A method for analyzing polycyclic aromatic hydrocarbons and halogenated polycyclic aromatic hydrocarbons by adsorption pen extraction-precolumn water removal-gas chromatography mass spectrometry

Abstract

The present application belongs to the technical field of organic matter detection, and particularly relates to a method for extracting polycyclic aromatic hydrocarbons and halogenated polycyclic aromatic hydrocarbons by using an adsorption pen, removing water by using a pre-column, and performing gas chromatography mass spectrometry analysis, which comprises the following steps: (1) collecting a sample, placing a water sample in a headspace bottle, and inserting an adsorption pen into the headspace bottle; (2) vacuumizing the adsorption pen; (3) removing the vacuum source, and placing the sample in a shaker for oscillation extraction; (4) removing the adsorption pen, and performing preliminary water removal at low temperature; and (5) installing a pre-column and a chromatographic column II, inserting the adsorption pen into a GC sample inlet for thermal desorption, simultaneously opening a V4 valve, controlling outlet flow at 20-40 ml / min, and controlling the temperature of the pre-column and the chromatographic column II during and after desorption. The present application uses an adsorption pen to extract polycyclic aromatic hydrocarbons and halogenated polycyclic aromatic hydrocarbons in water, removes water by using a pre-column, and performs gas chromatography mass spectrometry analysis, thereby overcoming the problems of large amount of organic solvent, complex operation, poor reproducibility, and water and solvent interference in the adsorption pen extraction technology in the prior art.

Description

Technical Field

[0001] This invention belongs to the field of organic matter detection technology, specifically relating to a method for the analysis of polycyclic aromatic hydrocarbons and halogenated polycyclic aromatic hydrocarbons by adsorption pen extraction, pre-column dehydration, and gas chromatography-mass spectrometry. Background Technology

[0002] Polycyclic aromatic hydrocarbons (PAHs) are a class of hydrocarbons composed of two or more benzene rings arranged in linear, angular, or clustered patterns. They are common environmental pollutants and pose a threat to human health. Sixteen PAHs are listed as priority pollutants by the U.S. Environmental Protection Agency (EPA). The carcinogenicity of PAHs increases with the number of benzene rings. Toxicological studies have shown that long-term exposure to environments containing PAHs, such as coal products, asphalt, and oilseeds, increases the incidence of diseases such as cancer. This is mainly because the metabolites of PAHs in the liver can bind to proteins, leading to cell mutations.

[0003] Halogenated polycyclic aromatic hydrocarbons (PAHs) are aromatic compounds in which one or more hydrogen atoms in a polycyclic aromatic hydrocarbon are replaced by halogen atoms. Their formation mechanism is similar to that of dioxins and PAHs. Halogenated PAHs also possess carcinogenic, teratogenic, and mutagenic toxicity, posing potential hazards to the ecological environment and human health. Existing research indicates that halogenated PAHs can be generated through processes such as solid waste incineration, fossil fuel combustion, vehicle exhaust emissions, and the extensive dismantling of electronic waste. Currently, halogenated PAHs have been detected in many environmental media, including water bodies, urban air, vehicle exhaust, bleached pulp, and soil and organisms in areas where electronic waste is dismantled.

[0004] Polycyclic aromatic hydrocarbons (PAHs) and halogenated PAHs exhibit bioaccumulation and can persist in the environment for extended periods, posing a growing global environmental concern. Environmental samples often show relatively low levels of PAHs and halogenated PAHs, and these samples are characterized by complex compositions and significant matrix interference. Therefore, appropriate sample pretreatment is fundamental for analytical determination, aiming to enrich analytes, eliminate matrix interference, improve detection sensitivity, and lower the detection limit. Current methods for extracting PAHs and halogenated PAHs from water bodies primarily employ liquid-liquid extraction and solid-phase extraction. However, these methods have drawbacks, such as high solvent consumption, potential for secondary pollution, complex operation, and poor reproducibility.

