A method for detecting the migration of organophosphorus flame retardants in consumer products

Abstract

The present invention relates to the field of materials science and engineering. Its purpose is to overcome the shortcomings of the aforementioned background technology and provide a method for detecting the migration of organophosphorus flame retardants in consumer products. The method should be simple, efficient, low-cost, and accurate. The technical solution of the present invention is: a method for detecting the migration of organophosphorus flame retardants in consumer products, comprising the following steps: S1) preparing a simulated liquid; S2) preparing a mixed standard working solution; S3) pre-treating the sample to allow potential organophosphorus flame retardants to migrate into the mixed standard working solution; S4) adding a magnetic graphene oxide material to adsorb the organophosphorus flame retardant; S5) removing the magnetic graphene oxide material through a magnetic field and eluting the organophosphorus flame retardant from the magnetic graphene oxide material using an eluent; S6) collecting the eluate and filtering it for liquid chromatography-mass spectrometry / mass spectrometry analysis.

Description

Technical Field

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

[0002] Organophosphorus flame retardants (OPFRs) are a new class of pollutants. They are widely used as an alternative to brominated flame retardants in textiles, plastics, electronic devices, furniture, chemicals, and other materials to improve the flame resistance and flame retardancy of various products. Due to their neurotoxicity, carcinogenicity, and bioaccumulation, OPFRs pose a direct threat to human health and safety and have attracted significant attention worldwide. With in-depth research into OPFRs' toxicology and safety assessments, an increasing number of OPFRs have been listed as banned or restricted. OPFRs have been detected in food, agricultural products, air, water, and soil.

[0003] Currently, the main standards for organophosphorus flame retardants include: SN / T 5317-2021 "Determination of organophosphorus flame retardants in imported and exported leather and their products by gas chromatography-mass spectrometry," GB / T 36922-2018 "Determination of organophosphorus flame retardants in toys by gas chromatography-mass spectrometry," and SN / T 3228-2012 "Test method for organophosphorus flame retardants in imported and exported textiles." However, no analytical standard for the migration of organophosphorus flame retardants has yet been established. Studying the migration of OPFRs in simulated sweat and saliva using simulated exposure has become a hot topic in recent years. Because simulated sweat and saliva contain large amounts of salt, the immersion solution obtained from the simulated migration cannot be directly analyzed by liquid chromatography-mass spectrometry / mass spectrometry and requires pretreatment such as extraction and concentration. Commonly used extraction methods include liquid-liquid extraction, solid-phase extraction, and headspace solid-phase microextraction. These extraction methods consume large amounts of organic reagents, resulting in a certain loss of target compounds 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 levels of OPFRs dissolved in simulated sweat and saliva are low, requiring enrichment before testing. This is typically done by concentrating the eluate after solid-phase extraction (SPE). However, due to the complexity of these pretreatment steps, target compounds are easily lost, and large amounts of simulated sweat and saliva can easily clog the SPE cartridges. Magnetic dispersion solid-phase extraction (SPE) uses magnetic materials as adsorbents, which are evenly dispersed in the sample solution. Separation from the sample solution is achieved under the influence of an external magnetic field. This technique offers advantages such as simplicity, rapidity, good selectivity, and high enrichment rates, overcoming the shortcomings of traditional SPE. As a new type of carbon nanomaterial, magnetic graphene oxide meal has the advantages of high hydrophilicity and good solubility of graphene oxide, as well as high dispersibility and superparamagnetism of ferroferric oxide. It can be used to remove pigments and other organic impurities in sample extracts. It has the advantages of strong adsorption performance, convenient separation, simple operation, and stable chemical properties. Magnetic graphene oxide solid-phase extraction uses a vortex mixer to disperse the magnetic adsorbent directly in the sample solution. After adsorbing impurities, the magnetic adsorbent is quickly separated from the sample solution by an external magnet. It is currently widely used in the enrichment and analysis of food, environmental and biological samples.

