Method for quantitatively detecting fluorinated electrolyte additive of lithium battery in soil based on gas chromatography-tandem mass spectrometry

Abstract

The invention belongs to the field of analysis and detection, and discloses a method for quantitatively detecting a fluorinated electrolyte additive of a lithium battery in soil based on gas chromatography-tandem mass spectrometry. After the environmental sample is subjected to extraction and concentration pretreatment, the eight lithium battery fluorinated electrolyte additives in the soil are subjected to quantitative analysis by adopting gas chromatography-tandem mass spectrometry (GC-MS / MS), the method is low in detection limit, simple and convenient to operate and high in recovery rate, sample matrix interference can be effectively reduced, and the detection accuracy is improved. The method is used for filling the blank of the method for detecting the lithium battery fluorinated electrolyte additive in the soil at home and abroad at present, and provides a method reference for detecting the lithium battery fluorinated electrolyte additive in the soil.

Description

Technical Field

[0001] This invention belongs to the field of analytical detection, and specifically relates to a method for quantitative detection of lithium battery fluorinated electrolyte additives in soil based on gas chromatography-tandem mass spectrometry. Background Technology

[0002] Lithium-ion batteries have become the mainstream energy storage technology due to their high energy density and long cycle life. The electrolyte, as a key component of the battery system, facilitates the directional migration of lithium ions between the positive and negative electrodes by constructing ion transport channels. However, traditional electrolytes still face problems such as insufficient thermal stability and susceptibility to gas expansion in practical applications. Precisely controlling the electrolyte system by adding functional additives has become an effective technical approach to improve the cycle stability, rate performance, and safety margin of lithium batteries. Among them, fluorinated electrolyte additives exhibit unique advantages in reducing interfacial impedance and suppressing side reactions by reconstructing the chemical environment at the electrode / electrolyte interface, resulting in a significant improvement in the overall battery performance.

[0003] With the rapid development of China's new energy vehicle and energy storage industries, China holds a significant position in the global electrolyte market. However, during the production, use, disposal, and recycling of lithium batteries, they may enter the environment through wastewater and exhaust gas emissions during production, electrolyte leakage due to high temperatures or physical damage during use, migration via leachate from landfills after disposal, and improper handling during recycling and dismantling. Soil, as one of the main destinations for pollutants, may accumulate these chemicals, especially persistent organic pollutants such as fluorinated electrolyte additives, through adsorption, leaching, or bioaccumulation. These pollutants can enter the human body through the food chain or direct contact, posing a potential threat to ecosystems and health. Currently, research on fluorinated electrolyte additives for lithium batteries is relatively limited, and a systematic method for qualitative and quantitative detection of fluorinated electrolyte additives for lithium batteries in soil has not yet been developed. Summary of the Invention

[0004] In order to overcome the shortcomings and deficiencies of the prior art, the primary objective of this invention is to provide a method for quantitative detection of lithium battery fluorinated electrolyte additives in soil based on gas chromatography-tandem mass spectrometry.

[0005] The objective of this invention is achieved through the following solution:

[0006] A method for quantitative detection of lithium battery fluorinated electrolyte additives in soil based on gas chromatography-tandem mass spectrometry, comprising the following steps:

[0007] (1) Pretreatment: Extract the soil sample to be tested with an extraction solvent, then centrifuge to separate the solid and liquid phases, take the supernatant, add the adsorbent, mix and centrifuge, take the supernatant, filter, and obtain the sample solution to be tested.

[0008] (2) Preparation of standard curves: Various lithium battery fluorinated electrolyte additive standards were prepared into standard working solutions with different concentration gradients using solvents. Then, gas chromatography-tandem mass spectrometry (GC-MS / MS) was used to detect the different concentrations of the standard working solutions of each lithium battery fluorinated electrolyte additive. The peak area of ​​each lithium battery fluorinated electrolyte additive standard in the standard working solution was used as the ordinate, and the concentration of the corresponding lithium battery fluorinated electrolyte additive standard in the standard working solution was used as the abscissa to establish standard working curves for various lithium battery fluorinated electrolyte additives.

[0009] (3) The test solution after pretreatment in step (1) is tested according to the operation of gas chromatography-tandem mass spectrometry (GC-MS / MS) in step (2). Then, the peak area of ​​each lithium battery fluorinated electrolyte additive is used as the ordinate and substituted into the standard working curve of the corresponding lithium battery fluorinated electrolyte additive in step (2) to obtain the corresponding concentration. Then, the obtained concentration is converted to obtain the concentration of each lithium battery fluorinated electrolyte additive in the soil sample to be tested.

