Method for detecting migration volume of organophosphorus flame retardant in consumer goods

Abstract

The invention relates to the field of material science and engineering, aims to overcome the defects in the background technology, and provides a method for detecting the migration volume of an organophosphorus flame retardant in consumer goods, and the method has the characteristics of simple steps, high efficiency, low cost and accurate result. According to the technical scheme, the method for detecting the migration volume of the organophosphorus flame retardant in the consumer goods comprises the following steps: S1) preparing a simulation solution; s2) preparing a mixed standard working solution; s3) migrating the potential organophosphorus flame retardant in the sample to be detected into the mixed standard working solution through pretreatment; the method comprises the following steps of 1, adding a magnetic graphene oxide material to adsorb an organophosphorus flame retardant, 2, taking out the magnetic graphene oxide material through a magnetic field, and eluting the organophosphorus flame retardant from the magnetic graphene oxide material through an eluent, and 3, collecting the eluent, filtering the eluent, and carrying out liquid chromatography-mass spectrometry / mass spectrometry analysis.

Description

Technical Field

[0001] The present invention relates to the field of materials science and engineering, and particularly to a method for detecting the migration amount of organophosphorus flame retardants in consumer products. Background Art

[0002] Organophosphorus flame retardants (OPFRs) are a type of emerging pollutants. As substitutes for brominated flame retardants, they are widely used in materials such as textiles, plastics, electronic devices, furniture, and chemicals to increase the flame resistance and fire resistance of various products. Since OPFRs have neurotoxicity, carcinogenicity, and bioaccumulation, which pose a direct threat to human health and safety, they have attracted great attention worldwide. With the in-depth study of the toxicology and safety assessment of OPFRs, more and more OPFRs have been listed in the scope of prohibited or restricted use, and there have been relevant reports on the detection of OPFRs in food, agricultural products, the atmosphere, water, and soil.

[0003] Currently, the main standards for organophosphorus flame retardants are: SN / T 5317-2021 "Determination of organophosphorus flame retardants in imported and exported leather and its products - Gas chromatography-mass spectrometry", GB / T 36922-2018 "Determination of organophosphorus flame retardant content in toys - Gas chromatography-mass spectrometry", SN / T 3228-2012 "Detection method for organophosphorus flame retardants in imported and exported textiles". There is no analysis standard for the migration amount of organophosphorus flame retardants yet. Using the principle of simulated exposure, studying the migration amount of OPFRs in simulated sweat and simulated saliva has become a research hotspot in recent years. Since simulated sweat and simulated saliva contain a large amount of salts, the immersion liquid obtained from simulated migration cannot be directly analyzed by liquid chromatography-mass spectrometry / mass spectrometry and requires pretreatment such as extraction and concentration. Currently, the commonly used extraction methods include liquid-liquid extraction, solid-phase extraction, headspace solid-phase microextraction, etc. Liquid-liquid extraction and solid-phase extraction consume a large amount of organic reagents, and the target compounds will suffer certain losses during the extraction and concentration processes. Since OPFRs are difficult to escape from simulated sweat and simulated saliva, a good pretreatment enrichment method is extremely important.

[0004] The contents of OPFRs dissolved in simulated sweat and simulated saliva are relatively low, and the target substances need to be enriched before testing. Generally, the method of concentrating the eluate after solid-phase extraction is used for pretreatment. Due to the complex pretreatment steps, the target compounds are prone to loss, and a large amount of simulated sweat and simulated saliva can easily cause clogging of the solid-phase extraction column. Magnetic dispersive solid-phase extraction technology uses magnetic materials as adsorbents, and the adsorbents are evenly dispersed in the sample solution, and the separation of the adsorbent from the sample solution is achieved under the action of an external magnetic field. This technology has the advantages of simple operation, rapidity, good selectivity, and high enrichment rate, overcoming the defects of traditional solid-phase extraction. Magnetic graphene oxide meal material, as a new type of carbon nanomaterial, has both the advantages of high hydrophilicity and good solubility of graphene oxide and the high dispersibility and superparamagnetism of magnetite, and can be used to remove pigments and other organic impurities in the sample extract, with strong adsorption performance, convenient separation, simple operation, stable chemical properties, etc. Magnetic graphene oxide solid-phase extraction directly disperses the magnetic adsorbent in the sample solution using a vortex mixer. After adsorbing impurities, the magnetic adsorbent is quickly separated from the sample solution by an external magnet. Currently, it has been widely used in the fields of enrichment and analysis of food, environment, and biological samples.

