Synchronous determination method for multiple endocrine disrupters in solid waste

Abstract

The invention discloses a method for synchronously measuring multiple endocrine disruptors in solid waste. The method comprises the following steps: collecting a solid waste sample, and refrigerating and storing the solid waste sample by adopting a colored sealed container; performing first vortex treatment on the solid waste sample by adopting a vortex reagent to obtain a to-be-extracted sample; performing ultrasonic extraction treatment on the to-be-extracted sample according to a first extraction condition to obtain a primary extraction product; determining a final object to be detected according to the turbidity condition of the primarily extracted product; setting chromatographic conditions and mass spectrum conditions, and performing HPLC-MS / MS measurement on the final to-be-measured substance based on the chromatographic conditions and the mass spectrum conditions to obtain content data of the 16 ED Cs in the solid waste sample; according to the method, ultrasonic extraction is combined with a high performance liquid chromatography-tandem mass spectrometry technology, related conditions are optimized, simple, convenient and rapid pretreatment steps are realized, and the analysis sensitivity, the recovery rate and the precision are improved.

Description

Technical Field

[0001] The invention relates to the technical field of chemical detection, and in particular to a method for synchronously determining multiple endocrine disruptors in solid waste. Background Art

[0002] Endocrine disruptors (EDCs) are exogenous chemicals that interfere with hormone regulation in organisms, affecting the immune, reproductive and nervous systems of organisms and inducing diseases. They are polar, persistent and widely present in the environment, such as solid waste, sediments, soil, water and atmosphere. Common EDCs include phthalates, alkylphenols, polybrominated diphenyl ethers, nonylphenol and bisphenols. Among them, bisphenol compounds are widely used, especially bisphenol A, which has a high annual output and is mostly used in baby products, tableware, coatings, medical devices and food packaging. Bisphenols have excellent properties and can improve the moisture resistance, heat resistance, insulation, optics and mechanical properties of materials.

[0003] In recent years, bisphenol A substitutes have brought human exposure risks due to their widespread use. Under the influence of the external environment, they will precipitate from the main substance and enrich in various environmental media, threatening human health. Studies have shown that bisphenol compounds have estrogenic activity, which is harmful to the development of human reproductive organs and brain tissue, and can easily induce cancer. Although bisphenol compounds have been detected in a variety of environmental media, there is still a lack of quantitative research on a variety of such compounds in solid waste. Due to the complexity of solid waste media and the extremely low content of compounds, accurate quantitative analysis has become difficult, and there is currently no relevant analysis method.

[0004] In addition, in the prior art, for different types of compounds in EDCs, such as phthalates, alkylphenols, polybrominated diphenyl ethers and bisphenols, a variety of detection methods have been developed and applied to water quality, soil, air and specific products (such as electronic and electrical products, food contact materials, aquatic products, cosmetics, toys, etc.). However, these detection methods have certain limitations in practical applications. For the LC method, it is difficult to completely distinguish a variety of EDCs due to the similar structure of EDCs compounds and similar retention times. Although the UPLC-MS / MS method can distinguish, the instrument is expensive and the operation is complicated, which limits its wide application. The GC-MS method has low sensitivity and cumbersome pretreatment. In addition, the current determination methods for EDCs are mainly concentrated in specific fields, and there is still a lack of relevant research on the determination of EDCs in environmental solid wastes. Summary of the invention

[0005] The object of the present invention is to provide a method for the simultaneous determination of multiple endocrine disrupting chemicals in solid waste, thereby solving all or one of the above problems existing in the prior art.

[0006] In order to solve the above technical problems, the specific technical solutions of the present invention are as follows:

[0007] The present invention provides a method for synchronously determining multiple endocrine disrupting substances in solid waste, comprising the following steps:

[0008] Sample collection steps:

[0009] Collect solid waste samples and store them in refrigerated containers in colored sealed containers;

[0010] Sample extraction steps:

[0011] The solid waste sample is subjected to a first vortex treatment using a vortex reagent to obtain a sample to be extracted; the sample to be extracted is subjected to an ultrasonic extraction treatment according to a first extraction condition to obtain a preliminary extraction product; and a final analyte is determined according to the turbidity of the preliminary extraction product;

[0012] Sample measurement steps:

[0013] Chromatographic conditions and mass spectrometry conditions are set, and HPLC-MS / MS determination is performed on the final analyte based on the chromatographic conditions and the mass spectrometry conditions to obtain content data of 16 EDCs in the solid waste sample.