[0010] Before the soil sample to be tested in step (1) is pre-treated, it is preferred to air-dry it first, then grind it and sieve it to remove large solid impurities in the soil. The sieving is preferably done by passing it through a 150μm stainless steel mesh.

[0011] The extraction solvent mentioned in step (1) is at least one of ethyl acetate, dichloromethane, and n-hexane, preferably dichloromethane; the amount of extraction solvent used is: 0.5 mL to 1 mL of extraction solvent for every 50 mg of soil sample to be tested.

[0012] The extraction described in step (1) is preferably ultrasonic extraction, with an ultrasonic extraction power of 300-500W, preferably 400W, and an extraction time of 10-20min;

[0013] In step (1), it is preferable to shake the sample on a shaker before extraction so that the extraction solvent can come into full contact with the sample. Shaking on a shaker means shaking at 2000 rpm for 2 min. After extraction, centrifugation to separate the solid and liquid phases is preferably performed at 3500-4000 rpm for 5 min.

[0014] In step (1), in order to fully extract the solid, the following solid can be extracted repeatedly after centrifugation, preferably three times, and then the supernatants are combined.

[0015] The adsorbent added in step (1) is at least one of octadecylsilane bonded silica gel and PSA (N-propylethylenediamine). The role of the adsorbent is to adsorb pigments and lipids. The amount of adsorbent added is such that the mass ratio of adsorbent to soil sample to be tested is 1:1. Centrifugation after adding adsorbent refers to centrifugation at 4000 rpm for 5 min.

[0016] The filtration mentioned in step (1) refers to passing through a 0.22 μm filter membrane;

[0017] The lithium battery fluorinated electrolyte additives mentioned in step (2) are one of N,N-dimethylaminosulfonyl fluoride, 1,1,1-trifluoro-n,n-dimethylmethanesulfonamide, trifluoromethanesulfonamide, tris(2,2,2-trifluoroethyl) phosphite, tris(2,2,2-trifluoroethyl) phosphate, tris(1H,1H,5H-octafluoropentyl) phosphate, fluoroethylene carbonate, and (trifluoromethyl)ethylene carbonate. Specific parameters are shown in Table 1.

[0018] Table 1 Fluorinated Additives for Lithium-ion Batteries

[0019]

[0020]

[0021] The solvent mentioned in step (2) is dichloromethane.

[0022] The concentration gradient mentioned in step (2) is preferably in the range of 1 ng / ml to 100 ng / ml; more preferably, seven standard working solutions with different concentration gradients are selected, namely 1 ng / ml, 2 ng / ml, 5 ng / ml, 10 ng / ml, 20 ng / ml, 50 ng / ml, and 100 ng / ml. The concentration is calculated by using the amount of standard additives for lithium battery fluorinated electrolytes and the actual volume of the final volume.

[0023] In step (2), the standard working curve can also be prepared by the following method: a mixed standard working solution is prepared by mixing various lithium battery fluorinated electrolyte additives with solvents. For each lithium battery fluorinated electrolyte additive, a mixed standard working solution with multiple concentration gradients is set. Then, the mixed standard working solution is detected by gas chromatography-tandem mass spectrometry (GC-MS / MS). The peak area of ​​each lithium battery fluorinated electrolyte additive in the mixed standard working solution is used as the ordinate, and the concentration of the corresponding lithium battery fluorinated electrolyte additive in the mixed standard working solution is used as the abscissa to establish the corresponding standard working curves for various lithium battery fluorinated electrolyte additives.

[0024] Preferably, when preparing the mixed standard working solution, the concentrations of the various lithium battery fluorinated electrolyte additives in the mixed standard working solution are all the same, and the concentration range of this uniform concentration is 1 ng / ml-100 ng / ml.

[0025] In step (2), gas chromatography-tandem triple quadrupole mass spectrometry (GC-MS / MS) was used to detect the fluorinated electrolyte additives. An Agilent HP-FFAP column (30m × 0.25mm × 0.25μm) was used for the gas chromatography.

