Method for detecting content of polycyclic aromatic hydrocarbon in atomized matrix aerosol

Abstract

The invention discloses a method for detecting the content of polycyclic aromatic hydrocarbon in atomized matrix aerosol, which comprises the following steps: extraction: introducing the atomized matrix aerosol into an extraction reagent, and dissolving a target object in the extraction reagent to obtain an extracting solution; wherein the target object comprises polycyclic aromatic hydrocarbon, and the extraction reagent comprises ethanol and normal hexane; and detection: detecting the extracting solution by adopting a liquid chromatography-mass spectrometry method. According to the method for detecting the content of the polycyclic aromatic hydrocarbon in the atomized matrix aerosol, the polycyclic aromatic hydrocarbon can be effectively extracted from the atomized matrix aerosol, and the polycyclic aromatic hydrocarbon can be accurately detected.

Description

Technical Field

[0001] The present application relates to the field of chromatography detection technology, and in particular to a method for detecting the content of polycyclic aromatic hydrocarbons in atomized matrix aerosol. Background Art

[0002] Electronic vaping devices convert an aerosolized matrix containing nicotine, flavorings, and other chemicals into an inhalable aerosol. The aerosolized matrix contains various organic compounds, and the high temperature of the aerosolization process can cause reactions between these organic compounds, producing polycyclic aromatic hydrocarbons (PAHs). PAHs are organic compounds composed of two or more benzene rings and are carcinogens that pose serious risks to human health.

[0003] At present, there are few detection methods for polycyclic aromatic hydrocarbons in aerosols from electronic atomization devices, and the content of polycyclic aromatic hydrocarbons in aerosols from electronic atomization devices is relatively low. Therefore, there are great technical difficulties in the extraction and determination of polycyclic aromatic hydrocarbons in aerosols from electronic atomization devices.

[0004] Therefore, developing a method that can accurately detect the content of polycyclic aromatic hydrocarbons in the aerosol of electronic atomization devices is of great significance for evaluating the safety of electronic atomization devices and atomization matrices. Summary of the Invention

[0005] The present application provides a method for detecting the content of polycyclic aromatic hydrocarbons in atomized matrix aerosol, which is used to solve the problem that there are few detection methods for polycyclic aromatic hydrocarbons in aerosols of electronic atomization devices in the prior art.

[0006] This application adopts the following technical solutions:

[0007] The present application discloses a method for detecting the content of polycyclic aromatic hydrocarbons in an atomized matrix aerosol, comprising: extraction: passing the atomized matrix aerosol into an extraction reagent, dissolving the target substance in the extraction reagent, and obtaining an extract; wherein the target substance includes polycyclic aromatic hydrocarbons, and the extraction reagent includes ethanol and n-hexane;

[0008] Detection: The extract is detected by liquid chromatography-mass spectrometry, including: preparing a series of standard solutions containing an internal standard and the target, wherein the target includes polycyclic aromatic hydrocarbons; wherein the concentration of the internal standard is the same and the concentration of the target is different in different standard solutions; detecting the series of standard solutions by liquid chromatography-mass spectrometry, and obtaining a standard curve based on the detection results; adding the internal standard to the extract to obtain a test solution; detecting the test solution by liquid chromatography-mass spectrometry, and determining the concentration of polycyclic aromatic hydrocarbons in the test solution based on the detection results and the standard curve.

[0009] In one implementation of the present application, after the extraction step, an enrichment step is also included, and the enrichment step includes: extracting and eluting the extract using solid phase microextraction technology to obtain an eluate for detection.

[0010] In one implementation of the present application, the polycyclic aromatic hydrocarbons include benz(a)anthracene, At least one of benzo(b)fluoranthene and benzo(α)pyrene.

[0011] In one implementation of the present application, the internal standard includes naphthalene-d8, -d12, at least one of benzo(b)fluoranthene-d12 and benzo(a)pyrene-d12.

[0012] In one implementation of the present application, the volume ratio of ethanol to n-hexane in the extraction reagent is 3:7 to 7:3.

[0013] In one implementation of the present application, the volume ratio of ethanol to n-hexane in the extraction reagent is 5:5.