[0005] Wang Xi et al. developed a method for the detection of 11 organophosphorus flame retardants in infant rice cereal using ultrasonic extraction with 0.5% formic acid in acetonitrile and cleanup of the extract with a dispersive solid-phase extraction adsorbent (150 mg MgSO₄, 50 mg C₁₄, 50 mg PSA, and 50 mg GCB). Using EMR-Lipid cleanup, combined with ultra-high performance liquid chromatography-tandem mass spectrometry, they developed a method for the simultaneous detection of 11 organophosphorus flame retardants in fish. Li Hui et al. developed a method for the detection of four organophosphorus flame retardants in coatings using acetone extraction. Xu Shanshan et al. developed a high-performance liquid chromatography-tandem mass spectrometry method for the detection of nine organophosphorus flame retardants in vegetables using a QuEChERS pretreatment method. Zhang Nan et al. developed a method for the detection of nine banned organophosphorus flame retardants in textiles using acetone ultrasonic extraction. Sun Duozhi developed a method for the detection of three organophosphorus flame retardants in children's stroller textiles using acetone extraction. Gao Xin et al. developed a method for the detection of three chlorinated organophosphorus flame retardants in toys using ultrasound-assisted extraction combined with high-performance liquid chromatography-mass spectrometry. Chen Fei developed a method for the determination of 24 organophosphorus flame retardants in automotive interior parts using ultrasound-assisted extraction-high-performance liquid chromatography-tandem mass spectrometry. Zheng Lei et al. developed a method for the determination of 10 organophosphorus flame retardants in drinking water using online solid-phase extraction-ultra-performance liquid chromatography-tandem mass spectrometry. Liu Dan developed a method for the determination of nine banned organophosphorus flame retardants in textiles using rapid solvent extraction combined with liquid chromatography-tandem mass spectrometry. Zhang Heng et al. developed an online method for the determination of organophosphates in surface water using solid-phase extraction-ultra-performance liquid chromatography-tandem mass spectrometry. Qin Weizhen developed a method for the determination of five organophosphate flame retardants in indoor dust using ultrasound-assisted extraction-solid-phase extraction-isotope dilution high-performance liquid chromatography-tandem mass spectrometry. Lin Chunmei studied the migration and migration patterns of DOPO organophosphorus flame retardants in plastic polymers. In summary, there is currently no report on the use of magnetic graphene oxide materials to enrich the migration of organophosphorus flame retardants in consumer products in simulated sweat and simulated saliva. Summary of the Invention

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

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

[0008] A method for detecting the migration amount of organophosphorus flame retardants in consumer products comprises the following steps:

[0009] S1) Prepare the simulation fluid;

[0010] S2) Prepare mixed standard working solution;

[0011] S3) pre-treating the sample to allow potential organophosphorus flame retardants to migrate into the mixed standard working solution;

[0012] S4) adding a magnetic graphene oxide material to adsorb the organophosphorus flame retardant;

[0013] S5) removing the magnetic graphene oxide material through a magnetic field, and eluting the organophosphorus flame retardant from the magnetic graphene oxide material with an eluent;

[0014] S6) The eluate is collected and filtered before analysis by liquid chromatography-mass spectrometry / mass spectrometry.

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

[0016] In the step S2, the organic phosphorus flame retardant includes triethyl phosphate, tris-, triphenylphosphine oxide, triisopropyl phosphate, tripropyl phosphate, tris(2-chloropropyl) phosphate, (2-chloroethyl) dichloroisopentyl phosphate, di-(2,3-dibromopropyl) phosphate, tris(1,3-dichloro-2-propyl) phosphate, triphenyl phosphate, tris(2,3-dibromopropyl) phosphate, triisobutyl phosphate, diphenylcresyl phosphate, tris(2,3-dibromopropyl) phosphate, tris(1,3-dichloro-2-propyl) ...1,3-dichloro-2-propyl) phosphate, tris(1,3-dichloro-2-propyl) phosphate, tris(1,3-dichloro-2-propyl) phosphate, tris(1,3-dichloro-2-propyl) phosphate, tris(1,3-dichloro-2-propyl) phosphate, tris(1,3-dichloro-2-propyl) phosphate, tris(1,3-dichloro-2-propyl) phosphate, tris(1, n-Butyl 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 bisdiphenyl phosphate, tris(3,5-dimethylphenyl) phosphate, tris(isopropylphenyl) phosphate, phenyl(di-tert-butylphenyl) phosphate, tri-n-hexyl phosphate, tris(2-ethylhexyl) phosphate.

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

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

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

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

[0021] Chromatographic column: T3 column; column temperature: 40 ℃; injection volume: 5.0 μL; flow rate: 0.3 mL / min; mobile phase: A: methanol, B: 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 of the liquid chromatography-mass spectrometry / mass spectrometry analysis in step S4 include:

[0023] Ion source: electrospray ion source; scan mode: positive ion mode; detection method: multiple reaction monitoring; spray voltage: 5500 V; ion source temperature: 550 ℃; 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 pre-treatment operation: By using the effect of an external magnetic field, the magnetic graphene oxide material can be quickly separated from the immersion solution and the elution solution.

[0026] (2) High enrichment efficiency: Only 20 mg of magnetic graphene oxide material can be used to enrich the organophosphorus flame retardant in the immersion solution.

[0027] (3) Small amount of reagents: Only 2 mL of 0.1% formic acid acetonitrile is needed during the elution process, and the organophosphorus flame retardant is completely eluted.