[0005] Wang Xi et al. used 0.5% formic acid acetonitrile solution for ultrasonic extraction. The extract was purified by dispersive solid-phase extraction adsorbent (150 mg MgSO4, 50 mg C18, 50 mg PSA, 50 mg GCB), and a detection method for 11 organophosphorus flame retardants in infant rice flour was established. Using EMR-Lipid purifying agent and combining with ultra-high performance liquid chromatography-tandem mass spectrometry technology, a method for simultaneously detecting 11 organophosphorus flame retardants in fish was established. Li Hui et al. used acetone extraction to establish a detection method for 4 organophosphorus flame retardants in coating products. Xu Shanshan et al. used QuEChERS pretreatment method to establish a high performance liquid chromatography-tandem mass spectrometry method for 9 organophosphorus flame retardants in vegetables. Zhang Nan et al. used acetone ultrasonic extraction to establish 9 prohibited organophosphorus flame retardants in textiles. Sun Duozhi used acetone extraction to establish a detection method for 3 organophosphorus flame retardants in children's stroller textiles. Gao Xin et al. used ultrasonic-assisted extraction and combined with high performance liquid chromatography-mass spectrometry technology to establish a detection method for 3 chlorine-based organophosphorus ester flame retardants in toys. Chen Fei established an analytical method for determining 24 organophosphorus flame retardants in automotive interior parts by ultrasonic extraction-high performance liquid chromatography-tandem mass spectrometry. Zheng Lei et al. established a method for determining 10 organophosphorus flame retardants in drinking water by online solid-phase extraction-ultra-high performance liquid chromatography-tandem mass spectrometry. Liu Dan used accelerated solvent extraction method combined with liquid chromatography tandem mass spectrometry to establish a test method for 9 prohibited organophosphorus flame retardants in textiles. Zhang Heng et al. established a method for determining organophosphoric acid esters in surface water by online solid-phase extraction-ultra-high performance liquid chromatography tandem mass spectrometry. Qin Weizhen used ultrasonic-assisted extraction-solid-phase extraction-isotope dilution high performance liquid chromatography tandem mass spectrometry to establish a method for 5 organophosphoric acid ester flame retardants in indoor dust. Lin Chunmei studied the migration amount and migration law of DOPO organophosphorus flame retardant in plastic polymers. To sum up, there is no report on enriching the migration amount of organophosphorus flame retardants in consumer products in simulated sweat and simulated saliva by magnetic graphene oxide materials. Summary of the Invention

[0006] The object of the present invention is to overcome the deficiencies in the above background technology and provide a detection method for the migration amount of organophosphorus flame retardants in consumer products, which should have the characteristics of simple steps, high efficiency, low cost and accurate results.

[0007] The technical solution of the present invention is as follows:

[0008] A detection method for the migration amount of organophosphorus flame retardants in consumer products, comprising the following steps:

[0009] S1) Prepare a simulated solution;

[0010] S2) Prepare a mixed standard working solution;

[0011] S3) Make the potential organophosphorus flame retardants in the sample to be tested migrate into the mixed standard working solution through pretreatment;

[0012] S4) Add magnetic graphene oxide material to adsorb organophosphorus flame retardants;

[0013] S5) Take out the magnetic graphene oxide material through a magnetic field, and elute the organophosphorus flame retardants from the magnetic graphene oxide material with an eluent;

[0014] S6) Collect the eluate and perform liquid chromatography - mass spectrometry / mass spectrometry analysis after filtration.