[0014] In one implementation of the present application, a C18 solid phase extraction column is used to extract the extract.

[0015] In one implementation of the present application, in the enrichment step, dichloromethane is used for elution.

[0016] In one implementation of the present application, the enrichment step further includes concentrating the eluted liquid to obtain the eluate.

[0017] In one implementation of the present application, in a series of the standard solutions, the concentration of the target substance includes 0.1 ng / L, 1 ng / L, 5 ng / L, 10 ng / L, 50 ng / L and 100 ng / L, and the concentration of the internal standard is a value within the range of 5 ng / L to 50 ng / L.

[0018] In one implementation of the present application, the chromatographic conditions of the liquid chromatography-mass spectrometry method include: the chromatographic column is a C18 chromatographic column or a chromatographic column equivalent to the C18 chromatographic column; the mobile phase includes an organic solvent and water, and the organic solvent includes at least one of n-hexane, methanol and acetonitrile; the column temperature is 30°C to 40°C; and the injection volume is 1 μL to 10 μL.

[0019] In one implementation of the present application, the mass spectrometry conditions of the liquid chromatography-mass spectrometry method include: collision energy: 20eV to 30eV; scanning mode: positive ion scanning mode; monitoring mode: multiple reaction monitoring mode.

[0020] The beneficial effects of this application are:

[0021] The method for detecting the content of polycyclic aromatic hydrocarbons in atomized matrix aerosol of the present application can effectively extract polycyclic aromatic hydrocarbons from atomized matrix aerosol and accurately detect polycyclic aromatic hydrocarbons. BRIEF DESCRIPTION OF THE DRAWINGS

[0022] Figure 1 It is a flow chart of the method for detecting the content of polycyclic aromatic hydrocarbons in atomized matrix aerosol involved in the present application.

[0023] Figure 2 It is a flow chart of a method for detecting a test solution using liquid chromatography-mass spectrometry (LC-MS) involved in the present application.

[0024] Figure 3 It is a schematic structural diagram of the extraction of polycyclic aromatic hydrocarbons in atomized matrix aerosol involved in this application.

[0025] Description of reference numerals:

[0026] 1…electronic atomization device, 2…clamping device, 3…pipeline, 4…extraction device, 5…suction device. DETAILED DESCRIPTION

[0027] The present invention is further described in detail below by specific embodiments in conjunction with the accompanying drawings. In the following embodiments, many detailed descriptions are intended to enable the present application to be better understood. However, those skilled in the art can readily appreciate that some of the features may be omitted in different circumstances, or may be replaced by other materials or methods. In some cases, some operations related to the present application are not shown or described in the specification. This is to avoid the core of the present application being overwhelmed by excessive descriptions, and for those skilled in the art, it is not necessary to describe these related operations in detail. They can fully understand the related operations based on the description in the specification and the general technical knowledge in the art.

[0028] In addition, the features, operations, or characteristics described in the specification may be combined in any appropriate manner to form various embodiments. Furthermore, the steps or actions in the method description may be reordered or adjusted in a manner readily apparent to those skilled in the art. Therefore, the various sequences in the specification and drawings are provided solely for the purpose of clearly describing a particular embodiment and are not intended to be mandatory, unless otherwise specified.

[0029] The serial numbers assigned to the components in this document, such as "first", "second", etc., are only used to distinguish the objects described and do not have any order or technical meaning.

[0030] Currently, there are few methods for detecting PAHs in electronic atomization matrix aerosols. Existing methods use a wide variety of solvents, have complex procedures, and are time-consuming. Existing methods also suffer from numerous interfering impurities, which affect the accuracy of test results. Furthermore, the PAH content in atomization matrix aerosols is relatively low, making it difficult for existing methods to effectively extract and enrich them. Therefore, developing a method that can quickly and accurately detect PAHs in atomization matrix aerosols is of great significance.

