CN113092633A - Method for detecting aromatic acid content in atmospheric particulates - Google Patents
Method for detecting aromatic acid content in atmospheric particulates Download PDFInfo
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
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- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
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- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The embodiment of the invention discloses a method for detecting the content of aromatic acid in atmospheric particulates, which belongs to the technical field of organic component detection and is convenient for effectively determining the content of aromatic acid in the atmospheric particulates. The method comprises the following steps: performing ultrasonic extraction on the collected atmospheric particle sample to obtain an extraction liquid; drying the extract liquor by using nitrogen to obtain a dry sample; adding a derivatization agent into the dry sample, and putting the dry sample added with the derivatization agent into an oven for derivatization reaction to obtain a dry sample derivative; and (3) carrying out qualitative and quantitative analysis on the dry sample derivative by using a gas chromatography-mass spectrometry method to obtain the aromatic acid in the atmospheric particulates and the content of each component of the aromatic acid. The invention is suitable for measuring and analyzing the aromatic acid components and the content in the atmospheric particulates.
Description
Technical Field
The invention belongs to the technical field of organic component detection, and particularly relates to a method for detecting the content of aromatic acid in atmospheric particulates.
Background
Atmospheric fines are one of the first pollutants responsible for urban haze and can affect the earth's radiation balance by scattering or absorbing solar radiation. Meanwhile, a large number of epidemiological studies prove that the atmospheric particulates are closely related to a series of diseases (cardiovascular diseases, respiratory diseases and the like) which are harmful to human health. The atmospheric particulates have complex chemical compositions, different from inorganic components, and various organic matters in the atmospheric particulates and complex structures.
Organic acids are important organic components of atmospheric particulates and play an important role in urban atmospheric chemistry. Because of the high polarity and surface tension of the pollutants, the hygroscopicity of the particles can be obviously changed, the earth radiation balance is influenced, and the atmospheric visibility is reduced and the global climate change is caused. The method for accurately measuring the content of various organic acid compounds in the atmospheric particulates has important significance for identifying the source and the formation process of the atmospheric particulates. The existing detection technology mainly aims at the linear acid compounds in the dibasic acid such as water-soluble organic acids like oxalic acid, malonic acid, succinic acid and the like, but the quantitative detection method aiming at various aromatic acid compound monomers (the monomers refer to components of the aromatic acid) in the atmospheric particulates is not mature.
Disclosure of Invention
In view of this, the embodiment of the invention provides a method for detecting the content of aromatic acid in atmospheric particulates, which is convenient for effectively determining the content of aromatic acid in atmospheric particulates.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for detecting the content of aromatic acid in atmospheric particulates comprises the following steps:
and (3) extraction: carrying out ultrasonic extraction on the collected atmospheric particle sample to obtain aromatic acid extract;
nitrogen blowing: drying the extract liquor by using nitrogen to obtain a dry sample;
derivatization: adding a derivatization agent into the dry sample, and putting the dry sample added with the derivatization agent into an oven for derivatization reaction to obtain a dry sample derivative;
and (3) determination: and (3) carrying out qualitative and quantitative analysis on the dry sample derivative by using a gas chromatography-mass spectrometry method to obtain the aromatic acid in the atmospheric particulates and the content of each component of the aromatic acid.
Optionally, prior to extracting, the method further comprises:
preparing a sample: placing the collected atmospheric particle sample into a refrigerator for refrigeration; the atmospheric particulate sample is attached to the filter membrane;
taking the refrigerated atmospheric particulate sample out of the refrigerator, cutting a filter membrane with a preset size and attached with the atmospheric particulate sample, and putting the filter membrane with the attached atmospheric particulate sample into a brown sample bottle by using tweezers;
a pipette was used to pipette 52 μ L of 10ppm recovery indicator to the atmospheric particulate sample to yield an atmospheric particulate sample for extraction.
Optionally, the recovery indicator is deuterated hexadecanoic acid.
Alternatively, in the nitrogen blowing step, the purity of the nitrogen gas is 99.999%.
