Method for determining perfluorotripropylamine in consumer goods

Abstract

The application provides a method for determining perfluorotripropylamine in consumer goods, comprising the steps of: sampling; adding a first volume of a first reagent to the sample and ultrasonicating at a first specified temperature for a first specified time to obtain an extraction solution; adding a second volume of a second reagent to the extraction solution and ultrasonicating at a second specified temperature for a second specified time, and obtaining a machine test solution after filtration; taking a third volume of the machine test solution and placing it in a headspace bottle and sealing it, and then placing the headspace bottle in a headspace-gas chromatography mass spectrometry instrument for qualitative and quantitative detection analysis; wherein the analysis parameters of the headspace-gas chromatography mass spectrometry instrument include: headspace temperature: 90 DEG C; equilibrium time: 30 min; chromatographic column: DB-624; carrier gas flow rate 0.6 ml / min; column oven temperature: 40 DEG C for 3 min; temperature rising at 25 DEG C / min to 240 DEG C, maintaining for 3 min; quantitative ion: 168.9; qualitative ion: 68.9, 213.9. The application optimizes the conditions and parameters of the method, and can accurately determine perfluorotripropylamine in consumer goods.

Description

Technical Field

[0001] This application relates to the field of chemical detection technology for consumer products, and in particular to a method for determining perfluorotripropylamine in consumer products. Background Technology

[0002] Perfluorotripropylamine is a typical perfluoroalkyl compound (PFAS), which can be added to high-performance materials as a surface treatment agent, lubricant, or industrial additive. PFAS compounds are widely used in non-stick coatings, waterproof textiles, fire-fighting foams, and the electronics industry due to their unique chemical stability.

[0003] Recent studies have shown that these substances have extremely high environmental persistence, bioaccumulation, and potential health hazards, potentially causing negative effects on the human body such as thyroid dysfunction, liver toxicity, and immunosuppression. Furthermore, multiple studies have indicated a link between some PFAS substances and cancer risk. Currently, many countries worldwide have implemented strict controls on PFAS substances; for example, the EU's REACH regulation and the US EPA action plan both list them as priority substances for restriction. Notably, perfluorotripropylamine was officially added to the EU's SVHC (Substances of Very High Concern) list in January 2025, becoming one of the regulated PFAS substances. It is foreseeable that this substance will face broader regulatory constraints from various countries and regions in the future.

[0004] However, there is currently no reliable method for determining the residual amount of perfluorotripropylamine in industrial products and environmental media. Summary of the Invention

[0005] In view of the aforementioned problems, this application is made in order to provide a method for determining perfluorotripropylamine in consumer products that overcomes or at least partially solves the aforementioned problems.

[0006] A method for determining perfluorotripropylamine in consumer products, comprising the following steps:

[0007] sampling;

[0008] A first volume of a first reagent is added to the sample, and the sample is sonicated at a first specified temperature for a first specified time to obtain an extract.

[0009] A second volume of the second reagent is added to the extract, and the mixture is sonicated at a second specified temperature for a second specified time. After filtration, the test solution is obtained.

[0010] Take a third volume of the test solution and place it in a headspace vial and seal it. Then place the headspace vial in a headspace-gas chromatography-mass spectrometry instrument for qualitative and quantitative detection and analysis.

[0011] The analytical parameters of the headspace-gas chromatography-mass spectrometry system include:

[0012] Headspace temperature: 90℃; Equilibrium time: 30 min;

[0013] Column: DB-624; Carrier gas flow rate: 0.6 ml / min;

[0014] Column oven temperature: 40℃ for 3 min; increase temperature to 240℃ at 25℃ / min and hold for 3 min;

[0015] Quantitative ions: 168.9; Qualitative ions: 68.9, 213.9.

[0016] Furthermore, the sampling step includes:

[0017] Cut the sample into small pieces and weigh 1g ± 0.05g of the homogenized sample into a test tube.

[0018] Further, the step of adding a second volume of the second reagent to the extract includes:

[0019] First, place the extract in a shaker for 28-32 minutes, then add a second volume of the second reagent to the extract.

[0020] Furthermore, the first volume is 10 ml ± 0.1 ml.

[0021] Furthermore, the second volume is 20 ml.

[0022] Furthermore, both the first specified temperature and the second specified temperature are 65℃-75℃.

[0023] Furthermore, both the first specified time and the second specified time are 28min-32min.

[0024] Furthermore, the first reagent is tetrahydrofuran.

[0025] Furthermore, the second reagent is acetonitrile.

[0026] Furthermore, the third volume is 0.1 ml.