[0031] In view of this, the present application creatively proposes a method for detecting the content of polycyclic aromatic hydrocarbons in atomized matrix aerosol, which uses a mixed solvent of ethanol + n-hexane to collect electronic cigarette aerosol, with fewer solvent types and simple operation, which greatly shortens the detection time; the use of solid phase microextraction technology can effectively avoid the influence of interfering impurities (propylene glycol, glycerol, nicotine, flavors, fragrances, etc.), improve the accuracy of the detection results, and enrich polycyclic aromatic hydrocarbons through solid phase microextraction. Even if the content of polycyclic aromatic hydrocarbons in electronic cigarette aerosol is low, it can be effectively extracted and detected; the present application adopts liquid chromatography-mass spectrometry (LC-MS) for detection. The method has simple operating steps and good repeatability, and does not require complex optimization of detection program parameters; the detection method of the present application has high separation (under specific detection conditions, the polycyclic aromatic hydrocarbons to be tested can be completely separated from other impurities or coexisting substances without interfering with each other) and good linearity (correlation coefficient R 2 The results show that the detection limit of PAHs is low (the detection limit is 0.05 ng / mL), the detection rate is high (the recovery rate is 90% to 110%), the relative standard deviation (RSD) is less than 10%), and the detection limit is low (the minimum detection limit is 0.05 ng / mL PAHs).

[0032] The present application relates to a method for detecting the content of polycyclic aromatic hydrocarbons in atomized matrix aerosol (hereinafter sometimes referred to as "detection method").

[0033] In one specific embodiment, the target of the detection method of the present application is polycyclic aromatic hydrocarbons in atomized matrix aerosol.

[0034] In one embodiment, an atomization substrate refers to a substance used to carry and deliver active ingredients during the atomization process. The atomization substrate may contain propylene glycol, glycerin, glycerol, nicotine or nicotine derivatives, flavorings, cooling agents, and sweeteners. During the atomization of the atomization substrate into an aerosol, polycyclic aromatic hydrocarbons (PAHs) may be produced. PAHs are harmful substances that may affect the user's health when inhaled into the user's body through the aerosol.

[0035] In a specific embodiment, the atomized substrate may refer to an atomized substrate of an electronic atomization device, which is a device that can convert the atomized substrate into an inhalable aerosol.

[0036] In a specific embodiment, polycyclic aromatic hydrocarbons may include benz(a)anthracene, At least one of benzo(b)fluoranthene and benzo(α)pyrene.

[0037] The detection method of the present application is further described below with reference to the accompanying drawings.

[0038] Figure 1 This is a flow chart of the method for detecting the content of polycyclic aromatic hydrocarbons in atomized matrix aerosols involved in this application. Figure 2 Schematic diagram of a method for detecting a test solution using liquid chromatography-mass spectrometry (LC-MS) according to the present application. Figure 3 It is a schematic structural diagram of the extraction of polycyclic aromatic hydrocarbons in atomized matrix aerosol involved in this application.

[0039] like Figure 1 As shown, the detection method of the present application may include: extraction: passing the atomized matrix aerosol into the extraction reagent to dissolve the target substance in the extraction reagent to obtain an extract (step S1); enrichment: extracting the extract using solid phase microextraction technology and eluting it to obtain an eluate (step S2); detection: detecting the eluate using liquid chromatography-mass spectrometry (step S3). In some cases, if the enrichment step is not performed (that is, if step S2 is not performed), the extract is directly detected.

[0040] As described above, the detection method of the present application includes step S1: extraction: passing the atomized matrix aerosol into an extraction reagent to dissolve the target substance in the extraction reagent to obtain an extract. In this way, the target substance in the atomized matrix aerosol can be extracted to obtain an extract for subsequent detection.

[0041] In a specific embodiment, in step S1, the following method can be used: Figure 3 The target compound is extracted by the structure shown in FIG. Figure 3 As shown, the electronic atomization device 1 carrying the atomized matrix can be fixed to the clamping device 2, so that the aerosol outlet of the electronic atomization device 1 is connected to the extraction device 4 through the pipe 3, and the extraction device 4 is connected to the suction device 5. The extraction device 4 contains an extraction reagent. Through the suction action of the suction device 5, the aerosol generated by the atomized matrix in the electronic atomization device 1 can enter the extraction reagent in the extraction device 4 through the pipe 3. The extraction reagent can dissolve the polycyclic aromatic hydrocarbons in the aerosol to obtain an extract.