Optionally, in the step of extracting, further comprising: adding an extracting agent into the collected atmospheric particulate sample before performing ultrasonic extraction on the collected atmospheric particulate sample;
after the extract was obtained, the extract was filtered into a transparent conical flask using a syringe equipped with a needle filter.
Optionally, the extractant is a mixed solution mainly prepared by mixing dichloromethane and methanol, wherein the volume ratio of dichloromethane to methanol is 4: 1, the extraction is carried out for 3 times, the addition amount of the first extractant is 4mL, the addition amounts of the second extractant and the third extractant are 2mL respectively, and each extraction time is 10 min.
Optionally, the deriving specifically includes: transferring 200 mu L of derivatization agent, adding the derivatization agent into the dry sample, and repeatedly washing for multiple times until mixed liquid formed by the derivatization agent and the dry sample flows down along the inner wall of the conical flask containing the dry sample;
transferring the mixed liquid to a brown chromatographic sample injection bottle, screwing down the cover of the brown chromatographic sample injection bottle, and wrapping the brown chromatographic sample injection bottle with a laboratory sealing film;
and then wrapping the brown chromatographic sample injection bottle with aluminum foil paper, and putting the bottle into a 70 ℃ oven for derivatization reaction for 2 hours to obtain a dry sample derivative.
Optionally, in the determining step, performing qualitative and quantitative analysis on the dry sample derivative by gas chromatography-mass spectrometry comprises:
the components of the dry sample derivative are characterized according to chromatographic peak retention time and characteristic ions of the target compound, and the components of the dry sample derivative are quantified based on an internal standard method.
Optionally, the derivatizing agent consists essentially of trimethylsilyltrifluoroacetamide, pyridine, and tetracosane-d50Mixing the prepared mixed solution according to the volume ratio of 2: 1: 1.144; the tetracosane-d50As an internal chromatographic standard, the concentration was 8 ppm.
Optionally, in the determining step, the gas chromatography conditions are: adopting a DB-5MS chromatographic column; the carrier gas is helium with the purity of 99.9999 percent, and the flow rate is 1.2 mL/min; adopting a non-shunting mode for sample injection, wherein the temperature of a sample injector is 275 ℃, and the sample injection amount is 2 mu L;
gas chromatography temperature rise control conditions: keeping at 80 deg.C for 5min, heating to 200 deg.C at 3 deg.C/min for 2min, heating to 310 deg.C at 10 deg.C/min, and keeping for 25 min.
Optionally, in the determining step, the mass spectrometry conditions are: electron bombardment positive ion source mode; the ratio of the number of protons to the number of charges ranges from 50 to 650 amu; the ion source temperature is 230 ℃; the temperature of the quadrupole rods is 150 ℃; the interfacial temperature is 280 ℃.
Alternatively, the aromatic acid comprises three phthalic acids, each being: o-phthalic acid, m-phthalic acid, and p-phthalic acid);
three kinds of benzene tricarboxylic acid are respectively: 1, 2, 3-benzenetricarboxylic acid, 1, 2, 4-benzenetricarboxylic acid and 1, 3, 5-benzenetricarboxylic acid; and the number of the first and second groups,
four phenolic acids, respectively: vanillic acid, syringic acid, 3-hydroxybenzoic acid and 4-hydroxybenzoic acid.
The method for detecting the content of aromatic acid in the atmospheric particulates comprises the steps of extraction, nitrogen blowing, derivation and determination, wherein the extraction liquid is obtained by performing ultrasonic extraction on an acquired atmospheric particulate sample; drying the extract liquor by using nitrogen to obtain a dry sample; adding a derivatization agent into the dry sample, and putting the dry sample added with the derivatization agent into an oven for derivatization reaction to obtain a dry sample derivative; and (3) carrying out qualitative and quantitative analysis on the dry sample derivative by using a gas chromatography-mass spectrometry method to obtain the aromatic acid in the atmospheric particulates and the content of each component of the aromatic acid. Therefore, the scheme of the embodiment is convenient for effectively measuring the content of the aromatic acid and each component of the aromatic acid in the atmospheric particulates, and the accuracy of the measuring result is higher.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a flowchart illustrating an embodiment of a method for detecting the content of aromatic acids in atmospheric particulates according to the present invention.