[0005] Adsorption pen extraction technology is a novel pretreatment technique that integrates extraction, concentration, and sample injection, and can be used to extract polycyclic aromatic hydrocarbons (PAHs) and halogenated PAHs. However, when using an adsorption pen, a large amount of water is adsorbed, leading to a decrease in the separation efficiency of the chromatographic column and the sensitivity of mass spectrometry, while also causing some damage to the instrument. Currently, the treatment of water adsorbed by the adsorption pen generally involves low-temperature dehydration, but its dehydration efficiency is limited and cannot completely remove the water. Summary of the Invention

[0006] To address the aforementioned technical problems, this invention provides a method for the extraction of polycyclic aromatic hydrocarbons (PAHs) and halogenated PAHs by an adsorption pen followed by pre-column dehydration and gas chromatography-mass spectrometry analysis. This method utilizes an adsorption pen to extract PAHs and halogenated PAHs from water, overcoming the problems of large amounts of organic solvents, complex operation, and poor reproducibility in existing technologies. Furthermore, the pre-column dehydration technology overcomes the interference of water and solvents in the adsorption pen extraction technique.

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

[0008] This invention provides a method for adsorption pen extraction-pre-column dehydration-gas chromatography-mass spectrometry analysis of polycyclic aromatic hydrocarbons (PAHs) and halogenated PAHs, comprising the following steps:

[0009] (1) Collect the sample. Place the water sample into the headspace bottle and insert the adsorption pen into the headspace bottle.

[0010] (2) Vacuum the absorbent pen;

[0011] (3) Remove the vacuum source and place the sample in a shaker for oscillation extraction;

[0012] (4) Remove the absorbent pen and remove the condensation from the outer wall;

[0013] (5) Install column I as a pre-column on the gas chromatograph and install column II on the gas chromatograph at the same time. Insert the adsorption pen into the GC (gas chromatograph) injection port for thermal desorption. At the same time, open the V4 valve on the gas chromatograph and control the outlet flow rate at 20-40 ml / min. During the thermal desorption, set the temperature of the pre-column to 5-10℃. After the thermal desorption is completed, close the V4 valve and perform separate heating operations on the pre-column and column II.

[0014] Preferably, the carrier gas in the GC-MS is high-purity helium (purity >99.999%), and the flow rate is 1-1.5 ml / min.

[0015] In (1), the water sample is 0.5-10 ml and the headspace bottle is 40 ml.

[0016] In (2), the vacuuming is to draw a vacuum to 28-29 inches of mercury from above the adsorption pen.

[0017] In step (3), the oscillation rate is 150 rpm, the extraction temperature is 70℃, and the extraction time is 12 h.

[0018] In step (4), removing the condensate on the outer wall specifically involves placing the adsorption pen in an ice tray for 30 minutes to remove the condensate on the outer wall of the adsorption pen.

[0019] In step (5), the thermal desorption temperature is 300℃ and the time is 4min.

[0020] In step (5), after thermal desorption is completed, the pre-column is heated to 250°C at a rate of 200°C / min, and the chromatographic column II is heated according to the following program: initial temperature of 65°C for 4 min, then increased to 140°C at 15°C / min, then increased to 245°C at 6°C / min for 2 min, and finally increased to 300°C at 6°C / min for 3 min.

[0021] When performing the above (5), the principle is as follows: the water and low-boiling-point components adsorbed by the adsorption pen packing are analyzed and flow out of the chromatographic column I (pre-column) first, and then flow out through the V4 valve to remove water and low-boiling-point substances; at this time, the high-boiling-point substances are still stored in the pre-column (chromatographic column 1). Before the high-boiling-point substances come out of the pre-column, the V4 valve is closed and the high-boiling-point substances enter the chromatographic column II in sequence for separation and reach the detector for analysis.

[0022] The chromatographic column I described in this invention is a pre-column, specifically: DB-1, 0.53mm×5μm×5cm.

[0023] Furthermore, the chromatographic column II of this invention is specifically: DB-5MS, 30m×0.25mm×0.25μm.

[0024] Furthermore, the filler for the adsorption pen of the present invention is Tenax TA 35 / 60.

[0025] Because the concentrations of polycyclic aromatic hydrocarbons (PAHs) and halogenated PAHs in water are low, necessary extraction and concentration are required before detection. This invention employs adsorption pen technology. Under vacuum conditions, the boiling point of the target analyte decreases, making it easier to diffuse into the gas phase. It is then adsorbed and enriched by the adsorption pen, which is equipped with multiple packing materials. The adsorption pen directly performs thermal desorption on the GC column head, and the analyte enters a self-designed pre-column. After removing water and solvent, it is separated and analyzed by chromatographic column II and instrument detectors. This achieves the integrated purpose of extraction, concentration, water removal, and injection of halogenated PAHs in water.

[0026] On the other hand, the present invention also provides the application of the above method in the analysis of polycyclic aromatic hydrocarbons and halogenated polycyclic aromatic hydrocarbons in water, which is also within the scope of protection of the present invention.