[0042] In a specific embodiment, in step S1, the extraction reagent includes ethanol and n-hexane. It should be noted that the present application uses ethanol and n-hexane as extraction reagents, which can effectively dissolve polycyclic aromatic hydrocarbons in aerosols. The extraction reagent formula of the present application is simple and does not require the use of complex solvents.

[0043] In one specific embodiment, the volume ratio of ethanol to n-hexane in the extraction reagent is 3:7 to 7:3. For example, the volume ratio of ethanol to n-hexane in the extraction reagent can be 3:7, 4:6, 5:5, 6:4, or 7:3. This can better dissolve polycyclic aromatic hydrocarbons in the aerosol and improve detection accuracy.

[0044] In a specific embodiment, the volume ratio of ethanol to n-hexane in the extraction reagent is 5:5. This can better dissolve the polycyclic aromatic hydrocarbons in the aerosol and improve the accuracy of detection.

[0045] As described above, the detection method of the present application includes step S2: enrichment: extracting the extract using solid-phase microextraction technology and then eluting it to obtain an eluate. It should be noted that the use of solid-phase microextraction technology can further enrich the target, and even if the content of polycyclic aromatic hydrocarbons in the aerosol is low, it can still be effectively extracted and detected; it can also effectively avoid the influence of interfering substances (such as propylene glycol, glycerol, nicotine, flavors, fragrances, etc.) on the detection, thereby improving the accuracy of the detection.

[0046] In a specific embodiment, in step S2, the extract can be extracted using a C18 solid-phase extraction column. It should be noted that polycyclic aromatic hydrocarbons are highly hydrophobic and have extremely low polarity. Their non-polar properties are highly compatible with the hydrophobic adsorption mechanism of C18 fillers. Polycyclic aromatic hydrocarbons are easily adsorbed by C18 chains through hydrophobic interactions. Impurities such as propylene glycol and glycerol are highly hydrophilic substances and are not easily adsorbed by C18 (basically no retention when directly passed through the column). Therefore, the use of a C18 solid-phase extraction column can effectively enrich the target and reduce impurities.

[0047] In a specific embodiment, in step S2, before the extraction, the extract may be filtered, for example, using a 0.45 μm filter membrane to remove suspended matter or particles in the extract.

[0048] In a specific embodiment, in step S2, after the extract is extracted, dichloromethane may be used for elution to obtain an eluate, thereby effectively eluting the polycyclic aromatic hydrocarbons from the extraction column.

[0049] In a specific embodiment, in step S2, the eluted liquid can be concentrated. For example, the eluate can be concentrated to near dryness (volume within 0.2 mL) by nitrogen purge. Thus, the possibility of detection can be increased by concentration.

[0050] As described above, the detection method of the present application includes step S3: detection: the eluent is detected by liquid chromatography-mass spectrometry. It should be noted that the detection of polycyclic aromatic hydrocarbons by liquid chromatography-mass spectrometry (LC-MS) has significant advantages over traditional methods (such as gas chromatography-mass spectrometry (GC-MS), high performance liquid chromatography-ultraviolet visible detection (HPLC-UV)). Specifically: compared with GC-MS, LC-MS does not require high-temperature vaporization, which can avoid the risk of thermal decomposition of high-boiling polycyclic aromatic hydrocarbons (such as benzo[a]pyrene); multiple reaction monitoring can eliminate matrix interference through parent ion-daughter ion pairs, significantly improving the signal-to-noise ratio; polycyclic aromatic hydrocarbons can be directly separated by liquid chromatography without the need for silanization derivatization like GC-MS; LC-MS can analyze polycyclic aromatic hydrocarbons with 4 rings or more (such as benzo[a]pyrene), while GC-MS has poor separation effect on high-ring polycyclic aromatic hydrocarbons.