[0015] In the step S1, the simulation liquid includes simulated sweat and simulated saliva.

[0016] In the step S2, the organophosphorus flame retardants include triethyl phosphate, tris(2-chloroethyl) phosphate, triphenylphosphine oxide, triisopropyl phosphate, tripropyl phosphate, tris(2-chloropropyl) phosphate, (2-chloroethyl)dichloroisopentyl phosphate, bis(2,3-dibromopropyl) phosphate, tris(1,3-dichloro-2-propyl) phosphate, triphenyl phosphate, tris(2,3-dibromopropyl) phosphate, triisobutyl phosphate, diphenylcresyl phosphate, tributyl phosphate, tris(2-butoxyethyl) phosphate, resorcinol tetraphenyl diphosphate, tri-o-cresyl phosphate, tri-m-cresyl phosphate, tert-butylphenyl diphenyl phosphate, 2-ethylhexyl diphenyl phosphate, tri-n-amyl phosphate, bisphenol A bis(diphenyl phosphate), tris(3,5-dimethylphenyl) phosphate, tris(isopropylphenyl) phosphate, phenyl(di-tert-butylphenyl) phosphate, tri-n-hexyl phosphate, tris(2-ethylhexyl) phosphate.

[0017] In the step S3, the pretreatment includes: soaking the sample to be tested in the mixed standard working solution at room temperature, and vortexing during the soaking process to obtain a soaking solution.

[0018] In the step S4, the adsorption time is 20 min, vortexing once every 5 min for 30 s each time.

[0019] In the step S5, the eluent is 0.1% formic acid acetonitrile.

[0020] The chromatographic conditions for the liquid chromatography - mass spectrometry / mass spectrometry analysis in the step S4 include:

[0021] Chromatographic column: T3 column; Column temperature: 40 °C; Injection volume: 5.0 µL; Flow rate: 0.3 mL / min; Mobile phase: A is methanol, B is 0.1% formic acid in water; Gradient elution program: 0 - 0.2 min, 80% B; 0.2 - 2.5 min, 80% - 35% B; 2.5 - 5.5 min, 35% - 30% B; 5.5 - 12.0 min, 30% - 25% B; 12.0 - 20.0 min, 25% - 5% B; 20.0 - 23.0 min, 5% - 0% B; 23.0 - 25.0 min, 0% B; 25.0 - 26.0 min, 0% - 80% B; 26.0 - 28.0 min, 80% B.

[0022] The mass spectrometry conditions for the liquid chromatography - mass spectrometry / mass spectrometry analysis in step S4 include:

[0023] Ion source: Electrospray ionization source; Scanning mode: Positive ion mode; Detection method: Multiple reaction monitoring; Spray voltage: 5500 V; Ion source temperature: 550 °C; Spray gas: 0.385 MPa; Auxiliary heating gas: 0.42 MPa; Curtain gas: 0.21 MPa.

[0024] The beneficial effects of the present invention are:

[0025] (1) Simple pretreatment operation: By utilizing the action of an external magnetic field, the magnetic graphene oxide material can be rapidly separated from the soaking solution and the eluent.

[0026] (2) High enrichment efficiency: Only 20 mg of magnetic graphene oxide material is needed to enrich the organophosphorus flame retardants in the soaking solution.

[0027] (3) Less reagent consumption: Only 2 mL of 0.1% formic acid in acetonitrile is needed during the elution process, and the organophosphorus flame retardants are completely eluted.

[0028] (4) Little loss of target compounds: Due to the simple pretreatment steps and small amount of eluent used, only 2 mL of 0.1% formic acid in acetonitrile can completely elute the organophosphorus flame retardants.

[0029] (5) Accurate quantitative results: Since the content of organophosphorus flame retardants in the soaking solution is enriched and the concentration is greatly increased, the peak area of the quantitative ions is more accurate. Description of the Drawings

[0030] Figure 1 is the chromatogram of organophosphorus flame retardants.