[0027] The beneficial effects of this invention are as follows:

[0028] (1) This invention utilizes an adsorption pen to extract polycyclic aromatic hydrocarbons and halogenated polycyclic aromatic hydrocarbons from water. The operation is simple and convenient, and it can integrate extraction, concentration and injection, overcoming the shortcomings of liquid-liquid extraction, solid-phase extraction and other technologies such as high consumption of organic solvents and cumbersome operation.

[0029] (2) In response to the problem of excess water in the adsorption pen, the present invention independently developed a pre-column dehydration technology, which solved the problems of excess water and solvent interference in the adsorption pen extraction technology, improved the sensitivity of the adsorption pen in extracting polycyclic aromatic hydrocarbons and halogenated polycyclic aromatic hydrocarbons, and avoided damage to the instrument due to the presence of water. The established method has good sensitivity, precision and accuracy. Attached Figure Description

[0030] Figure 1 Flowchart for adsorption pen extraction-pre-column dehydration analysis of polycyclic aromatic hydrocarbons and halogenated polycyclic aromatic hydrocarbons in water;

[0031] Figure 2 This is a flowchart of the pre-column dewatering process;

[0032] Figure 3 Comparison of the extraction efficiency of different adsorption pens for halogenated polycyclic aromatic hydrocarbons;

[0033] Figure 4 Comparison of the extraction efficiency of polycyclic aromatic hydrocarbons using different adsorption pens;

[0034] Figure 5 A comparison of extraction efficiencies of halogenated polycyclic aromatic hydrocarbons under vacuum and non-vacuum conditions;

[0035] Figure 6 A comparison of extraction efficiencies of polycyclic aromatic hydrocarbons under vacuum and non-vacuum conditions;

[0036] Figure 7 A comparison of the extraction efficiency of halogenated polycyclic aromatic hydrocarbons under conditions of no pre-column and with pre-column;

[0037] Figure 8 This study compares the extraction efficiency of polycyclic aromatic hydrocarbons under conditions without a pre-column and under different pre-column conditions. Detailed Implementation

[0038] To enable those skilled in the art to better understand the present invention, the present invention will now be further described in conjunction with specific embodiments.

[0039] Example 1: Preparation of standard solution

[0040] Example 1-1 Preparation of standard solutions of halogenated polycyclic aromatic hydrocarbons

[0041] Accurately prepare 20 ng / L standard solutions of 11 halogenated polycyclic aromatic hydrocarbons (2-bromofluorene, 9-chlorophenanthrene, 2-chloroanthracene, 2,7-dichlorofluorene, 9-bromophenanthrene, 9-bromoanthracene, 9,10-dichloroanthracene, 2,7-dibromofluorene, 9,10-dibromoanthracene, 1-bromopyrene, 7-bromo-benzo[a]anthracene).

[0042] Examples 1-2: Preparation of polycyclic aromatic hydrocarbon standard solutions

[0043] Accurately prepare 20 ng / L standard solutions of 16 polycyclic aromatic hydrocarbons (naphthalene, acenaphthene, acenaphthene, fluorene, phenanthrene, anthracene, fluoranthene, pyrene, benzo[a]anthracene, β, benzo(b)fluoranthene, benzo(k)fluoranthene, benzo[a]pyrene, benzo[g, h, i]perylene, dibenzo[a, h]anthracene, and indene(1,2,3-cd)pyrene).

