CN111929395A - Method for analyzing phthalic acid ester in soil by gas chromatography-mass spectrometry based on microwave extraction - Google Patents
Method for analyzing phthalic acid ester in soil by gas chromatography-mass spectrometry based on microwave extraction Download PDFInfo
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- CN111929395A CN111929395A CN202011011460.6A CN202011011460A CN111929395A CN 111929395 A CN111929395 A CN 111929395A CN 202011011460 A CN202011011460 A CN 202011011460A CN 111929395 A CN111929395 A CN 111929395A
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- 239000002689 soil Substances 0.000 title claims abstract description 30
- 238000000874 microwave-assisted extraction Methods 0.000 title claims abstract description 27
- 238000000034 method Methods 0.000 title claims abstract description 20
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 title claims abstract description 16
- XNGIFLGASWRNHJ-UHFFFAOYSA-N o-dicarboxybenzene Natural products OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 title abstract description 13
- -1 phthalic acid ester Chemical class 0.000 title abstract description 5
- 238000004458 analytical method Methods 0.000 claims abstract description 24
- 238000000605 extraction Methods 0.000 claims abstract description 11
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 8
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims abstract description 5
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000001914 filtration Methods 0.000 claims abstract description 4
- 238000000227 grinding Methods 0.000 claims abstract description 4
- 239000007788 liquid Substances 0.000 claims abstract description 4
- 239000012046 mixed solvent Substances 0.000 claims abstract description 4
- 238000002414 normal-phase solid-phase extraction Methods 0.000 claims abstract description 4
- 238000011049 filling Methods 0.000 claims abstract description 3
- 239000000203 mixture Substances 0.000 claims abstract description 3
- 239000007789 gas Substances 0.000 claims description 10
- 239000012159 carrier gas Substances 0.000 claims description 6
- 238000004817 gas chromatography Methods 0.000 claims description 6
- 150000003022 phthalic acids Chemical class 0.000 claims description 5
- 239000000243 solution Substances 0.000 claims description 5
- 239000002904 solvent Substances 0.000 claims description 4
- 230000005540 biological transmission Effects 0.000 claims description 3
- 239000001307 helium Substances 0.000 claims description 3
- 229910052734 helium Inorganic materials 0.000 claims description 3
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 3
- 238000002347 injection Methods 0.000 claims description 3
- 239000007924 injection Substances 0.000 claims description 3
- 150000002500 ions Chemical class 0.000 claims description 3
- 238000004949 mass spectrometry Methods 0.000 claims description 3
- 238000010408 sweeping Methods 0.000 claims description 3
- 125000005498 phthalate group Chemical class 0.000 claims 1
- 238000002203 pretreatment Methods 0.000 abstract description 8
- 238000012360 testing method Methods 0.000 abstract description 4
- XNGIFLGASWRNHJ-UHFFFAOYSA-L phthalate(2-) Chemical compound [O-]C(=O)C1=CC=CC=C1C([O-])=O XNGIFLGASWRNHJ-UHFFFAOYSA-L 0.000 description 4
- 238000000944 Soxhlet extraction Methods 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 239000003599 detergent Substances 0.000 description 1
- 229960001826 dimethylphthalate Drugs 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003480 eluent Substances 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- HCWCAKKEBCNQJP-UHFFFAOYSA-N magnesium orthosilicate Chemical compound [Mg+2].[Mg+2].[O-][Si]([O-])([O-])[O-] HCWCAKKEBCNQJP-UHFFFAOYSA-N 0.000 description 1
- 229910052919 magnesium silicate Inorganic materials 0.000 description 1
- 235000019792 magnesium silicate Nutrition 0.000 description 1
- 239000000391 magnesium silicate Substances 0.000 description 1
- 238000001819 mass spectrum Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000005022 packaging material Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 210000004994 reproductive system Anatomy 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 230000028327 secretion Effects 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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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
-
- 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)
- Pathology (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The invention relates to a gas chromatography-mass spectrometry analysis method for phthalic acid ester in soil based on microwave extraction, which comprises the following steps: step one, adding anhydrous sodium sulfate into a collected soil sample, uniformly mixing, dehydrating, grinding and uniformly mixing to obtain a granular mixture; step two, filling the soil to be detected processed in the step one into a microwave extraction tank, adding a normal hexane/acetone mixed solvent, and extracting by adopting a microwave extraction instrument under the set extraction condition; step three, filtering the extract obtained in the step two, concentrating, purifying by a solid phase extraction column, and concentrating to be detected; and step four, putting the liquid to be detected processed in the step three into a gas chromatography-mass spectrometer for analysis. The microwave extraction pretreatment method has the advantages of high automation degree, time and cost saving, high extraction efficiency and accurate analysis result, and is an efficient pretreatment method; the gas chromatography-mass spectrometer is adopted to carry out analysis and test on the sample, and the analysis accuracy is high, and the method is rapid and sensitive.
Description
Technical Field
The invention relates to a method for testing and analyzing phthalate esters in the field of soil monitoring, in particular to a method for analyzing phthalate esters in soil by gas chromatography-mass spectrometry based on microwave extraction.
Background
The phthalate esters are also called phthalate esters, are generally applied to products such as packaging materials, cosmetics, toys, detergents and the like, have interference effect on the secretion of human bodies after being contacted for a long time, and directly harm the reproductive systems of the human bodies.