[0027] This application has the following advantages:

[0028] In the embodiments of this application, the gap in the prior art regarding the determination of perfluorotripropylamine in consumer products is filled. A method for determining perfluorotripropylamine in consumer products includes the following steps: sampling; adding a first volume of a first reagent to the sample and sonicating at a first specified temperature for a first specified time to obtain an extract; adding a second volume of a second reagent to the extract and sonicating at a second specified temperature for a second specified time, filtering to obtain a test solution; taking a third volume of the test solution and placing it in a headspace vial and sealing it, then placing the headspace vial in a headspace-gas chromatography-mass spectrometry (GC-MS) instrument for qualitative and quantitative detection and analysis; wherein the analytical parameters of the headspace-gas chromatography-mass spectrometry instrument include: headspace temperature: 90℃; equilibration time: 30min; chromatographic column: DB-624; carrier gas flow rate: 0.6ml / min; column oven temperature: 40℃ held for 3min; temperature increased to 240℃ at 25℃ / min and held for 3min; quantitative ion: 168.9; qualitative ions: 68.9, 213.9. Based on the material structure and composition of perfluorotripropylamine, this application pre-processes it and performs qualitative and quantitative analysis using headspace gas chromatography-mass spectrometry. By optimizing the conditions and parameters of the method, it can accurately determine perfluorotripropylamine in consumer products, filling the gap in national standard methods. The method has a low detection limit, is simple to operate, and the equipment used is readily available, making it highly scalable. Attached Figure Description

[0029] To more clearly illustrate the technical solution of this application, the drawings used in the description of this application will be briefly introduced below. Obviously, the drawings described below are only some embodiments of this application. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0030] Figure 1 This is a flowchart illustrating the steps of a method for determining perfluorotripropylamine in a consumer product according to an embodiment of this application.

[0031] Figure 2 This is a chromatogram of perfluorotripropylamine in selective ion mode provided in the embodiments of this application. Detailed Implementation

[0032] To make the objectives, features, and advantages of this application more apparent and understandable, the application will be further described in detail below with reference to the accompanying drawings and specific embodiments. Obviously, the described embodiments are only some, not all, of the embodiments of this application. All other embodiments obtained by those skilled in the art based on the embodiments of this application without inventive effort are within the scope of protection of this application.

[0033] Reference Figure 1The diagram shows a flowchart of the steps of a method for determining perfluorotripropylamine in a consumer product according to an embodiment of this application.

[0034] The detection method includes:

[0035] S110, Sampling;

[0036] S120. Add a first volume of the first reagent to the sample and sonicate at a first specified temperature for a first specified time to obtain an extract;

[0037] S130. Add a second volume of the second reagent to the extract, sonicate at a second specified temperature for a second specified time, and filter to obtain the test solution for use.

[0038] S140. Take the third volume of the test solution and place it in a headspace vial and seal it. Then place the headspace vial in a headspace-gas chromatography-mass spectrometry instrument for qualitative and quantitative detection and analysis.

[0039] The analytical parameters of the headspace-gas chromatography-mass spectrometry system include:

[0040] Headspace temperature: 90℃; Equilibrium time: 30 min;

[0041] Column: DB-624; Carrier gas flow rate: 0.6 ml / min;

[0042] Column oven temperature: 40℃ for 3 min; increase temperature to 240℃ at 25℃ / min and hold for 3 min;

[0043] Quantitative ions: 168.9; Qualitative ions: 68.9, 213.9.

[0044] In the embodiments of this application, the gap in the prior art regarding the determination of perfluorotripropylamine in consumer products is filled. A method for determining perfluorotripropylamine in consumer products includes the following steps: sampling; adding a first volume of a first reagent to the sample and sonicating at a first specified temperature for a first specified time to obtain an extract; adding a second volume of a second reagent to the extract and sonicating at a second specified temperature for a second specified time, filtering to obtain a test solution; taking a third volume of the test solution and placing it in a headspace vial and sealing it, then placing the headspace vial in a headspace-gas chromatography-mass spectrometry (GC-MS) instrument for qualitative and quantitative detection and analysis; wherein the analytical parameters of the headspace-gas chromatography-mass spectrometry instrument include: headspace temperature: 90℃; equilibration time: 30min; chromatographic column: DB-624; carrier gas flow rate: 0.6ml / min; column oven temperature: 40℃ held for 3min; temperature increased to 240℃ at 25℃ / min and held for 3min; quantitative ion: 168.9; qualitative ions: 68.9, 213.9. Based on the material structure and composition of perfluorotripropylamine, this application pre-processes it and performs qualitative and quantitative analysis using headspace gas chromatography-mass spectrometry. By optimizing the conditions and parameters of the method, it can accurately determine perfluorotripropylamine in consumer products, filling the gap in national standard methods. The method has a low detection limit, is simple to operate, and the equipment used is readily available, making it highly scalable.

[0045] The following will further describe a method for determining perfluorotripropylamine in a consumer product according to an exemplary embodiment of this invention.