[0028] (4) Small loss of target compounds: Due to the simple pretreatment steps and small amount of eluent, only 2 mL of 0.1% formic acid acetonitrile can achieve complete elution of organophosphorus flame retardants.

[0029] (5) Accurate quantitative results: Since the content of organophosphorus flame retardant in the soaking solution has been enriched, the concentration is greatly increased, making the peak area of the quantitative ion more accurate. BRIEF DESCRIPTION OF THE DRAWINGS

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

[0031] Description of the drawings: 1 is triethyl phosphate, 2 is triphosphate, 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 di-(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 tri-n-butyl phosphate, 15 is phosphoric acid tris(2-butoxyethyl) phosphate, 16 is resorcinol tetraphenyl diphosphate, 17 is tri-o-cresyl phosphate, 18 is tri-m-cresyl phosphate, 19 is tert-butylphenyl diphenyl phosphate, 20 is 2-ethylhexyl diphenyl phosphate, 21 is tri-n-pentyl phosphate, 22 is bisphenol A bisdiphenyl 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, and 27 is tris(2-ethylhexyl) phosphate. DETAILED DESCRIPTION

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

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

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

[0035] S1) Preparation of simulation fluid

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

[0037] Preparation of 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 dilute to 1 L with a volumetric flask.

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

[0039] S2) Prepare mixed standard working solution

[0040] 1) Prepare standard substances:

[0041] There are 27 reference materials in total. The chemical information of the reference materials is shown in Table 1.

[0042] Table 1

[0043]

[0044] 2) Prepare standard stock solution

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

[0046] 3) Prepare mixed standard intermediate solution:

[0047] Accurately transfer a certain amount of standard stock solution to a 50 mL volumetric flask, add methanol to the mark, shake well, and dilute to a mixed standard intermediate solution of a certain concentration (the standard stock solutions of 27 standard substances are configured as a mixed standard intermediate solution).

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

[0049] 4) Prepare mixed standard working solution

[0050] Accurately pipette appropriate amounts of the mixed standard intermediate solution and dilute it with the matrix solutions of simulated sweat and simulated saliva to prepare mixed standard working solutions (one mixed standard intermediate solution is configured into 7 series of mixed standard working solutions).

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

[0052] S3) Migration

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

[0054] The samples to be tested are consumer products, and toys are selected in this embodiment.

[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 toys, the reference standard GB / T 38420-2019 "Determination of the migration of bisphenol A in toy polycarbonate and polysulfone materials by high performance liquid chromatography-tandem mass spectrometry" is used. 2 The toy was exposed to 10 mL of mixed standard working solution for migration test, and the toy was cut into 1 cm 2 Small pieces or cut directly into 10 cm 2 .

[0056] Take 10 cm 2 The toys were immersed in the mixed standard working solution at room temperature for 4 h. During the immersion process, the toys were vortexed once every 30 min for 30 s each time to obtain the immersion solution.

[0057] S4) Extraction

[0058] 50 mL of the soaking solution was transferred to a glass centrifuge tube, and 20 mg of magnetic graphene oxide material was added to adsorb the organophosphorus flame retardant. The adsorption was continued for 20 min, and the mixture was vortexed every 5 min for 30 s each time.

[0059] S5) Elution

[0060] Under the action of an external magnetic field, the magnetic graphene oxide material was removed and the soaking solution was discarded. 2 mL of 0.1% formic acid acetonitrile was added and desorbed for 20 min. The material was vortexed every 5 min for 30 s each time to elute the organophosphorus flame retardant from the magnetic graphene oxide material.

[0061] S6) Analysis

[0062] The 0.1% formic acid-acetonitrile eluate was taken out under the action of an external magnetic field, filtered through a membrane, and then subjected to 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: methanol, B: 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 ion source; scan mode: positive ion mode; detection method: multiple reaction monitoring (MRM); spray voltage: 5500 V; ion source temperature: 550 ℃; spray gas: 0.385 MPa; auxiliary heating gas: 0.42 MPa; curtain gas: 0.21 MPa.

[0067] S7) Qualitative and quantitative

[0068] The sample extract (formic acid-acetonitrile eluent) and the mixed standard working solution are measured under the above-mentioned liquid chromatography-tandem mass spectrometry conditions. If the retention time of the target compound in the sample extract differs from the retention time of the standard within ±2.5%; and if the relative abundance of the monitoring ion of the measured component in the sample spectrum is compared with the relative abundance of the corresponding monitoring ion in the standard solution with similar concentration, and the relative abundance of each ion is 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 is present in the sample.