[0051] In a specific embodiment, if Figure 2 As shown, the detection of the test solution by liquid chromatography-mass spectrometry (LC-MS) can specifically include: preparing a series of standard solutions containing internal standards and target substances (step S31); detecting the series of standard solutions by gas chromatography-mass spectrometry to obtain a standard curve (step S32); adding the internal standard to the eluent to obtain the test solution (step S33); detecting the test solution by gas chromatography-mass spectrometry to obtain the content of polycyclic aromatic hydrocarbons in the atomized matrix aerosol (step S34). It should be noted that step S31 and step S33 can have no order, that is, step S31 can be performed before step S33, step S33 can be performed before step S1, or step S31 and step S33 can be performed simultaneously.

[0052] In a specific embodiment, the liquid chromatography-mass spectrometry detection can be performed using an internal standard method. It should be noted that the internal standard method can use an internal standard substance of known concentration as a reference for simultaneous analysis with the target substance in the sample to correct the analysis results, which is conducive to improving the accuracy and reliability of the results.

[0053] In one embodiment, the test solution may contain an internal standard (IS). It should be noted that adding an internal standard to the test solution has the following advantages: eliminating injection errors, correcting instrument fluctuations, monitoring sample loss, improving analytical precision, correcting interference, and improving detection accuracy.

[0054] In a specific embodiment, the standard solution may contain an internal standard, thereby improving the detection accuracy through the stability of the internal standard calibration curve.

[0055] In a specific embodiment, the internal standard may include naphthalene-d8, At least one of benzo(b)fluoranthene-d12, benzo(b)fluoranthene-d12, and benzo(a)pyrene-d12. It should be noted that isotopic internal standards can effectively correct for matrix effects, pretreatment losses, and instrument fluctuations by synchronously tracking the entire analysis process, thereby improving data accuracy.

[0056] In one embodiment, when preparing a series of standard solutions, the concentration of the internal standard in different standard solutions is the same.

[0057] In one embodiment, when preparing a series of standard solutions, the concentrations of the target substance in different standard solutions are different.

[0058] In one embodiment, when preparing a series of standard solutions, the concentrations of the target substances in the same standard solution are the same.

[0059] In a specific embodiment, the concentration of the target substance in a series of standard solutions can range from 0 ng / L to 100 ng / L. It should be noted that, in this way, the standard curve can cover the concentration range of polycyclic aromatic hydrocarbons that may be present in the aerosolized matrix.

[0060] In a specific embodiment, the concentrations of the target substance in the series of standard solutions may be 0.1 ng / L, 1 ng / L, 5 ng / L, 10 ng / L, 50 ng / L and 100 ng / L, respectively.

[0061] In a specific embodiment, the concentration of the internal standard in the standard solution can be a value within the range of 5 ng / L to 50 ng / L. For example, the concentration of the internal standard in the standard solution can be 5 ng / L, 10 ng / L, 15 ng / L, 20 ng / L, 25 ng / L, 30 ng / L, 35 ng / L, 40 ng / L, 45 ng / L, or 50 ng / L. It should be noted that the concentration of the internal standard in the standard solution is preferably in the middle of the range covered by the standard curve.

[0062] In one embodiment, the concentration of the internal standard in the test solution is consistent with the concentration of the internal standard in the standard solution.

[0063] In one embodiment, the concentration of the internal standard in the standard solution is 10 ng / L.

[0064] In a specific embodiment, a liquid chromatography-mass spectrometer can be used to detect the standard solution to obtain a standard curve.

[0065] In a specific embodiment, a liquid chromatography-mass spectrometer can be used to detect the test solution, and the concentration of the target substance in the test solution can be obtained based on the test results and the standard curve, thereby obtaining the concentration or content of the target substance in the atomized matrix aerosol.

[0066] In one specific embodiment, the test solution can be filtered through a 0.22 μm filter membrane before liquid chromatography-mass spectrometry detection. This can remove microparticles, dust, and insoluble impurities from the sample, helping to protect instrument components such as the chromatographic column, injection port liner, and ion source. It can also improve detection stability and reproducibility, reduce ghost peaks and noise caused by particulate matter, and enhance data quality.

[0067] In a specific embodiment, the chromatographic conditions in the liquid chromatography-mass spectrometry method may include: the chromatographic column is a C18 chromatographic column or a chromatographic column equivalent to a C18 chromatographic column.