Detailed Description
Embodiments of the present invention will be described in detail below with reference to the accompanying drawings.
It should be understood that the described embodiments are merely exemplary of some, but not all embodiments of the invention, and that numerous specific details are set forth in order to provide a thorough understanding of the invention. In addition, some methods, means, components and applications thereof known to those skilled in the art are not described in detail in order to highlight the gist of the present invention, but the implementation of the present invention is not affected. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example one
The method for detecting the content of the aromatic acid in the atmospheric particulates, provided by the embodiment of the invention, is simple to operate, low in cost and suitable for determining and analyzing the components and the content of the aromatic acid in the atmospheric particulates.
In order to describe the technical scheme of the embodiment of the invention and prove the technical effect thereof, the description is given by combining with a specific scene of detecting the content of aromatic acid in atmospheric particulates in a laboratory, and it can be understood that the development place of the detection method is not limited to the laboratory.
Herein, unless otherwise stated, the detection and analysis are performed by using a chromatographically pure reagent meeting the national standard, and the chromatographically pure reagent generally refers to a special solvent or reagent for chromatography; the experimental water was ultrapure water.
The objects detected and analyzed in this embodiment are: aromatic acids (a composition) in atmospheric particulates. Generally, the aromatic acids that can be used in the assay include ten, respectively: three phthalic acids, including o-phthalic acid, m-phthalic acid, and p-phthalic acid; three kinds of benzene tricarboxylic acid are respectively: 1, 2, 3-benzenetricarboxylic acid [1, 2, 3-BTCA ], 1, 2, 4-benzenetricarboxylic acid [1, 2, 4-BTCA ], and 1, 3, 5-benzenetricarboxylic acid [1, 3, 5-BTCA ]); and four phenolic acids, vanillic acid [ vanillic acid ], syringic acid [ syringic acid ], 3-hydroxybenzoic acid [3-OHBA ] and 4-hydroxybenzoic acid [4-OHBA ], respectively.
Referring to fig. 1, in some embodiments, the method for detecting the content of aromatic acid in atmospheric particulates includes the steps of:
s110, extraction: and carrying out ultrasonic extraction on the collected atmospheric particle sample to obtain aromatic acid extract.
Wherein, the atmospheric particulate sample is collected by a filter membrane, and the collected atmospheric particulate sample is attached to the filter membrane, which is also called as a filter membrane sample (hereinafter, this scheme is also described in detail by referring to this example).
Specifically, in the extraction step, the method further comprises the following steps: an extractant is added to the collected sample of atmospheric particulates prior to subjecting the sample of atmospheric particulates to ultrasonic extraction.
In some embodiments, the extractant is a mixture solution prepared by mixing dichloromethane and methanol, and the mixture solution is prepared by adding methanol and dichloromethane. The volume ratio of the dichloromethane to the methanol is 4: 1, and the dichloromethane and the methanol are both chromatographic pure reagents.
In the ultrasonic extraction step, the total extraction is carried out for 3 times, the adding amount of the first extracting agent is 4mL, and the adding amounts of the second extracting agent and the third extracting agent are respectively 2mL, and each extraction time is 10 min.
Before step S110, the method further comprises: s100, preparing a sample:
the method specifically comprises the following steps: placing the collected atmospheric particle sample into a refrigerator for refrigeration; the atmospheric particulate sample is attached to a filter membrane.
Taking the refrigerated atmospheric particulate sample out of the refrigerator, cutting a filter membrane with a preset size and attached with the atmospheric particulate sample, and putting the filter membrane with the attached atmospheric particulate sample into a brown sample bottle by using tweezers; a pipette was used to pipette 52 μ L of 10ppm recovery indicator to the atmospheric particulate sample to yield an atmospheric particulate sample for extraction. In some embodiments, 1/4 of the filter membrane with the sample of atmospheric particulates attached thereto is cut.