[0014] In one embodiment, the colored sealed container includes: a clean brown glass bottle with a stopper and ground mouth;

[0015] The refrigerated storage includes: adjusting the storage environment of the solid waste sample to a sealed and light-proof environment with a temperature below 4°C.

[0016] In one embodiment, the vortex reagent includes: anhydrous sodium sulfate and acetonitrile;

[0017] The first extraction conditions include: an ultrasonic duration of 30 minutes and an ultrasonic environment below 40°C.

[0018] In one embodiment, the first vortex treatment comprises:

[0019] A first mass of the solid waste sample is weighed, a second mass of anhydrous sodium sulfate is added, and then a third mass of the acetonitrile is added and vortex-mixed to obtain the sample to be extracted.

[0020] In one embodiment, the ultrasonic extraction process comprises:

[0021] The sample to be extracted is placed in an ultrasonic instrument; ultrasonic extraction treatment is performed according to the first extraction condition; and the product after the ultrasonic extraction treatment is left to stand for ten minutes is used as the preliminary extraction product.

[0022] In one embodiment, determining the final analyte according to the turbidity of the preliminary extraction product comprises:

[0023] When the turbidity condition is that the preliminary extraction product is not turbid, the preliminary extraction product is used as the final analyte;

[0024] When the turbidity condition indicates that the primary extraction product is turbid, a secondary purification operation based on centrifugal filtration is performed on the primary extraction product.

[0025] In one embodiment, the complex purification operation includes:

[0026] The centrifuge tube containing the preliminary extraction product is placed in a centrifuge for a first time and a first speed of centrifugation. After the centrifugation, a fourth mass of the supernatant of the centrifuged product is filtered through a filter membrane and used as the final analyte.

[0027] In one embodiment, the chromatographic conditions include:

[0028] A C18 reverse phase column with dimension parameters of 100 mm × 2.1 mm × 3 μm was used;

[0029] The mobile phases were pure water and methanol;

[0030] The flow gradient during the measurement was: 30% methanol, 0.5 min; 30%-95% methanol, 3.5 min; 95% methanol, 2.0 min; 95%-30% methanol, 1.0 min; 30% methanol, 8.0 min;

[0031] The column temperature was 40°C;

[0032] The flow rate was 0.3 mL / min.

[0033] The injection volume was 10 μL.

[0034] In one embodiment, the mass spectrometry conditions include:

[0035] The ion sources were: electrospray ionization-negative ion mode;

[0036] The monitoring modes are: multiple reaction monitoring mode;

[0037] The atomizing gas flow rate is 3L / min;

[0038] The heating gas flow rate is 10L / min;

[0039] Interface temperature is 300℃

[0040] DL temperature is 250℃

[0041] Heating block temperature is 400°C

[0042] In one embodiment, the first mass is 10.00 g;

[0043] The third mass is 50 mL;

[0044] The first duration is 5 minutes;

[0045] The first speed is 3000r / min;

[0046] The fourth mass is 1 mL;

[0047] The filter membrane is 0.22 μm.

[0048] The beneficial effects of the technical solution of the present invention are:

[0049] The method for simultaneous determination of multiple endocrine disruptors in solid waste described in the present invention can use ultrasonic extraction combined with high performance liquid chromatography-tandem mass spectrometry technology, and optimize relevant conditions to achieve simple and fast pre-treatment steps, improve analytical sensitivity, recovery rate and precision, and provide a reliable means for effective monitoring of EDCs in environmental solid waste. BRIEF DESCRIPTION OF THE DRAWINGS

[0050] In order to more clearly illustrate the specific implementation methods of the present invention or the technical solutions in the prior art, the drawings required for use in the specific implementation methods or the description of the prior art will be briefly introduced below. Obviously, the drawings described below are some implementation methods of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying creative work.

