Method for determining tetra-pscas in consumer goods

Abstract

The application provides a method for determining Tetra-PSCA in daily consumer goods, comprising the following steps: sampling; adding a first volume of a first reagent into 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 into the extraction solution, and performing multiple washing and purification treatments on the extraction solution, then diluting and filtering the treated extraction solution to obtain a test solution for machine; and placing the test solution for machine into a liquid chromatograph tandem mass spectrometer for qualitative and quantitative detection analysis. According to the material structure composition of Tetra-PSCA, the corresponding pretreatment is performed, then the liquid chromatograph tandem mass spectrometer is used for qualitative and quantitative analysis, the conditions and parameters of the method are optimized, the content of Tetra-PSCA in daily consumer goods can be accurately determined, the blank of the national standard method is filled, the detection limit of the method is low, the operation is simple, the used equipment is easy to obtain, and the method is extremely popular.

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 Tetra-PSCA in consumer products. Background Technology

[0002] N-(5-Carboxypentyl)-Dodecenylsuccinamide (Tetra-PSCA) is a surfactant that is often added to fuels as an anti-corrosion agent in industry, and can also be used in other applications that require surfactants.

[0003] Recent studies have shown that such substances may pose certain health hazards to humans, causing negative effects such as neurotoxicity, reproductive toxicity, and developmental toxicity. Currently, various countries have regulations governing compounds with similar structures. Tetra-PSCA, as an emerging hazardous chemical, was officially added to the EU's SVHC (Substances of Very High Concern) list in January 2025, indicating that this substance may be subject to regulation by more countries and regions in the future.

[0004] However, there is currently no reliable method for determining the content of Tetra-PSCA in consumer products. Summary of the Invention

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

[0006] A method for determining Tetra-PSCA in a consumer product includes 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 extract is washed and purified multiple times. The treated extract is then diluted and filtered to obtain the test solution for use.

[0010] The test solution was placed in a liquid chromatography-tandem mass spectrometer for qualitative and quantitative detection and analysis;

[0011] The analytical parameters of the liquid chromatography-tandem mass spectrometry include:

[0012] ESI negative ion mode;

[0013] Chromatographic column: C18, 150 mm column length × 2.1 mm inner diameter × 3.5 μm particle size;

[0014] Injection volume: 1 μL;

[0015] Eluent: A: 5 mmol / L ammonium acetate aqueous solution, B: acetonitrile;

[0016] Gradient rinsing procedure:

[0017] 0-3min, 300μL / min, 80%A, 20%B;

[0018] 3-7min, 300μL / min, 80%A, 20%B;

[0019] 7-12min, 300μL / min, 10%A, 90%B;

[0020] 12-12.5min, 300μL / min, 10%A, 90%B;

[0021] 12.5-17min, 300μL / min, 80%A, 20%B;

[0022] SIM ion parameters:

[0023] Tetra-PSCA P1: Mother ion 378.4, daughter ion 264.2, declustering voltage -34, collision energy -80;

[0024] Tetra-PSCA P2: Mother ion 378.4, daughter ion 211.1, declustering voltage -34, collision energy -80.

[0025] Furthermore, the sampling step includes:

[0026] Cut the sample into small pieces and weigh 1g ± 0.05g of the homogenized sample into a test tube.

[0027] Further, the step of adding a second volume of the second reagent to the extract, washing and purifying the extract multiple times, and then diluting and filtering the treated extract to obtain the test solution includes:

[0028] Add a second volume of the second reagent to the extract, vortex for a second specified time, let stand for a third specified time, and then pour the supernatant into a flask;

[0029] The test tube is rinsed with a third volume of the third reagent in multiple portions, and then allowed to stand for a third specified time. The supernatant is then poured into the flask.

[0030] The solution in the flask was rotary evaporated to dryness, and a fourth volume of the fourth reagent was added to the flask. After rinsing the flask several times, the solution was removed and diluted 10 times with water.

[0031] Filter to obtain the test solution for use.

[0032] Furthermore, the first reagent is tetrahydrofuran.

[0033] Furthermore, both the second reagent and the third reagent are n-hexane.

[0034] Furthermore, the fourth reagent is a 0.01 mol / L sodium carbonate solution.

[0035] Furthermore, the first volume is 10ml ± 0.1ml, the first specified temperature is 65℃-75℃, and the first specified time is 28min-32min.

[0036] Furthermore, the second volume is 20 ml, the second specified time is 30 ± 2 s, and the third specified time is 28 min - 32 min.

[0037] Furthermore, the third volume is 15 ml.

[0038] Furthermore, the fourth volume is 10 ml ± 0.1 ml.