[0046] As described in step S110, sampling is generally one of the important steps to extract a small amount of target substance from the target object for testing. It is an effective way to obtain various data from the target object without affecting its main properties. The amount of the analyte extracted needs to be sufficient for 3-5 tests. The sampling area selection process for the analyte during sampling should be random.

[0047] As an example, the sample was cut into small pieces, and 1 g ± 0.05 g of homogenized sample was weighed into a 50 ml test tube.

[0048] As described in step S120, a first volume of a first reagent is added to the sample, and the sample is sonicated at a first specified temperature for a first specified time to obtain an extract. This is equivalent to pretreatment of the sample to be tested. Pretreatment generally involves steps such as purification and decontamination of the target substance before effective processing. In some special experiments, pretreatment steps may also include altering the properties of the substance. In this embodiment, ultrasonic treatment of the sample is preferred.

[0049] In this embodiment, the first reagent is tetrahydrofuran; the first volume is 10ml ± 0.1ml; the ultrasonic extraction conditions are: ultrasonic temperature 65℃-75℃, ultrasonic time 28min-32min.

[0050] As an example, 10 ml of tetrahydrofuran was added to the sample and ultrasonically extracted at 70 °C for 30 min to obtain the extract.

[0051] Tetrahydrofuran has good swelling or dissolving ability for most plastics and textiles, and the perfluorotripropylamine of this application is easily soluble in tetrahydrofuran. Therefore, using tetrahydrofuran as a solvent for the sample to be tested can better dissolve perfluorotripropylamine, which can improve the sample extraction efficiency and extraction rate, thereby improving the accuracy of the test results.

[0052] As described in step S130, a second volume of the second reagent is added to the extract, and the mixture is sonicated at a second specified temperature for a second specified time. After filtration, the test solution is obtained.

[0053] Furthermore, before adding the second reagent, the extract is placed on a shaker and shaken for a certain period of time, preferably 28-32 minutes in this embodiment.

[0054] In this embodiment, the second reagent is acetonitrile; the second volume is 20 ml; the ultrasonic conditions for the second ultrasonic extraction are: ultrasonic temperature 65℃-75℃, ultrasonic time 28 min-32 min.

[0055] As an example, the extract was placed on a shaker for 30 minutes, then 20 ml of acetonitrile was added to the extract, and the mixture was sonicated at 70°C for 30 minutes. The mixture was then filtered to obtain the filtered test solution.

[0056] The extract can be purified by adding acetonitrile. Most polymers are insoluble in acetonitrile, but the perfluorotripropylamine of this application is readily soluble in acetonitrile. Therefore, it can remove dissolved consumer product matrices such as plastic and textile matrices from tetrahydrofuran without significantly affecting the perfluorotripropylamine. This can prevent polymers from entering the instrument and protect the instrument. At the same time, filtration can improve the purity of the test solution and avoid the influence of impurities, thereby improving the accuracy of detection.

[0057] As described in step S140, a third volume of the test solution is placed in a headspace vial and sealed. The headspace vial is then placed in a headspace-gas chromatography-mass spectrometry instrument for qualitative and quantitative analysis. Specifically, the third volume is 0.1 ml.

[0058] The analytical parameters of the headspace-gas chromatography-mass spectrometry system include:

[0059] Headspace temperature: 90℃; Equilibrium time: 30 min;

[0060] Column: DB-624; Carrier gas flow rate: 0.6 ml / min;

[0061] Column oven temperature: 40℃ for 3 min; increase temperature to 240℃ at 25℃ / min and hold for 3 min;

[0062] Quantitative ions: 168.9; Qualitative ions: 68.9, 213.9.

[0063] It should be noted that, due to the very low boiling point of perfluorotripropylamine, headspace gas chromatography-mass spectrometry (HGC-MS) is specifically used for qualitative and quantitative detection and analysis. By setting the analytical parameters optimized through our own experiments, we can avoid the decomposition of perfluorotripropylamine and accurately determine its content. The method is highly sensitive, has strong anti-interference ability, and is simple to operate.

[0064] The following are embodiments of the present invention:

[0065] Example

[0066] By conducting simulation experiments on typical sample materials and adding a quantitative amount of the target analyte to the simulation solution, the corresponding equipment is used for detection and analysis.

[0067] 1: Sample Description: Plastic

[0068] 2: Spiking process:

[0069] Take 1g ± 0.01g of the sample, cut it into small pieces, and put it into a test tube. Add 150μL of 1000mg / L perfluorotripropylamine standard stock solution. Then add 10mL of tetrahydrofuran to the test tube, extract by ultrasonication at 70 degrees for 30 minutes, then shake on a shaker for 30 minutes. Add 20mL of acetonitrile, then sonicate at 70 degrees for 30 minutes. After filtration, take 0.1ml and put it into a headspace vial and seal it. Then use headspace-gas chromatography-mass spectrometry for qualitative and quantitative analysis.