[0044] Example 2: Optimization of Adsorption Pen Filler

[0045] Take 10 mL of the standard solutions from Examples 1-1 and 1-2 and add them to 40 mL headspace vials. Extract the target analytes using three different adsorption pens: Tenax TA 35 / 60, PDMS, and 1000 Carboxen packing material, respectively, under the conditions of a vacuum of 28-29 inches of mercury, an extraction temperature of 70°C, and an extraction time of 12 hours. After extraction, the adsorption pen was placed on an ice tray for 30 minutes. Then, the adsorption pen was inserted into the GC injection port for thermal desorption (desorption temperature 300℃, desorption time 4 min). Simultaneously, the V4 valve was opened, and the outlet flow rate was controlled within 20-40 ml / min. The pre-column temperature (DB-1, 0.53 mm × 5 μm × 5 cm, column I) was set to 5-10℃. After 4 minutes, the V4 valve was closed, and the pre-column temperature was rapidly increased (200℃ / min) to 250℃. Simultaneously, the column II temperature (DB-5MS, 30 m × 0.25 mm × 0.25 μm) was increased according to the following procedure: initial temperature 65 °C, held for 4 min; increased to 140 °C at 15 °C / min; increased to 245 °C at 6 °C / min, held for 2 min; and finally increased to 300 °C at 6 °C / min. The temperature was set at °C for 3 min, with high-purity helium (purity >99.999%) as the carrier gas and a flow rate of 1-1.5 ml / min. The mass spectrometer ion source was an EI source (70 eV); the injection port temperature, transfer line temperature, and ion source temperature were all 300°C. GC-MS was used for the quantitative detection of polycyclic aromatic hydrocarbons (PAHs) and halogenated PAHs using selected ion scan mode (SIM). Information on mass spectrometry fragmentation is shown in Tables 1 and 2. Peak areas of compounds extracted by different types of adsorption pens are shown in... Figure 3 and Figure 4 As shown, the results indicate that Tenax TA 35 / 60 exhibits the best extraction performance for both polycyclic aromatic hydrocarbons (PAHs) and halogenated PAHs.

[0046] Table 1. Qualitative and quantitative ions of 11 halocyclic polycyclic aromatic hydrocarbons 1 2-Bromofluorene 2-BrFlu 244,246,165 246 2 9-Chlorophenanthrene 9-ClPhe 212,176,150 212 3 2-Chloroanthracene 2-ClAnt 212,176,150 212 4 2,7-Dichlorofluorene <![CDATA[2,7-Cl2Flu]]> 163,199,234 234 5 9-Bromophenanthrene 9-BrPhe 256,258,176 256 6 9-Bromoanthracene 9-BrAnt 256,258,176 256 7 9,10-Dichloroanthracene <![CDATA[9,10-Cl2Ant]]> 246,176,123 246 8 2,7-Dibromofluorene <![CDATA[2,7-Br2Flu]]> 324,243,163 324 9 9,10-Dibromoanthracene <![CDATA[9,10-Br2Ant]]> 336,176,88 336 10 1-Bromopyrene 1-BrPyr 282,280,201 280 11 7-Bromo-benzo[a]anthracene 7-BrBaA 306,308,226 306

[0047] Table 2 Qualitative and quantitative ions of 16 polycyclic aromatic hydrocarbons 1 Naphthalene NaP 128,102 128 2 Acenaphthylene Acy 152,126,76 152 3 Acenaphthene Ace 153,126,76 153 4 Fluorene Flu 166,139,83 166 5 Phenanthrene Ant 178,152,89 178 6 Anthracene Phe 178,152,89 178 7 Fluoranthene Fla 202,200,101 202 8 Pyrene Pyr 202,200,101 202 9 Benzo[a]anthracene BaA 228,114,101 228 10 Chrysene Chr 228,113,101 228 11 Benzo(b)fluoranthene BbF 252,126,113 252 12 Benzo(k)fluoranthene BkF 252,125,113 252 13 Benzo(a)pyrene Pyr 252,126,113 252 14 Benzo(g,h,i)perylene BghiP 276,274,138 276 15 Dibenzo(a,h)anthracene DahA 278,276,139 278 16 Indeno(1,2,3-cd)pyrene IcdP 276,274,138 276

[0048] Example 3: Optimization of Vacuum and Non-Vacuum Conditions

[0049] The standard solutions from Examples 1-1 and 1-2 were used as standard solutions, respectively. An adsorption pen filled with Tenax TA 35 / 60 packing material was used for extraction at 70°C for 12 hours, under a vacuum of 28-29 inches of mercury or without vacuum, to extract the target analytes. Thermal desorption, pre-column preparation, and GC / MS conditions were the same as in Example 2. The peak areas of the compounds extracted by the adsorption pen under vacuum and non-vacuum conditions are shown in [Figure number missing]. Figure 5 and Figure 6 The results showed that vacuum conditions yielded the best extraction performance for both polycyclic aromatic hydrocarbons (PAHs) and halogenated PAHs.

[0050] Example 4: Optimization of Pre-column Types

[0051] The standard solutions from Examples 1-1 and 1-2 were used as standard solutions. Extraction of the target analytes was performed using a Tenax TA 35 / 60 packing adsorption pen at an extraction temperature of 70°C for 12 hours under a vacuum of 28-29 inches of mercury. Thermal desorption and GC / MS conditions were the same as in Example 2. Peak areas of the compound responses under conditions with and without pre-column are shown in [Figure number missing]. Figure 7 and Figure 8 The results show that the target object has the highest response under the condition of using the pre-column DB-1.