[0051] Figure 1 1 is a schematic flow chart of the method for simultaneously determining multiple endocrine disrupting chemicals in solid waste according to Example 1 of the present invention;

[0052] Figure 2 It is a total ion current chromatogram of 16 EDCs in the method for simultaneous determination of multiple endocrine disruptors in solid wastes described in Example 1 of the present invention;

[0053] The symbols in the accompanying drawings are explained as follows:

[0054] 1. Bisphenol S; 2. Bisphenol F; 3. Bisphenol E; 4. Bisphenol A; 5. Bisphenol B; 6. Bisphenol AF; 7. Bisphenol AP; 8. Bisphenol C; 9. Bisphenol Z; 10. Bisphenol FL; 11. Bisphenol BP; 12. Bisphenol M; 13. Bisphenol P; 14. Bisphenol TMC; 15. Bisphenol PH; 16. Tetrabromobisphenol A. DETAILED DESCRIPTION

[0055] The preferred embodiments of the present invention are described in detail below in conjunction with the accompanying drawings so that the advantages and features of the present invention can be more easily understood by those skilled in the art, thereby making a clearer and more definite definition of the protection scope of the present invention.

[0056] In the description of the present invention, it should be noted that the embodiments described in the present invention are only part of the embodiments of the present invention, rather than all of the embodiments; based on the embodiments in the present invention, all other embodiments obtained by ordinary technicians in the field without making creative work are within the scope of protection of the present invention.

[0057] The terms "first", "second", etc. in the specification and claims of this article and the above-mentioned drawings are used to distinguish similar objects, and are not necessarily used to describe a specific order or sequence. It should be understood that the data used in this way can be interchanged where appropriate, so that the embodiments of this article described here can be implemented in an order other than those illustrated or described here. In addition, the terms "including" and "having" and any variations thereof are intended to cover non-exclusive inclusions, for example, a process, method, device, product or equipment that includes a series of steps or units is not necessarily limited to those steps or units clearly listed, but may include other steps or units that are not clearly listed or inherent to these processes, methods, products or equipment.

[0058] In the description of the present invention, it should be noted that:

[0059] EDCs (Endocrine Disrupting Chemicals) are endocrine disruptors.

[0060] HPLC-MS / MS, (High performance liquid chromatography-tandem mass spectrometr), is high performance liquid chromatography-tandem mass spectrometry.

[0061] UE, (Ultrasound extraction), is ultrasonic extraction.

[0062] SW, (Solid waste), is solid waste.

[0063] In the description of the present invention, it should be noted that:

[0064] 1. In the embodiments of the present invention, the following listed instruments, reagents and conditions are all used as an implementation method, and the implementation method can be adapted and adjusted according to the implementation environment, objectives or conditions of the method in this embodiment.

[0065] 2. In the embodiments of the present invention, the instruments and equipment used are as follows:

[0066] 1. LCMS-8060 liquid chromatography-mass spectrometry instrument;

[0067] 2. 8510R-DTH CNC ultrasonic cleaner;

[0068] 3. Dura 12V ultrapure water machine.

[0069] 3. In the embodiments of the present invention, the reagent materials and their standards used are as follows:

[0070] 1. Methanol and acetonitrile: chromatographically pure;

[0071] 2. Anhydrous sodium sulfate: high purity;

[0072] 3. Bisphenol A, bisphenol S, bisphenol B, bisphenol F, bisphenol BP, bisphenol E, bisphenol PH, bisphenol C, bisphenol TMC, bisphenol M, bisphenol Z, tetrabromobisphenol A, bisphenol AF, bisphenol P, bisphenol FL, bisphenol AP;

[0073] 4. The experimental water is ultrapure water prepared by Dura 12V ultrapure water system.

[0074] In the description of the present invention, it should be noted that:

[0075] This method was used to simultaneously determine 16 EDCs in solid wastes, including bisphenol A (BPA), bisphenol B (BPB), bisphenol C (BPC), bisphenol F (BPF), bisphenol M (BPM), bisphenol Z (BPZ), bisphenol S (BPS), tetrabromobisphenol A (TBBPA), bisphenol BP (BPBP), bisphenol E (BPE), bisphenol AF (BPAF), bisphenol P (BPP), bisphenol FL (BPFL), bisphenol AP (BPAP), bisphenol pH (BPPH) and bisphenol TMC (BPTMC).