[0026] The detection parameters described in step (2) are as follows: injection port temperature is 260-290℃ (preferably 280℃), splitless injection, and injection volume is 1.0 μL. An Agilent HP-FFAP (30m × 0.25mm × 0.25μm) gas chromatographic column is used, with high-purity helium as the carrier gas and a column flow rate of 1.0 mL / min. The initial temperature of the column oven is 40℃, held for 1 min, then increased to 230℃ at a rate of 8℃ / min and held for 2 min. The subsequent running temperature is 235℃ for 3 min. The transfer line temperature is 260-290℃ (preferably 280℃). High-purity nitrogen is used as the collision gas at a flow rate of 1.5 mL / min. High-purity helium is used as the quenching gas at a flow rate of 2.25 mL / min. The target compound was ionized using an electron impact ionization (EI) source with temperatures of 230 °C and 150 °C, respectively. Multiple reaction monitoring (MRM) was used with a gain factor of 1–10.

[0027] Table 2 shows the optimized ion pairs and collision energies of eight lithium battery fluorinated electrolyte additives.

[0028] Table 2. Ion pair parameters of eight fluorinated electrolyte additives for lithium batteries

[0029]

[0030]

[0031] Bold text indicates quantitative ion pairs.

[0032] Compared with the prior art, the present invention has the following advantages and beneficial effects:

[0033] After pretreatment by extraction and concentration of environmental samples, gas chromatography-tandem mass spectrometry (GC-MS / MS) was used to quantitatively analyze eight lithium battery fluorinated electrolyte additives in soil. The method has low detection limits, simple operation, high recovery rate, and can effectively reduce sample matrix interference. It fills the gap in the current detection methods of lithium battery fluorinated electrolyte additives in soil at home and abroad, and provides a methodological reference for the detection of lithium battery fluorinated electrolyte additives in soil. Attached Figure Description

[0034] Figure 1 The TIC chromatograms of eight fluorinated electrolyte additives in a homogeneous mixed standard working solution with a concentration of 100 ng / ml are shown.

[0035] Figure 2 The image shows a TIC chromatogram of industrial soil within the lithium battery production plant area in Example 1.

[0036] Figure 3 The TIC chromatogram is shown for agricultural soil outside the lithium battery production plant in Example 2. Detailed Implementation

[0037] The present invention will be further described in detail below with reference to embodiments and accompanying drawings, but the embodiments of the present invention are not limited thereto. Unless otherwise specified in the embodiments, conventional conditions or conditions recommended by the manufacturer shall apply. Reagents or instruments used, unless otherwise specified, are all commercially available conventional products.

[0038] Unless otherwise specified, all reagents used in the examples are commercially available.

[0039] Example 1

[0040] This embodiment provides a method for analyzing lithium-ion battery fluorinated electrolyte additives in industrial soil based on GC-MS / MS technology. The sample to be analyzed in this embodiment is an industrial soil sample from a lithium-ion battery production plant. The method includes the following steps:

[0041] Industrial soil samples were collected from the lithium battery production plant area, transferred to clean aluminum foil and air-dried at room temperature. After grinding, the samples were sieved through a stainless steel mesh (150 μm) and stored in amber glass jars at -20°C until analysis.

[0042] (1) Pre-processing method:

[0043] Take 50 mg of industrial soil sample from a lithium battery production plant and place it in a 10 mL glass centrifuge tube. Add 0.5 mL of dichloromethane and place the sample on a shaker at 2000 rpm for 2 min, followed by ultrasonic extraction at 400 W for 20 min. After ultrasonic extraction, separate the solid and liquid phases by high-speed centrifugation (3800 rpm, 5 min). Repeat the "shaking-ultrasonic extraction-centrifugation" process twice, and combine the supernatant in a new glass centrifuge tube. Then, bring the volume to 1 mL with dichloromethane. Add 50 mg of DSC-C18 (i.e., octadecylsilane-bonded silica gel packed in a C18 SPE column), vortex for 2 min, centrifuge at 4000 rpm for 5 min, collect the supernatant, filter through a 0.22 μm filter membrane, and inject the sample directly into a brown sample vial. Place at -20℃ for instrument analysis.