Before the detection is started, preparing the following standard solutions for standby, wherein the standard solutions comprise:
aromatic acid standard stock solution: 10mg of phthalic acid was accurately weighed and dissolved in 10ml of acetonitrile solvent to prepare a standard stock solution having a concentration of 1000 ppm. Standard stock solutions of the remaining 9 aromatic acids were also prepared in the same manner and refrigerated in a refrigerator with a shelf life of 1 year.
Aromatic acid mixed standard sample: a small amount of acetonitrile is added into a 5ml volumetric flask, so that the standard stock solution is prevented from volatilizing when being added; and transferring 100 mu L of terephthalic acid standard stock solution to a volumetric flask by using a liquid transfer gun, adding 50 mu L of the remaining 9 aromatic acid standard stock solutions, and adding acetonitrile to a constant volume of 5ml to obtain the aromatic acid mixed standard sample.
Transferring the aromatic acid mixed standard sample into a brown sample bottle, and refrigerating in a refrigerator for 2 weeks. The concentration of terephthalic acid in the aromatic acid mixed standard sample is 20ppm, and the concentration of the rest 9 aromatic acids is 10 ppm. The component content in the aromatic acid mixed standard sample can be adjusted according to the different content of each component of the aromatic acid in the actual sample. In the experiment, the actually collected sample has high terephthalic acid content, so that the concentration content of the terephthalic acid in the aromatic acid mixed standard sample is higher than that of other components;
aromatic acid recovery indicates standard solution: 10mg of deuterated hexadecanoic acid (palmitic acid-d 31) was accurately weighed, dissolved in 10ml of acetonitrile solvent, prepared as an aromatic acid recovery rate indicating standard solution with a concentration of 1000ppm, and refrigerated in a refrigerator for a shelf life of 1 year.
Wherein acetonitrile (C) is employed2H3N) is a chromatographic pure reagent.
After the extract liquid is obtained, the method further comprises the following steps: the extract was filtered into a transparent conical flask using a syringe equipped with a needle filter. The needle filter adopts a Millipore 0.2 mu m polytetrafluoroethylene (English short for PTFE) hydrophobic needle filter.
S120, nitrogen blowing: subjecting the extract to nitrogen gas (N)2) And drying to obtain a dry sample.
In this example, the purity of nitrogen is 99.999%, which is commonly referred to as high-purity nitrogen. When the nitrogen is used for drying, the nitrogen cannot be blown too fast, and about 3 hours are needed.
S130, derivation: and adding a derivatization agent into the dry sample, and putting the dry sample added with the derivatization agent into an oven for derivatization reaction to obtain the dry sample derivative.
In this example, the derivatizing agent consists essentially of trimethyl (N-methyl-N-) silyltrifluoroacetamide, pyridine, and tetracosane-d50Mixing the prepared mixed solution according to the volume ratio of 2: 1: 1.144; the tetracosane-d50As an internal chromatographic standard, the concentration was 8 ppm.
Wherein, pyridine (C)5H5N) a chromatogram of 99%; color of N-methyl-N- (trimethylsilyl) trifluoroacetamide (MSTFA)The spectrum was 97%.
S140, measurement: and (3) carrying out qualitative and quantitative analysis on the dry sample derivative by using a gas chromatography-mass spectrometry method to obtain the aromatic acid in the atmospheric particulates and the content of each component of the aromatic acid.
In this example, the gas chromatography conditions were: adopting a DB-5MS chromatographic column; the carrier gas is helium with the purity of 99.9999 percent, commonly called high-purity nitrogen, and the flow rate is 1.2 mL/min; adopting a non-shunting mode for sample injection, wherein the temperature of a sample injector is 275 ℃, and the sample injection amount is 2 mu L;
gas chromatography temperature rise control conditions: keeping at 80 deg.C for 5min, heating to 200 deg.C at 3 deg.C/min for 2min, heating to 310 deg.C at 10 deg.C/min, and keeping for 25 min.