[0076] This embodiment provides a method for simultaneously determining multiple endocrine disrupting chemicals in solid waste, such as Figure 1 and Figure 2 As shown, the following steps are included:

[0077] S100, sample collection steps:

[0078] In this step, specific methods are used to collect and preserve solid waste samples, as follows:

[0079] S101. Collect and preserve solid waste in accordance with the relevant provisions of HJ / T 20 and HJ / T 298. The collected samples shall be stored in clean brown glass bottles with stoppers and ground-mouths. During the transportation of samples, ensure that the storage environment is sealed, light-proof and refrigerated at a temperature below 4°C.

[0080] S102. If the samples cannot be analyzed in time, refrigerate them below 4°C and keep them in a sealed and light-proof condition for no more than 10 days.

[0081] S200, sample extraction steps:

[0082] In this step, the sample is initially extracted, and further extraction is selectively performed on the sample based on the results of the initial extraction, as follows:

[0083] S201. Weigh 10.00 g (accurate to 0.01 g) of sample into a sample bottle, add an appropriate amount of anhydrous sodium sulfate, then add 50 mL of acetonitrile, vortex mix, and obtain the sample to be extracted; place the sample to be extracted in an ultrasonic instrument for 30 minutes of ultrasonic extraction, and control the temperature below 40°C during the ultrasonic extraction; after the ultrasonic extraction, let it stand for 10 minutes to clarify the supernatant to obtain a preliminary extraction product.

[0084] S202, judging the condition of the preliminary extraction product, if the preliminary extraction product is not turbid, the preliminary extraction product is used as the final analyte; if the preliminary extraction product is still turbid, the preliminary extraction product is transferred to a centrifuge tube, and the centrifuge tube containing the preliminary extraction product is placed in a centrifuge for centrifugation for 5 minutes at a speed of 3000r / min; after centrifugation, take about 1mL of the supernatant of the centrifuged product and filter it through a 0.22μm filter membrane into a chromatographic injection bottle as the final analyte.

[0085] S300, sample determination steps:

[0086] In this step, a C18 reverse phase column was used for separation, a mass spectrometer was used for detection, and the qualitative analysis was performed based on the retention time and characteristic ions, and the quantitative analysis was performed using the external standard method, as follows:

[0087] S301. Chromatographic conditions, including:

[0088] A C18 reverse phase chromatographic column (size parameters are 100mm×2.1mm×3μm) was used, the mobile phase was pure water and methanol, and the mobile gradient during the measurement was: 30% methanol, 0.5min; 30%-95% methanol, 3.5min; 95% methanol, 2.0min; 95%-30% methanol, 1.0min; 30% methanol, 8.0min; the column temperature was 40°C; the flow rate was 0.3mL / min; and the injection volume was 10μL.

[0089] S302. Mass spectrometry conditions, including:

[0090] The ion source was electrospray ionization-negative ion mode (ESI-); the monitoring mode was multiple reaction monitoring (MRM); the nebulizer gas flow rate was 3 L / min; the heating gas flow rate was 10 L / min; the interface temperature was 300 °C; the DL temperature was 250 °C; and the heating block temperature was 400 °C.

[0091] S303, standard solution determination, including:

[0092] (1) using methanol to prepare 1000 μg / L of the first EDCs mixed standard solution (bisphenol B, bisphenol F, bisphenol Z, bisphenol BP, bisphenol E, bisphenol PH, bisphenol TMC, bisphenol P);

[0093] (2) using methanol to prepare a 100 μg / L second EDCs mixed standard solution (bisphenol A, bisphenol M, bisphenol S, tetrabromobisphenol A, bisphenol AP);

[0094] (3) using methanol to prepare a 10 μg / L bisphenol AF mixed standard working solution;

[0095] (4) using methanol to prepare a 1000 μg / L third EDCs mixed standard solution (bisphenol C, bisphenol FL);

[0096] (5) The mixed standard solution should be refrigerated below 4°C, sealed, and stored away from light;

[0097] (6) Take appropriate amounts of EDCs mixed standard working solutions of different concentrations to prepare 16 EDCs mixed standard series. The concentrations of the standard series are as follows:

[0098] The mass concentrations of the standard solutions prepared based on the first EDCs mixed standard solution were 5.00 μg / L, 10.0 μg / L, 25.0 μg / L, 50.0 μg / L, and 100 μg / L.