[0052] Example 5: Method detection limit, precision, and recovery

[0053] Example 5-1

[0054] Eleven halogenated polycyclic aromatic hydrocarbons (PAHs) solutions at concentrations of 0.20, 0.40, 0.80, 1.60, 4.00, 10.0, 20.0, and 30.0 ng / L were prepared and analyzed according to the method in Example 2. The results are shown in Table 3. Table 3 shows that the linear correlation coefficients of the standard curves were all >0.997; the limits of detection (LOD) were 0.11-0.95 ng / L; the relative standard deviations of the six target analyte solutions at a concentration of 4.00 ng / L were <9.7%; and the recoveries of the eleven PAHs at a concentration of 3.00 ng / L were 77.4-109%. The results indicate that the established method has good linearity, sensitivity, precision, and accuracy.

[0055] Table 3. Method parameters for 11 types of halogenated polycyclic aromatic hydrocarbons 1 2-Bromofluorene 0.9995 0.34 9.6 89.7 2 9-Chlorophenanthrene 0.9985 0.23 6.9 109 3 2-Chloroanthracene 0.9995 0.15 4.1 80.3 4 2,7-Dichlorofluorene 0.9995 0.19 5.8 82.5 5 9-Bromophenanthrene 0.9995 0.40 9.7 90.2 6 9-Bromoanthracene 0.9995 0.11 3.2 77.4 7 9,10-Dichloroanthracene 0.9990 0.22 6.2 81.9 8 2,7-Dibromofluorene 0.9995 0.85 8.6 93.6 9 9,10-Dibromoanthracene 0.9970 0.95 9.5 99.3 10 1-Bromopyrene 0.9985 0.64 8.2 92.6 11 7-Bromo-benzo[a]anthracene 0.9995 0.80 6.6 96.7

[0056] Example 5-2

[0057] Sixteen polycyclic aromatic hydrocarbon (PAH) solutions at concentrations of 0.50, 1.00, 2.00, 4.00, 10.0, and 100 ng / L were prepared and analyzed according to the method in Example 2. The results are shown in Table 4. Table 4 shows that the linear correlation coefficients of the standard curves were all >0.995; the limits of detection (LOD) ranged from 0.14 to 0.64 ng / L; the relative standard deviations of the six target analyte solutions at a concentration of 4.00 ng / L were <8.7%; and the recoveries of the 16 PAHs at a concentration of 4.00 ng / L ranged from 91.2% to 124%. The results indicate that the established method exhibits good linearity, sensitivity, precision, and accuracy.

[0058] Table 4. Method parameters for 16 polycyclic aromatic hydrocarbons 1 Naphthalene 0.9990 0.29 6.8 124 2 Acenaphthylene 0.9990 0.25 4.9 120 3 Acenaphthene 0.9985 0.38 7.9 115 4 Fluorene 0.9990 0.42 4.7 109 5 Phenanthrene 0.9995 0.14 5.5 99.6 6 Anthracene 0.9990 0.27 5.4 99.0 7 Fluoranthene 0.9975 0.63 7.0 107 8 Pyrene 0.9975 0.64 5.2 109 9 Benzo[a]anthracene 0.9960 0.26 7.5 94.9 10 Chrysene 0.9985 0.32 7.3 121 11 Benzo(b)fluoranthene 0.9950 0.20 7.7 98.3 12 Benzo(k)fluoranthene 0.9995 0.29 8.2 115 13 0.9985 0.26 6.8 96.3 14 Benzo(a)pyrene 0.9990 0.49 7.7 91.2 15 Benzo(g,h,i)perylene 0.9995 0.19 8.7 91.4 16 Dibenzo(a,h)anthracene Indeno(1,2,3-cd)pyrene 0.9995 0.36 7.6 93.5

[0059] Example 6: Analysis of Actual Samples

[0060] Example 6-1

[0061] The established technique was applied to the analysis of halogenated polycyclic aromatic hydrocarbons (PAHs) in water samples from Luoma Lake, and the concentrations determined by this method were compared with those obtained by the traditional liquid-liquid extraction method. The results are shown in Table 5. The results showed that 9-chlorophenanthrene and 9-bromophenanthrene were detected in two water samples. Compared with the results obtained by the traditional liquid-liquid extraction method, the relative deviation of the PAH concentrations detected by the two methods was less than 7.4%. The actual sample recoveries ranged from 73.5% to 97.1%, and the relative standard deviations were 2.5% to 12.7%, indicating that the established technique can be applied to the analysis of halogenated PAHs in actual water samples.