The mass spectrum conditions are as follows: electron bombardment positive ion source mode; the ratio of the number of protons to the number of charges (m/z) ranges from 50 to 650 amu; the ion source temperature is 230 ℃; the temperature of the quadrupole rods is 150 ℃; the interfacial temperature is 280 ℃.
The method for detecting the content of aromatic acid in atmospheric particulates provided by the embodiment comprises the steps of extraction, nitrogen blowing, derivation and determination, wherein the extraction liquid is obtained by performing ultrasonic extraction on an acquired atmospheric particulate sample; drying the extract liquor by using nitrogen to obtain a dry sample; adding a derivatization agent into the dry sample, and putting the dry sample added with the derivatization agent into an oven for derivatization reaction to obtain a dry sample derivative; and (3) carrying out qualitative and quantitative analysis on the dry sample derivative by using a gas chromatography-mass spectrometry method to obtain the aromatic acid in the atmospheric particulates and the content of each component of the aromatic acid.
Therefore, the scheme of the embodiment is convenient for effectively measuring the content of the aromatic acid and each component of the aromatic acid in the atmospheric particulates, and the accuracy of the measuring result is higher.
In this embodiment, the instruments and devices used mainly include: a gas chromatography-mass spectrometer, wherein a chromatographic column of the gas chromatography-mass spectrometer is a J & W DB-5MS quartz capillary chromatographic column (30m multiplied by 0.25mm multiplied by 0.25 mu m); a constant temperature oven; a nitrogen blowing instrument; an ultrasonic cleaning machine and a ten thousand-level balance; other common laboratory instruments and devices, such as measuring cups, etc.
In order to more fully illustrate the technical solution of the embodiments of the present invention, taking the laboratory detection of the aromatic acid content in the atmospheric particulates as an example, the method for detecting the aromatic acid content in the atmospheric particulates, which is an embodiment developed in the laboratory based on the prepared apparatus and equipment, specifically includes the following steps:
1. sample preparation
Taking out the aluminum foil paper baked by the oven as a working platform, and cleaning scissors, tweezers and the like with methanol before and after use respectively. The collected sample of atmospheric particulates was removed from the refrigerator, the 1/4 filter samples were cut using scissors, and the cut samples were placed into brown sample bottles with tweezers. The sample bottle and the cap are marked (sample number). A pipette was used to pipette 52. mu.L of the 10ppm aromatic acid recovery indicating the intermediate solution (palmitic acid-d 31) onto the filter sample. Care was taken to allow the tip of the pipette to touch the filter and avoid touching the vial wall to allow sufficient penetration of the recovery indicator into the filter. And after the recovery rate indicator is added, replacing the pipette tip by one again, and adding the next sample.
2. Ultrasonic extraction
4mL of an extractant was added to the brown bottle to which the sample had been added, the cap was closed, and ultrasonic extraction was performed for 10 min. At the same time, N (number of samples) syringes and N needle filters were removed, the needle tubes were separated from the injection punch, and 0.2 μm PTFE (Polytetrafluoroethylene) needle filters were loaded. N transparent conical bottles are prepared, each bottle is marked and placed on a metal rack for standby.
After extraction, wiping water outside the brown sample bottle, pouring the extract into a needle tube for filtering, and then extruding the extract into a transparent conical bottle by using a needle tube punch; during this process, please take care not to pour out the filter.
2mL of extractant is added into the brown sample bottle, the cover is closed tightly, and ultrasonic extraction is carried out for 10 min. Meanwhile, the needle filter on the needle tube is detached, the punch is pulled out, and then the filter is screwed on. Please note that instead of pulling the punch directly, the filter needs to be removed first and then pulled out. The punch is not allowed to touch other things, and only the upper end thereof is grasped to avoid contamination. The syringe, filter, brown sample bottle and transparent conical bottle corresponding to each punch cannot be disordered, and preferably are marked to avoid the disorder.
The second extract was transferred to a clear conical flask using a needle tube, and 2mL of extractant was added to the brown sample flask and sonicated for 10 min. Meanwhile, the needle filter is disassembled, the punch is pulled out, and then the filter is installed.