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

[0070] Table 2

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

[0072] This patent utilizes a matrix-matched external standard method for quantitative detection. A standard curve is plotted using the concentration of the matrix-matched standard working solution as the horizontal axis and the quantification ion peak area of each organophosphorus flame retardant compound as the vertical axis. The concentration of each organophosphorus flame retardant compound in the sample solution is calculated using a linear regression equation. The response values of the target compound in both the standard working solution and the sample solution should be within the linear range of the instrument. If the response value exceeds the linear range, the sample should be diluted with a matrix blank solution and re-injected for analysis.

[0073] from Figure 1 It can be seen that 27 organophosphorus flame retardants were effectively separated and the detection of 27 organophosphorus flame retardants could 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] Whenever possible, glassware and chromatographically pure reagents should be used for experiments. A blank test should be performed for each operation to ensure that the blank background value is less than the quantitative limit of the corresponding compound.

[0080] S9) Limit of Quantitation

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

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

[0083] Table 4

[0084]

[0085] S10) Method recovery and method precision

[0086] A mixed standard intermediate solution of high, medium and low concentrations is quantitatively added to the sample, and a recovery test analysis is performed 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 the same operator using the same equipment and following the same test procedures in the same laboratory and on the same test object within a short period of time is less than 10%.

[0088] The recoveries and relative standard deviations of organophosphate compounds (n=6) are shown in Table 5.

[0089] Table 5

[0090]

[0091]

[0092] The embodiments described above provide a detailed description of 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 intended to limit the present invention. Any modifications, supplements or similar substitutions made within the scope of the principles of the present invention should be included in the scope of protection of the present invention.

Claims

1. A method for detecting the migration of organophosphorus flame retardants in consumer products, comprising the following steps: S1) preparing a simulated fluid; S2) preparing a mixed standard working solution; S3) allowing potential organophosphorus flame retardants in the sample to be tested to migrate into the mixed standard working solution through pretreatment; S4) adding a magnetic graphene oxide material to adsorb the organophosphorus flame retardant; S5) removing the magnetic graphene oxide material through a magnetic field, and eluting the organophosphorus flame retardant from the magnetic graphene oxide material with an eluent; S6) collecting the eluate and performing liquid chromatography-mass spectrometry / mass spectrometry analysis after filtration; In step S1, the simulated liquid includes simulated sweat and simulated saliva; In the step S2, the organophosphorus flame retardant includes triethyl phosphate, tris(2-chloropropyl) phosphate, triphenylphosphine oxide, triisopropyl phosphate, tripropyl phosphate, tris(2-chloropropyl) phosphate, (2-chloroethyl) dichloroisopentyl phosphate, di-(2,3-dibromopropyl) phosphate, tris(1,3-dichloro-2-propyl) phosphate, triphenyl phosphate, tris(2,3-dibromopropyl) phosphate, triisobutyl phosphate, diphenylcresyl phosphate, tris(2,3-dibromopropyl) phosphate, tris(1,3-dichloro-2-propyl) ...s(1 n-Butyl 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 bisdiphenyl phosphate, tris(3,5-dimethylphenyl) phosphate, tris(isopropylphenyl) phosphate, phenyl(di-tert-butylphenyl) phosphate, tri-n-hexyl phosphate, tris(2-ethylhexyl) phosphate; In step S3, the pretreatment includes: soaking the sample to be tested in a mixed standard working solution at room temperature, vortexing the solution during the soaking process, to obtain a soaking solution; In step S4, the adsorption time is 20 min, and vortexing is performed every 5 min for 30 s each time; In step S5, the eluent is 0.1% formic acid acetonitrile.

2. The method for detecting the migration of organophosphorus flame retardants in consumer products according to claim 1, characterized in that: The chromatographic conditions of the liquid chromatography-mass spectrometry / mass spectrometry analysis in step S4 include: Chromatographic column: T3 column; column temperature: 40℃; injection volume: 5.0μL; flow rate: 0.3mL / min; mobile phase: A is methanol, B is 0.1% formic acid water; gradient elution program: 0-0.2min, 80%B; 0.2-2.5min, 80%-35%B; 2.5-5.5min, 35%-30%B; 5.5-12.0min, 30%-25%B; 12.0-20.0min, 25%-5%B; 20.0-23.0min, 5%-0%B; 23.0-25.0min, 0%B; 25.0-26.0min, 0%-80%B; 26.0-28.0min, 80%B.

3. The method for detecting the migration of organophosphorus flame retardants in consumer products according to claim 1, characterized in that: The mass spectrometry conditions of the liquid chromatography-mass spectrometry / mass spectrometry analysis in step S4 include: Ion source: electrospray ion source; scan 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.

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