[0068] In a specific embodiment, the chromatographic conditions in liquid chromatography-mass spectrometry may include: the mobile phase includes an organic solvent and water.

[0069] In a specific embodiment, the organic solvent includes at least one of n-hexane, methanol, and acetonitrile.

[0070] In a specific embodiment, the volume ratio of the organic solvent to water in the mobile phase is 10:90 to 90:10. It should be noted that by selecting an appropriate ratio of the mobile phase, a good separation effect can be achieved for the detection of polycyclic aromatic hydrocarbons.

[0071] In a specific embodiment, the liquid phase elution method can be gradient elution. It should be noted that by selecting an appropriate elution method, a good separation effect can be achieved for the detection of polycyclic aromatic hydrocarbons.

[0072] In a specific embodiment, the liquid phase elution mode can be: 0 min to 2 min, 30% B, 70% A; 2 min to 15 min, 30% to 95% B, 70% to 5% A; 15 min to 18 min, 95% B, 5% A; 18 min to 18.5 min, 95% to 30% B, 5% to 70% A; 18.5 min to 25 min, 30% B, 70% A. Wherein A is an organic solvent, B is water, and each percentage refers to the volume fraction.

[0073] In a specific embodiment, the flow rate of the mobile phase can be 0.1 mL / min to 0.8 mL / min. For example, the flow rate of the mobile phase can be 0.1 mL / min, 0.2 mL / min, 0.3 mL / min, 0.4 mL / min, 0.5 mL / min, 0.6 mL / min, 0.7 mL / min, or 0.8 mL / min. It should be noted that by selecting an appropriate flow rate, good separation effect can be achieved for the detection of polycyclic aromatic hydrocarbons.

[0074] In a specific embodiment, the column temperature can be 30° C. to 40° C. For example, the column temperature can be 30° C., 31° C., 32° C., 33° C., 34° C., 35° C., 36° C., 37° C., 38° C., 39° C., or 40° C. It should be noted that by selecting an appropriate column temperature, a good separation effect can be achieved for the detection of polycyclic aromatic hydrocarbons.

[0075] In a specific embodiment, the injection volume can be 1 μL to 10 μL. It should be noted that by selecting an appropriate injection volume, a good separation effect and linear relationship can be achieved for the detection of polycyclic aromatic hydrocarbons.

[0076] In a specific embodiment, the mass spectrometry conditions in the liquid chromatography-mass spectrometry method may include: a collision energy of 20 eV to 30 eV, a positive ion scanning mode, and a monitoring mode of multiple reaction monitoring mode.

[0077] In one embodiment, the parent ions (m / z) are: benz(a)anthracene: 228; 228; Benzo(b)fluoranthene: 252; Benzo(α)pyrene: 252.

[0078] In one embodiment, the product ions (m / z) are: benz(a)anthracene: 228, 114; 228, 114; Benzo(b)fluoranthene: 252, 126; Benzo(α)pyrene: 252, 126.

[0079] In a specific embodiment, in the detection method of the present application, a test result of the peak time (retention time) of benz(a)anthracene is 6.2 minutes.

[0080] In a specific embodiment, in the detection method of the present application, One test result of the peak time (retention time) was 10.5 minutes.

[0081] In a specific embodiment, in the detection method of the present application, a test result of the peak time (retention time) of benzo(b)fluoranthene is 13.6 minutes.

[0082] In a specific embodiment, in the detection method of the present application, a test result of the peak time (retention time) of benzo(α)pyrene is 18.6 minutes.

[0083] In a specific embodiment, the detection method of the present application can detect PAHs at a minimum concentration of 0.05 ng / mL.

[0084] The present invention is further described in detail below by specific experimental process and experimental data examples. The following examples are only used to further illustrate the present invention and should not be construed as limiting the present invention. In the present embodiment, unless otherwise specified, the reagents and instruments used are all commercially available, and the experimental operations are all carried out in accordance with the product specifications and conventional experimental specifications.