[0039] This application has the following advantages:

[0040] In the embodiments of this application, a gap in the prior art regarding the determination of Tetra-PSCA in consumer products is filled. A method for determining Tetra-PSCA in consumer products includes the following steps: sampling; adding a first volume of a first reagent to the sample and sonicating it 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 performing multiple washing and purification treatments on the extract; then diluting and filtering the treated extract to obtain a test solution; and placing the test solution in a liquid chromatography-tandem mass spectrometry (LC-MS / MS) instrument for qualitative and quantitative analysis. The analytical parameters of the LC-MS / MS instrument include: ESI negative ion mode... Formula; Column: C18, 150 mm column length × 2.1 mm inner diameter × 3.5 μm particle size; Injection volume: 1 μL; Eluent: A: 5 mmol / L ammonium acetate aqueous solution, B: acetonitrile; Gradient elution program: 0-3 min, 300 μL / min, 80% A, 20% B; 3-7 min, 300 μL / min, 80% A, 20% B; 7-12 min, 300 μL / min, 10% A, 90% B; 12-12.5 min, 300 μL / min, 10% A, 90% B; 12.5-17 min, 300 μL / min, 80% A, 20% B; SIM ion parameters: Tetra-PSCA P1: Mother ion 378.4, daughter ion 264.2, declustering voltage -34, collision energy -80; Tetra-PSCA P2: Mother ion 378.4, daughter ion 211.1, declustering voltage -34, collision energy -80. Based on the material structure and composition of Tetra-PSCA, this application pre-processes it and uses liquid chromatography-tandem mass spectrometry for qualitative and quantitative analysis. The optimized method conditions and parameters enable accurate determination of the Tetra-PSCA content in consumer products, filling a gap in national standard methods. The method has a low detection limit, is simple to operate, and uses readily available equipment, making it highly scalable. Attached Figure Description

[0041] 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.

[0042] Figure 1 This is a flowchart illustrating the steps of a method for determining Tetra-PSCA in consumer products according to an embodiment of this application.

[0043] Figure 2 This is a chromatogram of Tetra-PSCA provided in the embodiments of this application. Detailed Implementation

[0044] 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.

[0045] Reference Figure 1 The diagram shows a flowchart of the steps for determining Tetra-PSCA in a consumer product according to an embodiment of this application.

[0046] The detection method includes:

[0047] S110, Sampling;

[0048] 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;

[0049] S130. Add a second volume of the second reagent to the extract, and wash and purify the extract multiple times. Then dilute and filter the treated extract to obtain the test solution for use.

[0050] S140. Place the test solution into a liquid chromatography-tandem mass spectrometer for qualitative and quantitative detection and analysis.

[0051] The analytical parameters of the liquid chromatography-tandem mass spectrometry include:

[0052] ESI negative ion mode;

[0053] Chromatographic column: C18, 150 mm column length × 2.1 mm inner diameter × 3.5 μm particle size;

[0054] Injection volume: 1 μL;

[0055] Eluent: A: 5 mmol / L ammonium acetate aqueous solution, B: acetonitrile;

[0056] Gradient rinsing procedure:

[0057] 0-3min, 300μL / min, 80%A, 20%B;

[0058] 3-7min, 300μL / min, 80%A, 20%B;

[0059] 7-12min, 300μL / min, 10%A, 90%B;

[0060] 12-12.5min, 300μL / min, 10%A, 90%B;

[0061] 12.5-17min, 300μL / min, 80%A, 20%B;

[0062] SIM ion parameters:

[0063] Tetra-PSCA P1: Mother ion 378.4, daughter ion 264.2, declustering voltage -34, collision energy -80;

[0064] Tetra-PSCA P2: Mother ion 378.4, daughter ion 211.1, declustering voltage -34, collision energy -80.

[0065] In the embodiments of this application, a gap in the prior art regarding the determination of Tetra-PSCA in consumer products is filled. A method for determining Tetra-PSCA in consumer products includes the following steps: sampling; adding a first volume of a first reagent to the sample and sonicating it 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 performing multiple washing and purification treatments on the extract; then diluting and filtering the treated extract to obtain a test solution; and placing the test solution in a liquid chromatography-tandem mass spectrometry (LC-MS / MS) instrument for qualitative and quantitative analysis. The analytical parameters of the LC-MS / MS instrument include: ESI negative ion mode... Formula; Column: C18, 150 mm column length × 2.1 mm inner diameter × 3.5 μm particle size; Injection volume: 1 μL; Eluent: A: 5 mmol / L ammonium acetate aqueous solution, B: acetonitrile; Gradient elution program: 0-3 min, 300 μL / min, 80% A, 20% B; 3-7 min, 300 μL / min, 80% A, 20% B; 7-12 min, 300 μL / min, 10% A, 90% B; 12-12.5 min, 300 μL / min, 10% A, 90% B; 12.5-17 min, 300 μL / min, 80% A, 20% B; SIM ion parameters: Tetra-PSCA P1: Mother ion 378.4, daughter ion 264.2, declustering voltage -34, collision energy -80; Tetra-PSCA P2: Mother ion 378.4, daughter ion 211.1, declustering voltage -34, collision energy -80. Based on the material structure and composition of Tetra-PSCA, this application pre-processes it and uses liquid chromatography-tandem mass spectrometry for qualitative and quantitative analysis. The optimized method conditions and parameters enable accurate determination of the Tetra-PSCA content in consumer products, filling a gap in national standard methods. The method has a low detection limit, is simple to operate, and uses readily available equipment, making it highly scalable.