The last (i.e., third) extraction was poured into the syringe, while the filter sample was also scraped into the syringe with a spatula, and the extraction was squeezed into a transparent flask.
3. Nitrogen blowing
The extract from the flask was blown dry with high purity (99.999%) nitrogen for approximately 3 hours, which did not blow too quickly.
4. Derivatization reaction
A labeled brown chromatographic vial, cap and 200 μ L liner were prepared. After the samples were blow dried, 200. mu.L (100. mu.L. times.2) of derivatizing agent was removed and added to the blow dried samples. The washing is repeated for a plurality of times until the liquid smoothly flows down from the inner wall of the conical flask. The liquid was transferred to a brown chromatographic loading vial, the cap was screwed down and wrapped with a laboratory sealing film. Wrapping all bottles with aluminum foil paper, putting the bottles into a 70 ℃ oven for derivatization reaction for 2 hours, and then carrying out gas chromatography-mass spectrometry;
5. gas chromatography-mass spectrometry and analysis
The gas chromatography-mass spectrometry determination and analysis comprises two links of qualitative analysis and quantitative analysis; the conditions of the gas chromatography and the mass spectrometry are the conditions of the gas chromatography and the mass spectrometry described above, and are not repeated herein, and the contents disclosed above can be referred to.
And (3) qualitative analysis: first, a series of standard working solutions were prepared based on the preparation method of the standard solutions described above: in this experiment, the burned blank filter was cut 1/4 (6 blank filters were cut out 1/4 in total) and placed in 6 brown sample vials, respectively. mu.L of the intermediate solution (palmitic acid-d 31) was added to each blank filter sample, and 10ppm recovery of aromatic acid was indicated, and 0. mu.L, 8. mu.L, 28. mu.L, 52. mu.L, 76. mu.L, 100. mu.L of the aromatic acid was added to mix the standards. 4mL of extractant was added to each sample vial, and the remaining steps were the same as for the analysis of the filter samples. A series of standard working solutions were prepared with a concentration gradient of 0ppm, 0.8ppm, 2.8ppm, 5.2ppm, 7.6ppm, 10ppm for terephthalic acid, 0ppm, 0.4ppm, 1.4ppm, 2.6ppm, 3.8ppm, 5ppm for the remaining 9 aromatic acids, and a concentration of 2.208ppm for the internal standard tetracosan-d 50.
The series of standard working solutions were subjected to full-scan qualitative analysis using a gas chromatograph-mass spectrometer, and the retention time and characteristic ions of the standard were determined as shown in table 1.
| Serial number | Name of Compound | Retention time | Characteristic ion | Assist feature ion |
| 1 | Phthalic acid | 23.95min | 295 | 221 |
| 2 | Isophthalic acid | 25.55min | 295 | 221 |
| 3 | Terephthalic acid (TPA) | 26.15min | 295 | 221 |
| 4 | 1, 2, 3-benzenetricarboxylic acid | 32.90min | 411 | 426、337 |
| 5 | 1, 2, 4-benzenetricarboxylic acid | 33.63min | 411 | 426、337 |
| 6 | 1, 3, 5-benzenetricarboxylic acid | 34.47min | 411 | 426、337 |
| 7 | Vanillic acid | 25.62min | 297 | 223 |
| 8 | Syringic acid | 28.40min | 327 | 342、253 |
| 9 | 3-Hydroxybenzoic acid | 21.16min | 267 | 193 |
| 10 | 4-hydroxybenzoic acid | 22.58min | 267 | 193 |
TABLE 1
And (3) carrying out Selective Ion (SIM) monitoring analysis on the series of standard working solutions by using a gas chromatograph-mass spectrometer, calculating and drawing a standard working curve, and establishing a regression equation of the standard working curve as shown in table 2.