[0031] Description of the Drawings: 1 is triethyl phosphate, 2 is phosphoric acid tri, 3 is triphenylphosphine oxide, 4 is triisopropyl phosphate, 5 is tripropyl phosphate, 6 is tris(2-chloropropyl) phosphate, 7 is (2-chloroethyl)dichloroisopentyl phosphate, 8 is bis(2,3-dibromopropyl) phosphate, 9 is tris(1,3-dichloro-2-propyl) phosphate, 10 is triphenyl phosphate, 11 is tris(2,3-dibromopropyl) phosphate, 12 is triisobutyl phosphate, 13 is diphenylcresyl phosphate, 14 is tributyl phosphate, 15 is tris(2-butoxyethyl) phosphate, 16 is resorcinol tetraphenyl diphosphate, 17 is tri-o-tolyl phosphate, 18 is tri-m-tolyl phosphate, 19 is tert-butylphenyl diphenyl phosphate, 20 is 2-ethylhexyl diphenyl phosphate, 21 is tri-n-pentyl phosphate, 22 is bisphenol A bis(diphenyl phosphate), 23 is tris(3,5-dimethylphenyl) phosphate, 24 is tris(isopropylphenyl) phosphate, 25 is phenyl(di-tert-butylphenyl) phosphate, 26 is tri-n-hexyl phosphate, 27 is tris(2-ethylhexyl) phosphate. Detailed Description of the Invention

[0032] In order to make the objectives, technical solutions and advantages of the present invention more clear and understandable, the present invention will be further described in detail below with reference to the drawings and embodiments. It should be understood that the specific embodiments described herein are only used to explain the present invention and are not used to limit the present invention.

[0033] The present invention has established a method for detecting the migration amounts of 27 organophosphorus flame retardants in consumer products. The sample is soaked in simulated sweat or simulated saliva, and the extract is enriched by magnetic graphene oxide and then eluted with 0.1% formic acid acetonitrile and tested by liquid chromatography-mass spectrometry / mass spectrometry.

[0034] As Figure 1 shown, a method for detecting the migration amounts of organophosphorus flame retardants in consumer products includes the following steps:

[0035] S1) Preparation of the simulated solution

[0036] The simulated solution includes simulated sweat and simulated saliva.

[0037] Preparation of the simulated sweat: Weigh 5.00 g of sodium chloride, 1.00 g of urea and 1.00 g of 90% lactic acid into a beaker, add 900 mL of pure water and stir to dissolve. Adjust the pH to 6.5 with 1% sodium hydroxide solution, and then make up to 1 L with a volumetric flask.

[0038] Preparation of simulated saliva: Weigh 0.17 g of magnesium chloride, 0.15 g of calcium chloride, 0.76 g of dipotassium hydrogen phosphate, 0.53 g of calcium carbonate, 0.33 g of sodium chloride, and 0.75 g of potassium chloride into a beaker, add 900 mL of pure water, stir to dissolve, adjust the pH to 6.8 with 1% hydrochloric acid solution, and then make up the volume to 1 L with a volumetric flask.

[0039] S2) Preparation of mixed standard working solutions

[0040] 1) Preparation of reference substances:

[0041] There are 27 reference substances in total, and the chemical information of the reference substances is shown in Table 1.

[0042] Table 1

[0043]

[0044] 2) Preparation of standard stock solutions

[0045] Accurately weigh 10 mg (accurate to 0.1 mg) of each solid standard of each reference substance, dissolve it in methanol and make up the volume to 10 mL in a volumetric flask, shake well, and prepare standard stock solutions of each reference substance with a concentration of 1 mg / mL (a total of 27 standard stock solutions of reference substances).

[0046] 3) Preparation of mixed standard intermediate solutions:

[0047] Accurately pipette a certain amount of the standard stock solution into a 50 mL volumetric flask, add methanol to make up the volume to the mark, shake well, and dilute it to a certain concentration of mixed standard intermediate solution (the standard stock solutions of 27 reference substances are prepared into one kind of mixed standard intermediate solution).