[0066] The following will further describe a method for determining Tetra-PSCA in a consumer product according to an exemplary embodiment.

[0067] 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.

[0068] 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.

[0069] 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.

[0070] 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.

[0071] 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.

[0072] Tetrahydrofuran has good swelling or dissolving ability for most plastics and textiles, and the Tetra-PSCA of this application is easily soluble in tetrahydrofuran. Therefore, using tetrahydrofuran as a solvent for the sample to be tested can better dissolve Tetra-PSCA, improve the sample extraction efficiency and extraction rate, and thus improve the accuracy of the test results.

[0073] As described in step S130, a second volume of the second reagent is added to the extract, and the extract is washed and purified multiple times. Then, the treated extract is diluted and filtered to obtain the test solution for use.

[0074] Specifically, the process includes: adding a second volume of a second reagent to the extract, vortexing for a second specified time, allowing it to stand for a third specified time, and then pouring the supernatant into a flask; adding a third volume of a third reagent to the test tube in multiple portions, rinsing the test tube, allowing it to stand for a third specified time, and then pouring the supernatant into the flask; rotary evaporating the solution in the flask to dryness, adding a fourth volume of a fourth reagent to the flask, rinsing the flask several times, removing the solution, and diluting it 10 times with water; filtering to obtain the test solution for instrumentation.

[0075] In this embodiment, the second and third reagents are both n-hexane; the fourth reagent is a 0.01 mol / L sodium carbonate solution; the first volume is 10 ml ± 0.1 ml, the first specified temperature is 65℃-75℃, and the first specified time is 28 min-32 min; the second volume is 20 ml, the second specified time is 30 ± 2 s, and the third specified time is 28 min-32 min; the third volume is 15 ml; and the fourth volume is 10 ml ± 0.1 ml.

[0076] As an example, add 20 mL of n-hexane to a test tube containing the extract, vortex for 30 seconds, and then let stand for 30 minutes. Pour the supernatant into a round-bottom flask, add 15 mL of n-hexane to the test tube in three portions, rinse the test tube and residue, and let stand before pouring the supernatant into the round-bottom flask. After completion, rotary evaporate the solution in the flask to dryness. Finally, add 10 mL of 0.01 mol / L sodium carbonate solution to the flask, rinse the flask walls several times, remove the solution, dilute it 10 times with water, filter, and obtain the test solution for instrumentation.

[0077] Tetra-PSCA is soluble in both hexane and dilute alkaline solutions. Purification by adding hexane for precipitation, followed by multiple washes with hexane and sodium carbonate solutions, effectively removes dissolved consumer product matrices such as plastics and textile matrices from tetrahydrofuran without significantly affecting Tetra-PSCA. This prevents polymers from entering instruments, protecting them. Furthermore, filtration improves the purity of the test solution, preventing contamination and enhancing detection accuracy.

[0078] As described in step S140, the test solution is placed in a liquid chromatography-tandem mass spectrometer for qualitative and quantitative detection and analysis.

[0079] The analytical parameters of the liquid chromatography-tandem mass spectrometry include:

[0080] ESI negative ion mode;

[0081] Chromatographic column: C18, 150 mm column length × 2.1 mm inner diameter × 3.5 μm particle size;

[0082] Injection volume: 1 μL;

[0083] Eluent: A: 5 mmol / L ammonium acetate aqueous solution, B: acetonitrile;

[0084] Gradient rinsing procedure:

[0085] 0-3min, 300μL / min, 80%A, 20%B;

[0086] 3-7min, 300μL / min, 80%A, 20%B;

[0087] 7-12min, 300μL / min, 10%A, 90%B;

[0088] 12-12.5min, 300μL / min, 10%A, 90%B;

[0089] 12.5-17min, 300μL / min, 80%A, 20%B;

[0090] SIM ion parameters:

[0091] Tetra-PSCA P1: Mother ion 378.4, daughter ion 264.2, declustering voltage -34, collision energy -80;

[0092] Tetra-PSCA P2: Mother ion 378.4, daughter ion 211.1, declustering voltage -34, collision energy -80.