[0085] Example:

[0086] (1) Collecting atomized matrix aerosol:

[0087] The electronic atomization device was connected to the aerosol collection device, 25 mL of a mixed solvent of ethanol and n-hexane (volume ratio 1:1) was added to the aerosol collection device, and then the electronic atomization device was turned on to allow the aerosol to enter the mixed solvent of ethanol and n-hexane to obtain an extract.

[0088] (2) Enrichment:

[0089] The extract was subjected to polycyclic aromatic hydrocarbon extraction using a Waters Sep-pak C18 solid phase extraction cartridge (Waters Corporation), and then the solid phase microextraction cartridge was eluted with 5 mL of dichloromethane solution, and the eluate was collected;

[0090] The eluate was purged with nitrogen at 40°C to concentrate the eluate to less than 0.2 mL;

[0091] To the concentrated eluate, 10 μL of internal standard naphthalene-d8 was added, and the volume was adjusted to 1 mL with n-hexane to obtain a test solution.

[0092] (3) Detection:

[0093] In this embodiment, liquid chromatography-mass spectrometry detection was performed using the instrument parameters shown in Table 1 below:

[0094] Table 1

[0095]

[0096]

[0097] ① Establish a standard curve: prepare target compounds (including benzo(a)anthracene, A series of standard solutions of benzo(b)fluoranthene and benzo(α)pyrene at concentrations of 0.1 ng / mL, 1 ng / mL, 5 ng / mL, 10 ng / mL, 50 ng / mL, and 100 ng / mL were prepared. The concentration of each target substance in the same standard solution was the same. For example, in a standard solution with a target concentration of 0.1 ng / mL, 0.1 ng / mL of benzo(b)fluoranthene, 0.1 ng / mL of benzo(a)pyrene, and 100 ng / mL of benzo(b)fluoranthene were contained. 0.1 ng / mL of benzo(b)fluoranthene and 0.1 ng / mL of benzo(α)pyrene. The internal standard naphthalene-d8 concentration in each of the series of standard solutions was 10 ng / mL. Liquid chromatography-mass spectrometry was performed on each standard solution according to the parameters in Table 1 above to obtain the peak areas of the target compound and the internal standard. The results are shown in Table 2:

[0098] Table 2

[0099]

[0100] The concentration ratio of the target substance and the internal standard substance was used as the horizontal axis, and the peak area ratio of the target substance and the internal standard substance was used as the vertical axis to establish a standard curve. The linear equation of the standard curve of benz(a)anthracene was y=0.3945x+0.0032, R 2 is 0.9998; The linear equation of the standard curve is y = 1.6705x + 0.0289, R 2 The linear equation of the standard curve of benzo(b)fluoranthene is y=0.8856x+0.0043, R 2 is 0.9999, the linear equation of the standard curve of benzo(α)pyrene is y=0.8812x+0.0021, R 2 It can be seen that the standard curves of the target substances are all linear.

[0101] Detection of the test solution: The test solution obtained by the above extraction and enrichment is subjected to liquid chromatography-mass spectrometry detection according to the parameters in Table 1, and the concentration of the target substance in the test solution is obtained according to the corresponding standard curve.

[0102] ② Accuracy analysis: The intermediate linear concentration (5 nm / mL) was added to the blank sample matrix and liquid chromatography-mass spectrometry was performed. Table 3 below shows the accuracy results of each target:

[0103] Table 3

[0104]

[0105] As can be seen from the above table, the recovery rates of the target substances all meet the requirements of 90% to 110%, indicating that the accuracy of this method is good.

[0106] ③ Precision Analysis: An equal amount of target compound at the same concentration (5 nm / mL) was added to the blank sample matrix and subjected to liquid chromatography-mass spectrometry detection. The following data were obtained. Table 4 shows the relative standard deviation (RSD) (%):

[0107] Table 4

[0108]

[0109] As can be seen from Table 4, the RSDs of the target substances all met the requirement of <10%, indicating that the precision of this method is good.

[0110] ④Separation effect analysis:

[0111] Retention time: Benz(a)anthracene is 6.2 min, is 10.5 min, benzo(b)fluoranthene is 13.6 min, and benzo(α)pyrene is 18.6 min.

[0112] Conclusion: There are no interfering peaks within ±0.3 min of the retention time of each target compound, with good baseline separation and strong selectivity.