| Serial number | Name of Compound | Regression equation |
| 1 | Phthalic acid | 0.375x+0.105 |
| 2 | Isophthalic acid | 1.364x-0.014 |
| 3 | Terephthalic acid (TPA) | 2.022x+1.493 |
| 4 | 1, 2, 3-benzenetricarboxylic acid | 0.672x+0.425 |
| 5 | 1, 2, 4-benzenetricarboxylic acid | 0.421x+0.482 |
| 6 | 1, 3, 5-benzenetricarboxylic acid | 1.312x-0.337 |
| 7 | Vanillic acid | 0.691x-0.108 |
| 8 | Syringic acid | 0.496x-0.042 |
| 9 | 3-hydroxybenzoic acid | 1.182x-0.094 |
| 10 | 4-hydroxybenzoic acid | 1.102x-0.017 |
TABLE 2
Recovery was obtained by comparing the ratio of a given amount of the spiked aromatic acid mixed standard to the filter membrane sample, following the above sample treatment procedure, to the ratio of the same amount of spiked aromatic acid mixed standard directly without the filter membrane sample. Finding the lowest concentration which can be detected by the instrument by a standard sample dilution mode step by step, calculating by using a gas chromatography-mass spectrometer with a signal-to-noise ratio (S/N) of 3 (substantially 3: 1) to obtain a detection limit, and calculating by using a signal-to-noise ratio (S/N) of 10 to obtain a quantitative limit; the detection limit is the minimum concentration detected by a sample in a liquid phase, the signal-to-noise ratio is 3: 1, namely, the peak height of a signal peak (namely, a sample peak) is 3 times higher than that of a noise peak, a relatively flat section of base line can be selected as a standard reference for determining the peak height of the noise peak, the height of the noise peak of the base line is recorded after amplification, then the sample is diluted until the peak height of the sample is about three times higher than that of the noise peak, and the concentration of the sample is the detection limit at this time. The limit of quantitation refers to the lowest amount of analyte in the sample that can be quantitatively determined, and the limit of quantitation can be calculated by using the S/N ratio of 10 in a similar manner to the detection limit.
| Serial number | Name of Compound | Recovery rate | Detection limit (ng/m)3) | Limit of quantitation (ng/m)3) |
| 1 | Phthalic acid | 83.5±7.5 | 0.45 | 1.52 |
| 2 | Isophthalic acid | 80.9±1.8 | 0.51 | 1.89 |
| 3 | Terephthalic acid (TPA) | 82.9±2.7 | 0.80 | 2.49 |
| 4 | 1, 2, 3-benzenetricarboxylic acid | 79.8±2.3 | 0.87 | 2.88 |
| 5 | 1, 2, 4-benzenetricarboxylic acid | 95.8±5.8 | 0.51 | 1.61 |
| 6 | 1, 3, 5-benzenetricarboxylic acid | 95.3±5.7 | 0.48 | 1.59 |
| 7 | Vanillic acid | 81.6±6.1 | 0.47 | 1.49 |
| 8 | Syringic acid | 81.0±3.1 | 0.70 | 2.35 |
| 9 | 3-hydroxybenzoic acid | 83.8±7.0 | 0.56 | 1.63 |
| 10 | 4-hydroxybenzoic acid | 85.2±7.2 | 0.20 | 0.62 |
TABLE 3
Quantitative analysis: and (3) carrying out Selective Ion Monitoring (SIM) analysis on the filter membrane sample, substituting the peak area ratio of each substance to be detected and the internal standard into the standard working curve regression equation in the table 2, calculating to obtain the content of each substance to be detected (each component of aromatic acid), and evaluating the accuracy of the atmospheric particle sample according to the detection limit and the quantitative limit.
The method for detecting the content of the aromatic acid in the atmospheric particulates, provided by the embodiment of the invention, is simple and convenient to operate and low in cost, can effectively determine the content of the aromatic acid component in the atmospheric particulates according to the description, has accurate and reliable analysis results, has good detection repeatability through experimental verification, has low requirements on instruments, and has good application prospect and popularization value.
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. The term "comprising", without further limitation, means that the element so defined is not excluded from the group consisting of additional identical elements in the process, method, article, or apparatus that comprises the element. As will be appreciated by one of ordinary skill in the art, the situation may be specified.