[0099] The mass concentrations of the standard solutions prepared based on the second EDCs mixed standard solution were 0.50 μg / L, 1.00 μg / L, 2.50 μg / L, 5.00 μg / L, and 10.0 μg / L.

[0100] The mass concentrations of the standard solutions prepared based on the bisphenol AF mixed standard solution are: 0.10μg / L, 0.20μg / L, 0.50μg / L, 1.00μg / L, 2.00μg / L;

[0101] The mass concentrations of the standard solutions prepared based on the third EDCs mixed standard solution are 10.0μg / L, 20.0μg / L, 50.0μg / L, 100μg / L, and 200μg / L, respectively.

[0102] S304. According to the above chromatographic conditions, 16 EDCs standard solutions are measured from low concentration to high concentration, and a calibration curve is drawn with the target compound content as the horizontal axis and the chromatographic peak area as the vertical axis.

[0103] S305. Establish the same instrument conditions according to the calibration curve to perform sample measurement.

[0104] It should be noted that in order to prove the technical effect of this method, the linear range and detection limit of this method were verified as follows: According to the requirements of the "Technical Guidelines for the Development of Environmental Monitoring Analytical Method Standards" (HJ 168-2020), according to the full procedure of sample analysis, the blank spiked samples with a spike amount of 3 to 5 times the estimated method detection limit were repeated 9 times, and the method detection limit was calculated according to the formula LD = 2.896 × S, and the quantitative lower limit was calculated at 4 times the detection limit, where S is the standard deviation of the results of 9 parallel measurements; the results show that bisphenol B, bisphenol F, bisphenol Z, bisphenol BP, bisphenol E, bisphenol PH, bisphenol TMC and bisphenol P have good linear relationships in the concentration range of 5.00-100μg / L, and bisphenol A, bisphenol M, bisphenol S, tetrabromobisphenol A, and bisphenol AP have good linear relationships in the concentration range of 5.00-100μg / L. There is a good linear relationship in the concentration range of 0.50-10.0μg / L, bisphenol AF has a good linear relationship in the concentration range of 0.10-2.00μg / L, bisphenol C and bisphenol FL have a good linear relationship in the concentration range of 10.0-200μg / L, and the correlation coefficient r is greater than 0.995; when the sample size is 10.0g and the fixed volume is 50mL, the method detection limit of 16 EDCs is 0.10-15.8μg / kg, and the quantification limit is 0.40-63.2μg / kg, which can meet the detection requirements of EDCs in solid waste.

[0105] It should be noted that in order to prove the technical effect of this method, the recovery rate and precision of this method were verified as follows: 12 different types of actual solid waste samples collected in Suzhou City, Jiangsu Province were taken, and two groups of parallel spiked recovery experiments with different concentrations were performed. The contents of the first group of spiked samples were: 10ng (bisphenol AF), 50ng (bisphenol A, bisphenol M, bisphenol S, tetrabromobisphenol A, bisphenol AP), 0.5μg (bisphenol B, bisphenol F, bisphenol Z, bisphenol BP, bisphenol E, bisphenol PH , bisphenol TMC and bisphenol P), 1.0μg (bisphenol C, bisphenol FL); the second group of contents was 50ng (bisphenol AF), 0.25μg (bisphenol A, bisphenol M, bisphenol S, tetrabromobisphenol A, bisphenol AP), 2.5μg (bisphenol B, bisphenol F, bisphenol Z, bisphenol BP, bisphenol E, bisphenol PH, bisphenol TMC and bisphenol P), 5.0μg (bisphenol C, bisphenol FL); the determination was carried out according to the optimized method, and the spiked recoveries and relative standard deviations (RSD) of the determination results were calculated. At the low and high spiked concentration levels, the spiked recoveries of 16 PBBs were 81.1% to 110.14%, and the RSDs were 0.12% to 9.2%.