[0113] Therefore, the detection method of this embodiment has high sensitivity, strong anti-interference ability and good selectivity.

[0114] ⑤ Detection limit analysis:

[0115] Limit of detection (LOD): Calculated at a signal-to-noise ratio of 3 (S / N=3), the LOD for each target was 0.05 ng / mL.

[0116] Limit of quantification (LOQ): Calculated at a 10-fold signal-to-noise ratio (S / N=10), the LOQ for each target was 0.1 ng / mL.

[0117] Conclusion: The sensitivity of this method meets the requirements for the detection of trace PAHs.

[0118] The above content is a further detailed description of the present application in conjunction with specific implementation methods, and the specific implementation of the present application cannot be considered to be limited to these descriptions. For ordinary technicians in the technical field to which the present application belongs, several simple deductions or substitutions can be made without departing from the concept of the present application.

Claims

1. A method for detecting the content of polycyclic aromatic hydrocarbons in atomized matrix aerosol, characterized in that: include: Extraction: The atomized matrix aerosol is introduced into an extraction reagent to dissolve the target substance in the extraction reagent to obtain an extract; wherein the target substance includes polycyclic aromatic hydrocarbons and the extraction reagent includes ethanol and n-hexane; Detection: The extract is detected by liquid chromatography-mass spectrometry, including: preparing a series of standard solutions containing an internal standard and the target substance, wherein the target substance comprises polycyclic aromatic hydrocarbons; wherein the concentration of the internal standard is the same and the concentration of the target substance is different in different standard solutions; A series of standard solutions are tested using liquid chromatography-mass spectrometry, and a standard curve is obtained according to the test results; adding the internal standard substance to the extract to obtain a solution to be tested; The solution to be tested is tested by liquid chromatography-mass spectrometry, and the concentration of polycyclic aromatic hydrocarbons in the solution to be tested is determined according to the test result and the standard curve.

2. The detection method according to claim 1, wherein After the extraction step, an enrichment step is also included, and the enrichment step includes: extracting and eluting the extract by solid phase microextraction technology to obtain an eluate for detection.

3. The detection method according to claim 1, wherein The polycyclic aromatic hydrocarbons include at least one of benzo(a)anthracene, benzo(b)fluoranthene and benzo(α)pyrene; And / or, the internal standard comprises naphthalene-d8, -d12, at least one of benzo(b)fluoranthene-d12 and benzo(a)pyrene-d12.

4. The detection method according to claim 1, wherein In the extraction reagent, the volume ratio of ethanol to n-hexane is 3:7 to 7:3; And / or, in the extraction reagent, the volume ratio of ethanol to n-hexane is 5:

5.

5. The detection method according to claim 2, wherein The extract is extracted using a C18 solid phase extraction column.

6. The detection method according to claim 2, wherein In the enrichment step, dichloromethane was used for elution.

7. The detection method according to claim 2 or 6, wherein The enrichment step further includes concentrating the eluted liquid to obtain the eluate.

8. The detection method according to claim 1, wherein In a series of the standard solutions, the concentrations of the target substance include 0.1 ng / L, 1 ng / L, 5 ng / L, 10 ng / L, 50 ng / L and 100 ng / L, and the concentration of the internal standard is within the range of 5 ng / L to 50 ng / L.

9. The detection method according to any one of claims 1 to 8, wherein The chromatographic conditions of the liquid chromatography-mass spectrometry method include: the chromatographic column is a C18 chromatographic column or a chromatographic column equivalent to the C18 chromatographic column; the mobile phase includes an organic solvent and water, and the organic solvent includes at least one of n-hexane, methanol and acetonitrile; the flow rate is 0.1 mL / min to 0.8 mL / min; the column temperature is 30°C to 40°C; and the injection volume is 1 μL to 10 μL.

10. The detection method according to any one of claims 1 to 8, wherein The mass spectrometry conditions of the liquid chromatography-mass spectrometry method include: collision energy: 20eV to 30eV; scanning mode: positive ion scanning mode; monitoring mode: multiple reaction monitoring mode.

Images