[0044] (2) GC-MS / MS detection:

[0045] Additives in lithium-ion battery fluorinated electrolytes were detected using an Agilent gas chromatography-tandem triple quadrupole mass spectrometer (7890B-7000D). The injection port temperature was 280℃, splitless injection was used, and the injection volume was 1.0 μL. An Agilent HP-FFAP column (30 m × 0.25 mm × 0.25 μm) was used with high-purity helium as the carrier gas at a flow rate of 1.0 mL / min. The column oven temperature was initially set at 40℃ and held for 1 min, then increased to 230℃ at a rate of 8℃ / min and held for 2 min. Finally, the temperature was increased to 235℃ and run for 3 min. The transfer line temperature was 280℃. High-purity nitrogen was used as the collision gas at a flow rate of 1.5 mL / min. High-purity helium was used as the quenching gas at a flow rate of 2.25 mL / min. The target compound was ionized using an electron impact ionization (EI) source with temperatures of 230 °C and 150 °C, respectively. Multiple reaction monitoring (MRM) was used with a gain factor of 10.

[0046] (3) Plotting the standard working curve:

[0047] Eight solutions of single lithium-ion battery fluorinated electrolyte additives with a concentration of 10 mg / mL were prepared using dichloromethane. Equal volumes of these solutions were then mixed and diluted with dichloromethane to obtain mixed standard working solutions with concentrations of 1 ng / ml, 2 ng / ml, 5 ng / ml, 10 ng / ml, 20 ng / ml, 50 ng / ml, and 100 ng / ml. Gas chromatography-tandem mass spectrometry (GC-MS / MS) was used to detect the seven mixed standard working solutions with different concentration gradients. The peak areas of the lithium-ion battery fluorinated electrolyte additives in the mixed standard working solutions were used as the ordinate, and the concentrations of the corresponding lithium-ion battery fluorinated electrolyte additives in the mixed standard working solutions were used as the abscissa. Standard working curves for each lithium-ion battery fluorinated electrolyte additive were obtained using these seven points. The corresponding linear equations and correlation coefficients are shown in Table 3.

[0048] (4) Accuracy evaluation

[0049] Eight different lithium battery fluorinated electrolyte additives (5 ng each) were added to 50 mg of industrial soil containing no lithium battery fluorinated electrolyte additives. After thorough mixing, the pretreatment step (1) was repeated, and the samples were analyzed according to the GC-MS / MS detection parameters of step (2). The matrix spike recovery rate was calculated based on the standard working curves of each lithium battery fluorinated electrolyte additive and the peak area of ​​the corresponding lithium battery fluorinated electrolyte additive in the spiked mixture. The details are shown in Table 3.

[0050] (5) Method detection limit

[0051] The detection limit of this invention is calculated using a signal-to-noise ratio of 3. Table 3 analyzes samples of 50 mg of industrial soil containing no lithium battery fluorinated electrolyte additives, in which 5 ng of each of the eight lithium battery fluorinated electrolyte additives were spiked.

[0052] (6) Matrix effect

[0053] Eight lithium battery fluorinated electrolyte additives were added to 50 mg of industrial soil containing no lithium battery fluorinated electrolyte additives. The amount of each fluorinated electrolyte additive added was 5 ng. Then, the pretreatment operation in step (1) was repeated, and the volume was finally adjusted to 1 mL. At the same time, the eight lithium battery fluorinated electrolyte additives were added to dichloromethane. The amount of each fluorinated electrolyte additive added was 5 ng, and the volume was adjusted to 1 mL. The two solutions were analyzed by GC-MS / MS according to the parameters in step (2) and compared. The matrix effect of each fluorinated compound (the response increases or decreases due to the influence of the matrix) was obtained by the ratio of the peak areas.

[0054] Table 3

[0055]

[0056]

[0057] As can be seen from Table 3, this method, through small-volume solvent extraction and the addition of an adsorbent, can be used to solve the problem of concentration and extraction of semi-volatile substances in the environment. The method has a low detection limit, is simple to operate, has a high recovery rate, and can effectively reduce sample matrix interference. It is suitable for rapid detection and analysis of trace compounds in fields such as environmental monitoring.

[0058] Example 2: This example provides a method for analyzing lithium battery fluorinated electrolyte additives in agricultural soil based on GC-MS / MS technology; the sample to be analyzed in this example is an agricultural soil sample from near a lithium battery production plant. This method includes the following steps:

[0059] Agricultural soil samples were collected from farmland near the lithium battery manufacturing plant. The samples were transferred to clean aluminum foil and air-dried at room temperature. After grinding, the samples were sieved through a stainless steel mesh (150 μm) and stored in amber glass jars at -20°C until analysis.