[0106] In addition, the following table shows the effect of the method:

[0107] Table 1: Standard curve equations, correlation coefficients, method detection limits and quantification limits of 16 EDCs:

[0108]

[0109]

[0110] Table 2: Retention time, quantitative / qualitative analysis characteristic ions and cone / collision voltage of 16 EDCs:

[0111]

[0112]

[0113] In summary, this method can determine 16 EDCs in solid waste based on ultrasonic extraction / high performance liquid chromatography-tandem mass spectrometry, wherein the 16 EDCs in solid waste can be rapidly and accurately determined by optimizing the instrumental analysis parameters and ultrasonic extraction conditions.

[0114] It should be noted that the examples herein are only for explaining the present invention and are not intended to limit the protection scope of the present invention.

[0115] Different from the prior art, the method for the simultaneous determination of multiple endocrine disruptors in solid waste in the present application can use ultrasonic extraction combined with high performance liquid chromatography-tandem mass spectrometry technology, and optimize the relevant conditions to achieve simple and fast pre-treatment steps, improve analytical sensitivity, recovery rate and precision, and provide a reliable means for the effective monitoring of EDCs in environmental solid waste.

[0116] It should be understood that in the various embodiments of this document, the size of the serial numbers of the above-mentioned processes does not mean the order of execution. The execution order of each process should be determined by its function and internal logic, and should not constitute any limitation on the implementation process of the embodiments of this document.

[0117] It should also be understood that in the embodiments of this document, the term "and / or" is only a description of the association relationship of the associated objects, indicating that three relationships may exist. For example, A and / or B can represent: A exists alone, A and B exist at the same time, and B exists alone. In addition, the character " / " in this document generally indicates that the associated objects before and after are in an "or" relationship.

[0118] Those of ordinary skill in the art will appreciate that the units and algorithm steps of each example described in conjunction with the embodiments disclosed herein can be implemented in electronic hardware, computer software, or a combination of the two. In order to clearly illustrate the interchangeability of hardware and software, the composition and steps of each example have been generally described in terms of function in the above description. Whether these functions are performed in hardware or software depends on the specific application and design constraints of the technical solution. Professional and technical personnel can use different methods to implement the described functions for each specific application, but such implementation should not be considered to be beyond the scope of this article.

[0119] Those skilled in the art can clearly understand that, for the convenience and brevity of description, the specific working processes of the systems, devices and units described above can refer to the corresponding processes in the aforementioned method embodiments and will not be repeated here.

[0120] In the several embodiments provided herein, it should be understood that the disclosed systems, devices and methods can be implemented in other ways. For example, the device embodiments described above are only schematic, for example, the division of the units is only a logical function division, and there may be other division methods in actual implementation, such as multiple units or components can be combined or integrated into another system, or some features can be ignored or not executed. In addition, the mutual coupling or direct coupling or communication connection shown or discussed can be an indirect coupling or communication connection through some interfaces, devices or units, or can be electrical, mechanical or other forms of connection.

[0121] The units described as separate components may or may not be physically separated, and the components shown as units may or may not be physical units, that is, they may be located in one place or distributed on multiple network units. Some or all of the units may be selected according to actual needs to achieve the purpose of the embodiments of this article.

[0122] In addition, each functional unit in each embodiment of this invention may be integrated into one processing unit, or each unit may exist physically separately, or two or more units may be integrated into one unit. The above integrated unit may be implemented in the form of hardware or in the form of software functional unit.

[0123] If the integrated unit is implemented in the form of a software functional unit and sold or used as an independent product, it can be stored in a computer-readable storage medium. Based on this understanding, the technical solution of this article is essentially or the part that contributes to the prior art, or all or part of the technical solution can be embodied in the form of a software product, and the computer software product is stored in a storage medium, including a number of instructions to enable a computer device (which can be a personal computer, a server, or a network device, etc.) to perform all or part of the steps of the method described in each embodiment of this article. The aforementioned storage medium includes: U disk, mobile hard disk, read-only memory (ROM, Read-Only Memory), random access memory (RAM, Random Access Memory), disk or optical disk and other media that can store program codes.

[0124] The above descriptions are merely embodiments of the present invention and are not intended to limit the patent scope of the present invention. Any equivalent structure or equivalent process transformation made using the contents of the present invention specification and drawings, or directly or indirectly applied in other related technical fields, are also included in the patent protection scope of the present invention.

