as follows: A. Reagent preparation: Weigh a certain amount of each perfluorinated and polyfluorinated compound standard to prepare an independent standard stock solution (1000 mg / L). Then, mix the independent standard stock solutions together to prepare a mixed standard intermediate solution (50 mg / L). Finally, prepare standard working solutions of different concentrations (0.01 mg / L-25 mg / L) from the mixed standard intermediate solution for later use. B. Sample preparation: Take a certain weight of textile and cut it into pieces. The size of the pieces should be less than 5mm×5mm to obtain the sample. C. Extraction: Take a certain amount of the sample obtained in step B into a container, add a certain amount of acetonitrile to the container to completely submerge the sample; place the container containing the sample in the extraction device, and extract at an extraction temperature of 40~80℃ for 10~60min, and separate to obtain the extract. Then add a certain amount of acetonitrile to the same container to extract and separate the same sample. Repeat this operation to extract the same sample 1~3 times, and obtain the extracts separately. Then combine the extracts obtained from each extraction. The combined extract is dried by rotary evaporation and nitrogen blowing, diluted with acetonitrile, and filtered to obtain the extract to be tested. D. Gas Chromatography-Mass Spectrometry: Take a certain amount of the standard working solution prepared in step A and put it into the gas chromatograph-mass spectrometer for detection. Prepare a working curve based on the data of the detection chromatogram. Put the test extract prepared in step C into the gas chromatograph-mass spectrometer for detection. Then compare the data of the detection chromatogram of the test extract with the working curve to obtain the content of perfluorinated and polyfluorinated compounds in the test sample.

2. The method for detecting the content of perfluorinated and polyfluorinated compounds in textiles according to claim 1, characterized in that, The phase chromatography-mass spectrometry determination conditions are as follows: a) Chromatographic column: DB-5MS capillary column (30m×0.25mm×0.25µm) or its equivalent; b) The heating program is as follows: initial temperature 40℃ (hold for 0 min), increase to 100℃ at 5℃ / min (hold for 0 min), and then rapidly increase to 280℃ at 20℃ / min (hold for 3 min). c) Carrier gas: Helium, purity ≥ 99.999%, flow rate 1.2 mL / min; d) Inlet temperature: 280℃; e) Injection volume: 1 μL; f) Mass spectrometry interface temperature: 260℃; g) Ion source: Electron impact ionization source (EI), temperature 250℃; h) Transmission line temperature: 280℃; i) Detection method: Select Ion Scan (SIM) mode.

3. The method for detecting the content of perfluorinated and polyfluorinated compounds in textiles according to claim 1, characterized in that, The perfluorinated and polyfluorinated compounds include at least one of fluorinated telomer alcohols, fluorinated acrylates, and perfluorooctane sulfonamides, wherein, The fluorinated telomer alcohol includes at least one of 1H,1H,2H,2H-perfluorohexanol, 1H,1H,2H,2H-perfluorooctanol, 1H,1H,2H,2H-perfluorodecanol, and 1H,1H,2H,2H-perfluorododecylol. The fluorinated acrylates include at least one of 1H,1H,2H,2H-perfluorohexanol acrylate, 1H,1H,2H,2H-perfluorooctanol acrylate, and 1H,1H,2H,2H-perfluorododecyl acrylate. The perfluorooctane sulfonamide compounds include at least one of N-methylperfluorooctane sulfonamide ethanol, N-ethylperfluorooctane sulfonamide ethanol, perfluorooctane sulfonamide, perfluoro-N-methyloctane sulfonamide, and perfluoro-N-ethyloctane sulfonamide.

4. The method for detecting the content of perfluorinated and polyfluorinated compounds in textiles according to claim 1, characterized in that, The fluoropolymers, including fluoropolymers (FTOHs), fluoropolymers (FTAs), perfluorooctylsulfonamides (FOSAs), and perfluorooctylsulfonamide ethanol (FOSEs), were separated using a DB-5 (30m × 0.25mm × 0.25µm) chromatographic column.

5. The method for detecting the content of perfluorinated and polyfluorinated compounds in textiles according to claim 1, characterized in that, Preparation of the standard stock solution (1000 mg / L): Accurately weigh 0.025 g (accurate to 0.1 mg) of each perfluorinated and polyfluorinated compound standard, place them in 25 mL volumetric flasks respectively, dilute to the mark with methanol, mix well, and store in brown stock bottles; Preparation of the mixed standard intermediate solution (50 mg / L): Accurately transfer 1.25 mL of each standard stock solution into a 25 mL volumetric flask, dilute to the mark with acetonitrile, mix well, and store in a brown storage bottle; Preparation of the standard working solution (0.01 mg / L-25 mg / L): As needed, accurately transfer a certain volume of the mixed standard intermediate solution, dilute it with acetonitrile to form a mixed standard working solution, mix well, and store in a brown storage bottle.

6. The method for detecting the content of perfluorinated and polyfluorinated compounds in textiles according to claim 1, characterized in that: In step A, the standard working solution is prepared as follows: a certain volume of mixed standard intermediate solution is accurately transferred and diluted with acetonitrile to obtain standard working solutions with concentrations of 0.01 mg / L and 25 mg / L, respectively. Then, within the concentration range of 0.01 mg / L to 25 mg / L, using the same acetonitrile dilution method, a certain volume of mixed standard intermediate solution is taken to prepare several standard working solutions with different concentration values, which are stored in brown storage bottles for later use. For ease of calculation, the subsequent concentration value is set to be n times the previous concentration value, where n is 5, 10, 15, 20, or other values ​​that are easy to calculate. However, in the same batch of standard working solutions, the multiple n between adjacent concentration values ​​is the same fixed value.

7. The method for detecting the content of perfluorinated and polyfluorinated compounds in textiles according to claim 1, characterized in that, During each extraction operation in step C, 20-30 ml of acetonitrile is added to each gram (g) of sample.

8. The method for detecting the content of perfluorinated and polyfluorinated compounds in textiles according to claim 1, characterized in that, In step C, when making up the volume, the volume ratio of the extract to acetonitrile is 0.8 to 1:

1.

9. The method for detecting the content of perfluorinated and polyfluorinated compounds in textiles according to claim 1, characterized in that, In step C, a microporous membrane is used for filtration, and the pore size of the microporous membrane is less than 0.22µm.

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