[0093] By setting the analytical parameters optimized through independent experiments, the Tetra-PSCA content can be accurately determined with high sensitivity, strong anti-interference ability, and simple operation.

[0094] The following are embodiments of the present invention:

[0095] Example

[0096] 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.

[0097] 1: Sample Description: Coating

[0098] 2: Spiking process:

[0099] Take 1 g ± 0.01 g of the sample, cut it into small pieces, and weigh it into a test tube. Add 150 μL of 1000 mg / L Tetra-PSCA standard stock solution. Then add 10 mL of tetrahydrofuran to the test tube, and extract with ultrasound at 70°C for 30 minutes. Add 20 mL of n-hexane, vortex for 30 seconds, and let stand for 30 minutes. Pour the supernatant into a round-bottom flask. Add 15 mL of n-hexane to the test tube in three portions, rinse the test tube and residue, and let stand. Pour the supernatant into the round-bottom flask. After completion, rotary evaporate the solution in the flask to dryness. Finally, add 10 mL of 0.01 mol / L sodium carbonate solution to the flask, rinse the flask wall several times, remove the solution, dilute it 10 times with water, filter, and qualitatively and quantitatively analyze it using liquid chromatography-tandem mass spectrometry.

[0100] The target peak in the standard curve showed good linearity, with a linear range (mg / L) of 0.05, 0.1, and 0.2; the correlation coefficient R² = 0.995. The limit of detection (LOD) was calculated to be 5 mg / kg based on the linear minimum point, sample amount, extraction volume, and dilution factor, indicating the feasibility of the analytical method. Figure 2 The chromatogram of Tetra-PSCA in this embodiment is shown.

[0101] 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 93%, which is relatively high, indicating that the content of Tetra-PSCA in consumer products can be detected efficiently.

[0102] This application proposes a method to accurately determine the content of Tetra-PSCA in consumer products by treating samples under appropriate conditions and then analyzing and determining its content using liquid chromatography-tandem mass spectrometry (LC-MS-MS). This method aims to mitigate risks in social production and assist related industries in accelerating the process of obtaining international market access.

[0103] 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.

[0104] 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.

[0105] The above provides a detailed description of a method for determining Tetra-PSCA 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 core ideas of this application. 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 Tetra-PSCA 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. Add a second volume of a second reagent to the extract, and wash and purify the extract multiple times. Then dilute and filter the treated extract to obtain a test solution for use. The process includes: adding a second volume of a second reagent to the extract, vortexing for a second specified time, allowing it to stand for a third specified time, and then pouring the supernatant into a flask; adding a third volume of a third reagent to the test tube multiple times, rinsing the test tube, allowing it to stand for a third specified time, and then pouring the supernatant into the flask; rotary evaporating the solution in the flask to dryness, adding a fourth volume of a fourth reagent to the flask, rinsing the flask several times, removing the solution, and diluting it 10 times with water; filtering to obtain the test solution for use. The test solution was placed in a liquid chromatography-tandem mass spectrometer for qualitative and quantitative detection and analysis; Wherein, the first reagent is tetrahydrofuran; the second and third reagents are both n-hexane; and the fourth reagent is a 0.01 mol / L sodium carbonate solution. The analytical parameters of the liquid chromatography-tandem mass spectrometry include: ESI negative ion mode; Chromatographic column: C18, 150 mm column length × 2.1 mm inner diameter × 3.5 μm particle size; Injection volume: 1 μL; Eluent: A: 5 mmol / L ammonium acetate aqueous solution; B: acetonitrile; Gradient rinsing procedure: 0-3min, 300μL / min, 80%A, 20%B; 3-7min, 300μL / min, 80%A, 20%B; 7-12min, 300μL / min, 10%A, 90%B; 12-12.5min, 300μL / min, 10%A, 90%B; 12.5-17min, 300μL / min, 80%A, 20%B; SIM ion parameters: Tetra-PSCA P1: Mother ion 378.4, daughter ion 264.2, declustering voltage -34, collision energy -80; Tetra-PSCA P2: Mother ion 378.4, daughter ion 211.1, declustering voltage -34, collision energy -80.

2. The method for determining Tetra-PSCA 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 Tetra-PSCA in consumer products according to claim 1, characterized in that, The first volume is 10ml ± 0.1ml, the first specified temperature is 65℃-75℃, and the first specified time is 28min-32min.

4. The method for determining Tetra-PSCA in consumer products according to claim 1, characterized in that, The second volume is 20 ml, the second specified time is 30 ± 2 s, and the third specified time is 28 min - 32 min.

5. The method for determining Tetra-PSCA in consumer products according to claim 1, characterized in that, The third volume is 15 ml.

6. The method for determining Tetra-PSCA in consumer products according to claim 5, characterized in that, The fourth volume is 10ml ± 0.1ml.

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