[0048] Among them: the concentrations of BIS, TDCP, TDBPP, and V6 are 100.0 μg / mL, the concentrations of TCEP, MDPP, TIPPP, and BDP are 50.0 μg / mL, and the concentrations of the remaining compounds are 10.0 μg / mL.

[0049] 4) Preparation of mixed standard working solutions

[0050] Accurately pipette an appropriate amount of the mixed standard intermediate solution, and dilute and prepare mixed standard working solutions with the matrix solutions of simulated sweat and simulated saliva respectively (one kind of mixed standard intermediate solution is prepared into 7 series of mixed standard working solutions).

[0051] Among them, the concentrations of BIS, TDCP, TDBPP, and V6 are 5, 50, 100, 200, 300, 400, 500 μg / L; the concentrations of TCEP, MDPP, TIPPP, and BDP are 2.5, 25, 50, 100, 150, 200, 250 μg / L; and the concentrations of the remaining compounds are 0.5, 5, 10, 20, 30, 40, 50 μg / L.

[0052] S3) Migration

[0053] Through pretreatment, the potential organophosphorus flame retardants in the sample to be tested are migrated into the mixed standard working solution.

[0054] The sample to be tested is a consumer product. In this example, a toy is selected.

[0055] Since there is no relevant standard for the migration of organophosphorus flame retardants in consumer products in simulated sweat and simulated saliva, and the research object is a toy, referring to the standard GB / T 38420-2019 "Determination of bisphenol A migration in toy polycarbonate and polysulfone materials - High performance liquid chromatography - tandem mass spectrometry", for every 1 cm 2 The toy is contacted with 10 mL of the mixed standard working solution for the migration experiment. The toy is cut into small pieces of 1 cm 2 or directly cut into 10 cm 2 .

[0056] Take 10 cm 2 of the toy for soaking. Soak it in the mixed standard working solution at room temperature for 4 h, and vortex it once every 30 min for 30 s each time to obtain the soaking solution.

[0057] S4) Extraction

[0058] Transfer 50 mL of the soaking solution into a glass centrifuge tube, add 20 mg of magnetic graphene oxide material to adsorb the organophosphorus flame retardants, adsorb for 20 min, and vortex once every 5 min for 30 s each time.

[0059] S5) Elution

[0060] Under the action of an external magnetic field, take out the magnetic graphene oxide material and discard the soaking solution. Add 2 mL of 0.1% formic acid acetonitrile, desorb for 20 min, and vortex once every 5 min for 30 s each time to elute the organophosphorus flame retardants from the magnetic graphene oxide material.

[0061] S6) Analysis

[0062] Under the action of an external magnetic field, take out the 0.1% formic acid acetonitrile eluate, filter it through a membrane, and then perform liquid chromatography - mass spectrometry / mass spectrometry analysis.

[0063] 1) Chromatographic conditions:

[0064] Chromatographic column: Atlantis TM T3 (150 mm × 2.1 mm, 3 µm); Column temperature: 40 °C; Injection volume: 5.0 µL; Flow rate: 0.3 mL / min; Mobile phase: A is methanol, B is 0.1% formic acid in water; Gradient elution program: 0 - 0.2 min, 80% B; 0.2 - 2.5 min, 80% - 35% B; 2.5 - 5.5 min, 35% - 30% B; 5.5 - 12.0 min, 30% - 25% B; 12.0 - 20.0 min, 25% - 5% B; 20.0 - 23.0 min, 5% - 0% B; 23.0 - 25.0 min, 0% B; 25.0 - 26.0 min, 0% - 80% B; 26.0 - 28.0 min, 80% B.