[0062] Example 6-2

[0063] The established technique was applied to the detection of polycyclic aromatic hydrocarbons in water samples from Luoma Lake, and the concentrations determined by this method were compared with those obtained by the traditional liquid-liquid extraction method. The results are shown in Table 5.

[0064] Table 5 Comparison of results of detection using adsorption pen technology and liquid-liquid extraction technology.

[0065] (Note: " / " indicates no detection or no relevant data)

[0066] The results showed that naphthalene, fluorene, phenanthrene, fluoranthene, and pyrene were detected in both water samples. Compared with the results of the traditional liquid-liquid extraction method, the relative deviation of the PAH concentrations detected by the two methods was less than 19.4%. The actual sample recovery rate ranged from 76.4% to 93.3%, with a relative standard deviation of 2.5% to 13.2%, indicating that the established technique can be applied to the analysis of polycyclic aromatic hydrocarbons in actual water samples.

Claims

1. A method for adsorption pen extraction-pre-column dehydration-gas chromatography-mass spectrometry analysis of polycyclic aromatic hydrocarbons and halogenated polycyclic aromatic hydrocarbons, characterized in that, The polycyclic aromatic hydrocarbons mentioned are: naphthalene, acenaphthene, acenaphthene, fluorene, phenanthrene, anthracene, fluoranthene, pyrene, benzo[a]anthracene, β, benzo(b)fluoranthene, benzo(k)fluoranthene, benzo(a)pyrene, benzo(g, h, i)perylene, dibenzo(a, h)anthracene and indene(1,2,3-cd)pyrene; The halocyclic polycyclic aromatic hydrocarbons mentioned are: 2-bromofluorene, 9-chlorophenanthrene, 2-chloroanthracene, 2,7-dichlorofluorene, 9-bromophenanthrene, 9,10-dichloroanthracene, 2,7-dibromofluorene, 9,10-dibromoanthracene, 1-bromopyrene and 7-bromo-benzo[a]anthracene; The method includes the following steps: (1) Collect the sample, put the water sample into the headspace bottle, and insert the adsorption pen into the headspace bottle; the adsorption pen filler is Tenax TA 35 / 60; (2) Vacuum the adsorption pen; the vacuuming is: evacuate the adsorption pen from above to a vacuum level of 28-29 inches of mercury; (3) Remove the vacuum source and place the sample in a shaker for oscillation extraction; the oscillation rate is 150 rpm, the extraction temperature is 70℃, and the extraction time is 12 h. (4) Remove the absorbent pen and remove the condensate on the outer wall; to remove the condensate, place the absorbent pen in an ice tray for 30 minutes to remove the condensate on the outer wall of the absorbent pen. (5) Install column I as a pre-column on the gas chromatograph. Pre-column: DB-1, 0.53mm×5μm×5cm; At the same time, install column II on the gas chromatograph. Insert the adsorption pen into the gas chromatograph inlet for thermal desorption. The thermal desorption temperature is 300℃ and the time is 4 min. At the same time, open the V4 valve on the gas chromatograph and control the outlet flow rate at 20-40ml / min. During the thermal desorption, set the temperature of the pre-column to 5-10℃. After the thermal desorption is completed, close the V4 valve and perform separate temperature increases on column I and column II. Column II: DB-5MS, 30m × 0.25mm × 0.25μm; After analysis, the pre-column was heated to 250°C at a rate of 200°C / min; column II was heated according to the following program: initial temperature 65°C held for 4 min, increased to 140°C at 15°C / min, then increased to 245°C at 6°C / min held for 2 min, and finally increased to 300°C at 6°C / min held for 3 min; the carrier gas was high-purity helium with a purity >99.999%, and the flow rate was 1-1.5 ml / min; the mass spectrometer ion source was a 70 eV EI source; the injection port temperature, transfer line temperature, and ion source temperature were all 300°C; GC-MS was used to quantitatively detect polycyclic aromatic hydrocarbons and halogenated polycyclic aromatic hydrocarbons by selected ion scanning mode.

2. The application of the method of claim 1 in the analysis of polycyclic aromatic hydrocarbons and halogenated polycyclic aromatic hydrocarbons in water.

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