Claims

1. A method for simultaneous determination of multiple endocrine disruptors in solid waste, characterized in that: The following steps are involved: Sample collection steps: Collect solid waste samples and store them in refrigerated containers in colored sealed containers; Sample extraction steps: The solid waste sample is subjected to a first vortex treatment using a vortex reagent to obtain a sample to be extracted; the sample to be extracted is subjected to an ultrasonic extraction treatment according to a first extraction condition to obtain a preliminary extraction product; and a final analyte is determined according to the turbidity of the preliminary extraction product; Sample measurement steps: Chromatographic conditions and mass spectrometry conditions are set, and HPLC-MS / MS determination is performed on the final analyte based on the chromatographic conditions and the mass spectrometry conditions to obtain content data of 16 EDCs in the solid waste sample.

2. The method for simultaneous determination of multiple endocrine disrupting chemicals in solid waste according to claim 1, characterized in that: The colored sealed container includes: a clean brown glass bottle with a stopper and a ground mouth; The refrigerated storage includes: adjusting the storage environment of the solid waste sample to a sealed and light-proof environment with a temperature below 4°C.

3. The method for simultaneous determination of multiple endocrine disrupting chemicals in solid waste according to claim 1, characterized in that: The vortex reagent comprises: anhydrous sodium sulfate and acetonitrile; The first extraction conditions include: an ultrasonic duration of 30 minutes and an ultrasonic environment below 40°C.

4. The method for simultaneous determination of multiple endocrine disrupting chemicals in solid waste according to claim 3, characterized in that: The first vortex treatment comprises: A first mass of the solid waste sample is weighed, a second mass of anhydrous sodium sulfate is added, and then a third mass of the acetonitrile is added and vortex-mixed to obtain the sample to be extracted.

5. The method for simultaneous determination of multiple endocrine disrupting chemicals in solid waste according to claim 3, characterized in that: The ultrasonic extraction process comprises: The sample to be extracted is placed in an ultrasonic instrument; ultrasonic extraction treatment is performed according to the first extraction condition; and the product after the ultrasonic extraction treatment is left to stand for ten minutes is used as the preliminary extraction product.

6. The method for simultaneous determination of multiple endocrine disrupting chemicals in solid waste according to claim 4, characterized in that: The method of determining the final analyte according to the turbidity of the preliminary extraction product comprises: When the turbidity condition is that the preliminary extraction product is not turbid, the preliminary extraction product is used as the final analyte; When the turbidity condition indicates that the primary extraction product is turbid, a secondary purification operation based on centrifugal filtration is performed on the primary extraction product.

7. The method for simultaneous determination of multiple endocrine disrupting chemicals in solid waste according to claim 6, characterized in that: The complex purification operation comprises: The centrifuge tube containing the preliminary extraction product is placed in a centrifuge for a first time and a first speed of centrifugation. After the centrifugation, a fourth mass of the supernatant of the centrifuged product is filtered through a filter membrane and used as the final analyte.

8. The method for simultaneous determination of multiple endocrine disrupting chemicals in solid waste according to claim 1, characterized in that: The chromatographic conditions include: A C18 reverse phase column with dimension parameters of 100 mm × 2.1 mm × 3 μm was used; The mobile phases were pure water and methanol; The flow gradient during the measurement was: 30% methanol, 0.5 min; 30%-95% methanol, 3.5 min; 95% methanol, 2.0 min; 95%-30% methanol, 1.0 min; 30% methanol, 8.0 min; The column temperature was 40°C; The flow rate was 0.3 mL / min; The injection volume was 10 μL.

9. The method for simultaneous determination of multiple endocrine disrupting chemicals in solid waste according to claim 1, characterized in that: The mass spectrometry conditions include: The ion sources were: electrospray ionization-negative ion mode; The monitoring modes are: multiple reaction monitoring mode; The atomizing gas flow rate is 3L / min; The heating gas flow rate is 10L / min; Interface temperature is 300℃ DL temperature is 250℃ The heating block temperature was 400°C.

10. The method for simultaneous determination of multiple endocrine disrupting chemicals in solid waste according to claim 7, characterized in that: The first mass is 10.00 g; The third mass is 50 mL; The first duration is 5 minutes; The first speed is 3000r / min; The fourth mass is 1 mL; The filter membrane is 0.22 μm.

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