[0060] (1) Pre-processing method:

[0061] Same as Example 1

[0062] (2) GC-MS / MS detection:

[0063] Same as Example 1

[0064] (3) Plotting the standard working curve:

[0065] Same as Example 1

[0066] (4) Accuracy evaluation

[0067] Eight different lithium battery fluorinated electrolyte additives (5 ng each) were added to 50 mg of agricultural soil sample that did not contain such additives. After thorough mixing, the pretreatment step (1) was repeated, and the sample was analyzed according to the GC-MS / MS detection parameters of step (2). The matrix spike recovery rate was calculated based on the standard working curve of each lithium battery fluorinated electrolyte additive and the peak area of ​​the corresponding additive in the spiked mixture. The details are shown in Table 4.

[0068] (5) Method detection limit

[0069] The detection limit of this invention is calculated using a signal-to-noise ratio of 3. Table 4 analyzes samples of agricultural soil containing 50 mg of agricultural soil without lithium battery fluorinated electrolyte additives, in which all eight lithium battery fluorinated electrolyte additives were spiked with 5 ng.

[0070] (6) Matrix effect

[0071] Eight lithium battery fluorinated electrolyte additives were added to 50 mg of agricultural soil without lithium battery fluorinated electrolyte additives. The amount of each fluorinated electrolyte additive added was 5 ng. Then the pretreatment operation in step (1) was repeated, and finally the volume was adjusted to 1 mL. At the same time, the eight lithium battery fluorinated electrolyte additives were added to dichloromethane. The amount of each fluorinated electrolyte additive added was 5 ng, and the volume was adjusted to 1 mL. The two solutions were detected and compared by GC-MS / MS according to the parameters in step (2). The matrix effect of each fluorinated compound (the response increases or decreases due to the influence of the matrix) was obtained by the ratio of the peak areas.

[0072] Table 4

[0073]

[0074] The above embodiments are preferred embodiments of the present invention, but the embodiments of the present invention are not limited to the above embodiments. Any changes, modifications, substitutions, combinations, or simplifications made without departing from the spirit and principle of the present invention shall be considered equivalent substitutions and shall be included within the protection scope of the present invention.

Claims

1. A method for quantitative detection of lithium battery fluorinated electrolyte additives in soil based on gas chromatography-tandem mass spectrometry, characterized in that... Includes the following steps: (1) Pretreatment: Extract the soil sample to be tested with an extraction solvent, then centrifuge to separate the solid and liquid phases, take the supernatant, add the adsorbent, mix and centrifuge, take the supernatant, filter, and obtain the sample solution to be tested. (2) Preparation of standard curves: Various lithium battery fluorinated electrolyte additive standards were prepared into standard working solutions with different concentration gradients using solvents. Then, gas chromatography-tandem mass spectrometry was used to detect the different concentrations of standard working solutions of each lithium battery fluorinated electrolyte additive. The peak area of ​​each lithium battery fluorinated electrolyte additive standard in the standard working solution was used as the ordinate, and the concentration of the corresponding lithium battery fluorinated electrolyte additive standard in the standard working solution was used as the abscissa to establish standard working curves for various lithium battery fluorinated electrolyte additives. (3) The test solution after pretreatment in step (1) is tested according to the gas chromatography-tandem mass spectrometry operation in step (2). Then, the peak area of ​​each lithium battery fluorinated electrolyte additive is used as the ordinate and substituted into the standard working curve of the corresponding lithium battery fluorinated electrolyte additive in step (2) to obtain the corresponding concentration. Then, the obtained concentration is converted to obtain the concentration of each lithium battery fluorinated electrolyte additive in the soil sample to be tested.

2. The method for quantitative detection of lithium battery fluorinated electrolyte additives in soil based on gas chromatography-tandem mass spectrometry according to claim 1, characterized in that: The extraction solvent mentioned in step (1) is at least one of ethyl acetate, dichloromethane, and n-hexane.

3. The method for quantitative detection of lithium battery fluorinated electrolyte additives in soil based on gas chromatography-tandem mass spectrometry according to claim 1, characterized in that: The amount of extraction solvent used in step (1) is such that 0.5 mL to 1 mL of extraction solvent is used for every 50 mg of soil sample to be tested. The extraction described in step (1) is ultrasonic extraction, with a power of 300-500W and an extraction time of 10-20min.