The above description is only for the specific embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (10)
1. A method for detecting the content of aromatic acid in atmospheric particulates is characterized by comprising the following steps:
and (3) extraction: carrying out ultrasonic extraction on the collected atmospheric particle sample to obtain aromatic acid extract;
nitrogen blowing: drying the extract liquor by using nitrogen to obtain a dry sample;
derivatization: adding a derivatization agent into the dry sample, and putting the dry sample added with the derivatization agent into an oven for derivatization reaction to obtain a dry sample derivative;
and (3) determination: and (3) carrying out qualitative and quantitative analysis on the dry sample derivative by using a gas chromatography-mass spectrometry method to obtain the aromatic acid in the atmospheric particulates and the content of each component of the aromatic acid.
2. The method of claim 1, wherein prior to extracting, the method further comprises:
preparing a sample: placing the collected atmospheric particle sample into a refrigerator for refrigeration; the atmospheric particulate sample is attached to the filter membrane;
taking the refrigerated atmospheric particulate sample out of the refrigerator, cutting a filter membrane with a preset size and attached with the atmospheric particulate sample, and putting the filter membrane with the attached atmospheric particulate sample into a brown sample bottle by using tweezers;
a pipette was used to pipette 52 μ L of 10ppm recovery indicator to the atmospheric particulate sample to yield an atmospheric particulate sample for extraction.
3. The method of claim 2, wherein the recovery indicator is deuterated hexadecanoic acid.
4. The method according to claim 1, wherein the purity of the nitrogen gas in the nitrogen blowing step is 99.999%.
5. The method of claim 1, wherein in the step of extracting, further comprising: adding an extracting agent into the collected atmospheric particulate sample before performing ultrasonic extraction on the collected atmospheric particulate sample;
after the extract was obtained, the extract was filtered into a transparent conical flask using a syringe equipped with a needle filter.
6. The method according to claim 5, wherein the extractant is a mixed solution prepared by mixing dichloromethane and methanol, wherein the volume ratio of dichloromethane to methanol is 4: 1, the extraction is performed for 3 times, the addition amount of the first extractant is 4mL, and the addition amounts of the second extractant and the third extractant are 2mL respectively, and each extraction time is 10 min.
7. The method according to claim 1 or 5, wherein the deriving comprises in particular: transferring 200 mu L of derivatization agent, adding the derivatization agent into the dry sample, and repeatedly washing for multiple times until mixed liquid formed by the derivatization agent and the dry sample flows down along the inner wall of the conical flask containing the dry sample;
transferring the mixed liquid to a brown chromatographic sample injection bottle, screwing down the cover of the brown chromatographic sample injection bottle, and wrapping the brown chromatographic sample injection bottle with a laboratory sealing film;
and then wrapping the brown chromatographic sample injection bottle with aluminum foil paper, and putting the bottle into a 70 ℃ oven for derivatization reaction for 2 hours to obtain a dry sample derivative.
8. The method of claim 7, wherein the derivatizing agent consists essentially of trimethylsilyltrifluoroacetamide, pyridine, and tetracosane-d50Mixing the prepared mixed solution according to the volume ratio of 2: 1: 1.144; the tetracosane-d50As an internal chromatographic standard, the concentration was 8 ppm.
9. The method according to claim 1, wherein in the determining step, the gas chromatography conditions are: adopting a DB-5MS chromatographic column; the carrier gas is helium with the purity of 99.9999 percent, and the flow rate is 1.2 mL/min; adopting a non-shunting mode for sample injection, wherein the temperature of a sample injector is 275 ℃, and the sample injection amount is 2 mu L;
gas chromatography temperature rise control conditions: keeping at 80 deg.C for 5min, heating to 200 deg.C at 3 deg.C/min for 2min, heating to 310 deg.C at 10 deg.C/min, and keeping for 25 min.
10. The method of claim 1 or 9, wherein in the determining step, the mass spectrometry conditions are: electron bombardment positive ion source mode; the ratio of the number of protons to the number of charges ranges from 50 to 650 amu; the ion source temperature is 230 ℃; the temperature of the quadrupole rods is 150 ℃; the interfacial temperature is 280 ℃.
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