[0065] 2) Mass spectrometry conditions

[0066] Ion source: Electrospray ionization source; Scanning mode: Positive ion mode; Detection method: Multiple reaction monitoring (MRM); Spray voltage: 5500 V; Ion source temperature: 550 °C; Spray gas: 0.385 MPa; Auxiliary heating gas: 0.42 MPa; Curtain gas: 0.21 MPa.

[0067] S7) Qualitative and quantitative

[0068] Determine the sample extract (ethyl formate - acetonitrile eluate) and the mixed standard working solution according to the above liquid chromatography - tandem mass spectrometry conditions. If the retention time of the target compound in the sample extract differs from that of the standard by no more than ±2.5%; and the relative abundances of the monitored ions of the analyte in the sample spectrum are compared with those of the corresponding monitored ions in the standard solution with similar concentrations, and the relative abundances of each ion are consistent, and the allowable deviation of the abundance ratio does not exceed the range specified in Table 1, then it can be determined that the corresponding analyte to be measured exists in the sample.

[0069] The maximum allowable deviation of the relative ion abundances for qualitative confirmation is shown in Table 2.

[0070] Table 2

[0071] Relative ion abundance / % ＞50% ＞20%～50% ＞10%～20% ≤10% Allowed relative deviation / % ±20% ±25% ±30% ±50%

[0072] This patent selects matrix external standard method for quantitative detection. Taking the concentration of matrix-matched standard working solution as the abscissa and the peak area of the quantitative ion of various organophosphorus flame retardant compounds as the ordinate, a standard curve is drawn. The concentration of various organophosphorus flame retardant compounds in the sample solution is calculated according to the linear regression equation. The response values of the target substances in the series of standard working solutions and the sample solution should be within the linear range monitored by the instrument. If the response value exceeds the linear range, it needs to be diluted with matrix blank solution and re-injected for analysis.

[0073] From Figure 1 It can be seen that 27 organophosphorus flame retardants are effectively separated, and the detection of 27 organophosphorus flame retardants can be completed simultaneously within 28 minutes.

[0074] The mass spectrometry parameters of 27 organophosphorus flame retardants are shown in Table 3.

[0075] Table 3

[0076]

[0077] Note: *Quantitative ion.

[0078] S8) Blank test:

[0079] Glassware should be used for experiments as much as possible, and chromatographically pure reagents should be used for experiments. Blank experiments should be carried out for each operation to ensure that the blank background value is less than the quantitative limit of the corresponding compound.

[0080] S9) Quantitative limit

[0081] The quantitative limit of this method: 5.0 μg / L for BIS, TDCP, TDBPP, V6; 2.5 μg / L for TCEP, MDPP, TIPPP, BDP; 0.5 μg / L for the remaining compounds.

[0082] The linear range, linear equation, correlation coefficient and quantitative limit of organophosphorus flame retardants are shown in Table 4.

[0083] Table 4

[0084]

[0085] S10) Method recovery rate and method precision

[0086] Mixing standard intermediate solutions with high, medium and low concentration levels are quantitatively added to the sample, and the recovery rate test analysis is carried out according to the above detection steps (Steps S3 - S6). The recovery rate of each organophosphorus flame retardant should be within the range of 80 - 120%.

[0087] The precision of six independent test results obtained by tests that are independently carried out on the same test object by the same operator in the same laboratory using the same equipment and following the same test procedures within a short period of time is less than 10%.

[0088] The spiked recovery rates and relative standard deviation results (n = 6) of organophosphate compounds are shown in Table 5.

[0089] Table 5

[0090]

[0091]

[0092] The embodiments described above have elaborated on the technical solutions of the present invention. It should be understood that the above are only specific embodiments of the present invention and are not used to limit the present invention. Any modifications, supplements, or substitutions in a similar manner within the scope of the principles of the present invention should be included within the protection scope of the present invention.