[0070] like Figure 2 The image shows the spectrum of perfluorotripropylamine in selective ion mode in this embodiment. It can be clearly seen that the three characteristic ions at m / z 168.9, m / z 68.9, and m / z 213.9 all exhibit significant chromatographic peaks at 3.365 minutes. The peaks of these three ions are sharp and symmetrical, indicating good chromatographic behavior of the target analyte. In the mass spectrum, the large peak values ​​of the three characteristic ions indicate a high ion current intensity, meaning a large number of ions with that mass-to-charge ratio are formed.

[0071] Meanwhile, the target peak in the standard curve showed good linearity, with a linear range (mg / L) of 0.1, 0.2, 0.5, and 1; the linearity coefficient R0 was [missing value]. 2The linear minimum value was 0.995. The limit of detection was calculated to be 50 mg / kg based on the linear minimum point, sample amount, and extraction volume. All of these values ​​meet the requirements of the EU SVHC regulations, indicating that the assay method is feasible.

[0072] The above spiking process was repeated to conduct six independent standard spiking tests. The average value of the six test data was taken. The results showed that the average recovery rate was 105%, which is relatively high, indicating that the content of perfluorotripropylamine in consumer products can be detected efficiently.

[0073] This application utilizes headspace gas chromatography-mass spectrometry (HCGC-MS) for the qualitative and quantitative detection of perfluorotripropylamine (PFAT) in consumer products. It optimizes the method and analytical parameters, filling a gap in national standard methods. The invented method features a low detection limit, simple operation, and readily available equipment, making it highly scalable. It establishes a highly sensitive analytical method for detecting PFAT residues in industrial products and environmental media, providing forward-looking risk management support for the industry chain and helping companies cope with increasingly stringent global chemical regulations.

[0074] Although preferred embodiments of the present application have been described, those skilled in the art, upon learning the basic inventive concept, can make other changes and modifications to these embodiments. Therefore, the appended claims are intended to be interpreted as including the preferred embodiments as well as all changes and modifications falling within the scope of the embodiments of the present application.

[0075] Finally, it should be noted that in this document, relational terms such as "first" and "second" are used only to distinguish one entity or operation from another, and do not necessarily require or imply any such actual relationship or order between these entities or operations. Furthermore, the terms "comprising," "including," or any other variations thereof are intended to cover non-exclusive inclusion, such that a process, method, article, or terminal device that comprises a list of elements includes not only those elements but also other elements not expressly listed, or elements inherent to such a process, method, article, or terminal device. Without further limitations, an element defined by the phrase "comprising one..." does not exclude the presence of other identical elements in the process, method, article, or terminal device that includes said element.

[0076] The above provides a detailed description of a method for determining perfluorotripropylamine in consumer products. Specific examples have been used to illustrate the principles and implementation methods of this application. The descriptions of the above embodiments are only for the purpose of helping to understand the method and its core ideas. At the same time, those skilled in the art will recognize that there will be changes in the specific implementation methods and application scope based on the ideas of this application. Therefore, the content of this specification should not be construed as a limitation of this application.

Claims

1. A method for determining perfluorotripropylamine in consumer products, characterized in that, Includes the following steps: sampling; A first volume of a first reagent is added to the sample, and the sample is sonicated at a first specified temperature for a first specified time to obtain an extract. A second volume of the second reagent is added to the extract, and the mixture is sonicated at a second specified temperature for a second specified time. After filtration, the test solution is obtained. Take a third volume of the test solution and place it in a headspace vial and seal it. Then place the headspace vial in a headspace-gas chromatography-mass spectrometry instrument for qualitative and quantitative detection and analysis. Wherein, the first volume is 10ml ± 0.1ml; the second volume is 20ml; the third volume is 0.1ml; the first specified temperature and the second specified temperature are both 65℃-75℃; the first specified time and the second specified time are both 28min-32min; the first reagent is tetrahydrofuran; the second reagent is acetonitrile; The analytical parameters of the headspace-gas chromatography-mass spectrometry system include: Headspace temperature: 90℃; Equilibrium time: 30 min; Column: DB-624; Carrier gas flow rate: 0.6 ml / min; Column oven temperature: 40℃ for 3 min; increase temperature to 240℃ at 25℃ / min and hold for 3 min; Quantitative ions: 168.9; Qualitative ions: 68.9, 213.

9.

2. The method for determining perfluorotripropylamine in consumer products according to claim 1, characterized in that, The sampling steps include: Cut the sample into small pieces and weigh 1g ± 0.05g of the homogenized sample into a test tube.

3. The method for determining perfluorotripropylamine in consumer products according to claim 1, characterized in that, The step of adding a second volume of the second reagent to the extract includes: First, place the extract on a shaker and shake for 28-32 minutes, then add a second volume of the second reagent to the extract.

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