4. The method for quantitative detection of lithium battery fluorinated electrolyte additives in soil based on gas chromatography-tandem mass spectrometry according to claim 1, characterized in that: Before the soil sample to be tested in step (1) is pretreated, it is first air-dried, then ground and sieved to remove large solid impurities in the soil. The sieving is done by passing through a 150μm stainless steel mesh. Before extraction in step (1), the sample is shaken to ensure that the extraction solvent is in full contact with the sample; after extraction, the solid and liquid phases are separated by centrifugation at 3500-4000 rpm for 5 min.

5. The method for quantitative detection of lithium battery fluorinated electrolyte additives in soil based on gas chromatography-tandem mass spectrometry according to claim 1, characterized in that: The adsorbent added in step (1) is at least one of octadecylsilane-bonded silica gel and N-propylethylenediamine.

6. The method for quantitative detection of lithium battery fluorinated electrolyte additives in soil based on gas chromatography-tandem mass spectrometry according to claim 1, characterized in that: The amount of adsorbent added in step (1) is such that the mass ratio of adsorbent to soil sample to be tested is 1:1; centrifugation after adding adsorbent refers to centrifugation at 4000 rpm for 5 min; The filtration mentioned in step (1) refers to passing through a 0.22 μm filter membrane.

7. The method for quantitative detection of lithium battery fluorinated electrolyte additives in soil based on gas chromatography-tandem mass spectrometry according to claim 1, characterized in that: The lithium battery fluorinated electrolyte additives mentioned in step (2) are one of N,N-dimethylaminosulfonyl fluoride, 1,1,1-trifluoro-n,n-dimethylmethanesulfonamide, trifluoromethanesulfonamide, tri(2,2,2-trifluoroethyl) phosphite, tri(2,2,2-trifluoroethyl) phosphate, tri(1H,1H,5H-octafluoropentyl) phosphate, fluoroethylene carbonate, and (trifluoromethyl)ethylene carbonate.

8. The method for quantitative detection of lithium battery fluorinated electrolyte additives in soil based on gas chromatography-tandem mass spectrometry according to claim 1, characterized in that: The solvent mentioned in step (2) is dichloromethane; The concentration gradient mentioned in step (2) is a concentration range of 1 ng / ml to 100 ng / ml.

9. The method for quantitative detection of lithium battery fluorinated electrolyte additives in soil based on gas chromatography-tandem mass spectrometry according to claim 1, characterized in that: In step (2), the standard working curve is prepared by the following method: a mixture of standard samples of various lithium battery fluorinated electrolyte additives is prepared together with a solvent to form a mixed standard working solution. For each lithium battery fluorinated electrolyte additive, a mixture of standard working solutions with multiple concentration gradients is set. Then, the mixed standard working solution is detected by gas chromatography-tandem mass spectrometry. The peak area of ​​each lithium battery fluorinated electrolyte additive standard in the mixed standard working solution is used as the ordinate, and the concentration of the corresponding lithium battery fluorinated electrolyte additive standard in the mixed standard working solution is used as the abscissa to establish the corresponding standard working curves for various lithium battery fluorinated electrolyte additives.

10. The method for quantitative detection of lithium battery fluorinated electrolyte additives in soil based on gas chromatography-tandem mass spectrometry according to claim 1, characterized in that: In step (2), gas chromatography-tandem triple quadrupole mass spectrometry was used to detect the fluorinated electrolyte additives; The detection parameters described in step (2) are as follows: the injection port temperature is 260-290℃, splitless injection, and the injection volume is 1.0μL; the gas chromatography column used is Agilent HP-FFAP, with high-purity helium as the carrier gas and a column flow rate of 1.0mL / min; the initial temperature of the column oven is 40℃, held for 1min, then increased to 230℃ at a rate of 8℃ / min and held for 2min; the subsequent running temperature is 235℃ and held for 3min; the transfer line temperature is 260-290℃; high-purity nitrogen is used as the collision gas with a flow rate of 1.5mL / min; high-purity helium is used as the quenching gas with a flow rate of 2.25mL / min; the target compound is ionized using an electron impact ion source, with the ion source and quadrupole temperatures at 230℃ and 150℃, respectively; multiple reaction monitoring is used in the monitoring mode, and the gain factor is 1-10.

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