Claims

1. A method for detecting the migration amount of organophosphorus flame retardants in consumer products, comprising the following steps: S1) Prepare a simulation solution; S2) Prepare a mixed standard working solution; S3) Through pretreatment, the potential organophosphorus flame retardants in the sample to be tested migrate into the mixed standard working solution; S4) Add magnetic graphene oxide material to adsorb organophosphorus flame retardants; S5) Remove the magnetic graphene oxide material through a magnetic field, and elute the organophosphorus flame retardants from the magnetic graphene oxide material with an eluent; S6) Collect the eluate and perform liquid chromatography - mass spectrometry / mass spectrometry analysis after filtration.

2. The detection method for the migration amount of organophosphorus flame retardants in consumer products according to claim 1, wherein: In the step S1, the simulation solution includes simulated sweat and simulated saliva.

3. The detection method for the migration amount of organophosphorus flame retardants in consumer products according to claim 1, characterized in that: In the step S2, the organophosphorus flame retardants include triethyl phosphate, tris(2-chloroethyl) phosphate, triphenylphosphine oxide, triisopropyl phosphate, tripropyl phosphate, tris(2-chloropropyl) phosphate, (2-chloroethyl)dichloroisopentyl phosphate, bis(2,3-dibromopropyl) phosphate, tris(1,3-dichloro-2-propyl) phosphate, triphenyl phosphate, tris(2,3-dibromopropyl) phosphate, triisobutyl phosphate, diphenylcresyl phosphate, tributyl phosphate, tris(2-butoxyethyl) phosphate, resorcinol tetraphenyl diphosphate, tri-o-cresyl phosphate, tri-m-cresyl phosphate, tert-butylphenyl diphenyl phosphate, 2-ethylhexyl diphenyl phosphate, tri-n-pentyl phosphate, bisphenol A bis(diphenyl phosphate), tris(3,5-dimethylphenyl) phosphate, tris(isopropylphenyl) phosphate, phenyl bis(di-tert-butylphenyl) phosphate, tri-n-hexyl phosphate, tris(2-ethylhexyl) phosphate.

4. The detection method for the migration amount of organophosphorus flame retardants in consumer products according to claim 1, wherein: In the step S3, the pretreatment includes: soaking the sample to be tested in the mixed standard working solution at room temperature, and vortexing during the soaking process to obtain a soaking solution.

5. The detection method for the migration amount of organophosphorus flame retardants in consumer products according to claim 1, characterized in that: In the step S4, the adsorption time is 20 min, vortexing once every 5 min, each time for 30 s.

6. The detection method for the migration amount of organophosphorus flame retardants in consumer products according to claim 1, characterized in that: In the step S5, the eluent is 0.1% formic acid acetonitrile.

7. The detection method for the migration amount of organophosphorus flame retardants in consumer products according to claim 1, wherein: The chromatographic conditions for the liquid chromatography - mass spectrometry / mass spectrometry analysis in the step S4 include: Chromatographic column: T3 column; Column temperature: 40 °C; Injection volume: 5.0 µL; Flow rate: 0.3 mL / min; Mobile phase: A is methanol, B is 0.1% formic acid water; Gradient elution program: 0 - 0.2 min, 80% B; 0.2 - 2.5 min, 80% - 35% B; 2.5 - 5.5 min, 35% - 30% B; 5.5 - 12.0 min, 30% - 25% B; 12.0 - 20.0 min, 25% - 5% B; 20.0 - 23.0 min, 5% - 0% B; 23.0 - 25.0 min, 0% B; 25.0 - 26.0 min, 0% - 80% B; 26.0 - 28.0 min, 80% B.

8. The detection method for the migration amount of organophosphorus flame retardants in consumer products according to claim 1, characterized in that: The mass spectrometry conditions for the liquid chromatography - mass spectrometry / mass spectrometry analysis in the step S4 include: Ion source: Electrospray ionization source; Scanning mode: Positive ion mode; Detection method: Multiple reaction monitoring; Spray voltage: 5500 V; Ion source temperature: 550 °C; Spray gas: 0.385 MPa; Auxiliary heating gas: 0.42 MPa; Curtain gas: 0.21 MPa.

Images