At present, the method for analyzing the phthalate esters in the soil has no right in China, the pretreatment method is generally a Soxhlet extraction method, the time consumption is long, the operation is troublesome, the automation degree is low, the using amount of an organic solvent is large, and the health of an analyst is influenced by the volatilization of the solvent. It is highly desirable to find a more efficient and simple pretreatment method that can replace the conventional method.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a method for analyzing phthalic acid ester in soil by gas chromatography-mass spectrometry based on microwave extraction, and the specific technical scheme is as follows:
a method for analyzing phthalic acid esters in soil by gas chromatography-mass spectrometry based on microwave extraction comprises the following steps:
step one, adding anhydrous sodium sulfate into a collected soil sample, uniformly mixing, dehydrating, grinding and uniformly mixing to obtain a granular mixture;
step two, filling the soil to be detected processed in the step one into a microwave extraction tank, adding a normal hexane/acetone mixed solvent, and extracting by adopting a microwave extraction instrument under the set extraction condition;
step three, filtering the extract obtained in the step two, concentrating, purifying by a solid phase extraction column, and concentrating to be detected;
and step four, putting the liquid to be detected processed in the step three into a gas chromatography-mass spectrometer for analysis.
As an improvement of the present invention, the gas chromatography conditions in step four are: a chromatographic column: HP-5 MS: 30 m.times.0.25 mm.times.0.25 μm; carrier gas: helium gas; the carrier gas flow is 1.0 mL/min; sample introduction amount: 1 mu L of the solution; sample inlet temperature: 250 ℃; auxiliary temperature: 280 ℃, sample injection mode: split-flow sample introduction, split-flow ratio: 10:1.
As a modification of the present invention, in the gas chromatography analysis in the fourth step, the temperature of the column is raised by the following procedure: the initial temperature was 45 ℃ and after 2 minutes, the temperature was raised to 320 ℃ at 10 ℃/min and held for 5.5 minutes.
As an improvement of the present invention, the mass spectrometry conditions in the fourth step are: the scanning mode is as follows: fully sweeping; the scanning range is 35-500 amu; ionization energy: 70 eV; the ion source temperature is 250 ℃; temperature of the quadrupole rods: 150 ℃, transmission line temperature: 280 ℃, solvent retardation: for 10 min.
The invention has the beneficial effects that: the invention is a gas chromatography-mass spectrometry analysis method of phthalate in soil based on microwave extraction, compared with the traditional Soxhlet extraction pretreatment, the microwave extraction pretreatment method has the advantages of high automation degree, time and cost saving, high extraction efficiency and accurate analysis result, and is an efficient pretreatment method; the gas chromatography-mass spectrometer is adopted to carry out analysis and test on the sample, and the analysis accuracy is high, and the method is rapid and sensitive. The invention provides a gas chromatography-mass spectrometry analysis method for phthalate in soil based on microwave extraction, which fills the blank of a phthalate analysis method in soil in domestic standards.
Drawings
FIG. 1 is a spectrum of a gas chromatography-mass spectrometry analysis of phthalate esters in soil according to an embodiment of the present invention.
Wherein, 1-dimethyl phthalate; 2-diethyl phthalate; 3-diisobutylphthalate; 4-dibutyl phthalate; 5-butyl benzyl phthalate; 6-di (2-ethylhexyl) phthalate; 7-di-n-octyl phthalate.
The specific implementation mode is as follows:
the present invention is further explained by the following examples.
Examples
A method for analyzing phthalic acid esters in soil by gas chromatography-mass spectrometry based on microwave extraction comprises the following specific steps:
1. microwave extraction pretreatment:
adding anhydrous sodium sulfate into 5-10g of collected soil sample, mixing, dehydrating, grinding, and mixing to obtain granular soil; loading soil to be detected into a microwave extraction tank, adding 100ml of n-hexane/acetone mixed solvent (1:1), sealing the extraction tank, placing the extraction tank into a microwave extraction instrument, setting the preheating time for 5min, the extraction temperature for 110 ℃, and the extraction time for 10min, and extracting; and after the extraction is finished and the solution is cooled, passing the extract through a sand core funnel filled with anhydrous sodium sulfate for dewatering and filtering, concentrating to 1ml by using a concentrator, purifying and washing the concentrated solution through a magnesium silicate solid phase extraction column, collecting eluent, and concentrating to 1ml again to be detected.
2. Analysis conditions of the gas chromatography-mass spectrometer are as follows:
and (3) putting the pretreated liquid to be detected into a gas chromatography-mass spectrometer for analysis.
The analysis conditions of the gas chromatography-mass spectrometer are as follows: a chromatographic column: HP-5 MS: 30 m.times.0.25 mm.times.0.25 μm; carrier gas: helium gas; the carrier gas flow is 1.0 mL/min; sample introduction amount: 1 mu L of the solution; sample inlet temperature: 250 ℃; auxiliary temperature: 280 ℃, sample injection mode: split-flow sample introduction, split-flow ratio: 10:1. During gas chromatography, the column was heated using the following procedure: the initial temperature was 45 ℃ and after 2 minutes, the temperature was raised to 320 ℃ at 10 ℃/min and held for 5.5 minutes. The mass spectrum conditions are as follows: the scanning mode is as follows: fully sweeping; the scanning range is 35-500 amu; ionization energy: 70 eV; the ion source temperature is 250 ℃; temperature of the quadrupole rods: 150 ℃, transmission line temperature: 280 ℃, solvent retardation: for 10 min.
A method for analyzing phthalate esters in soil by adopting gas chromatography-mass spectrometry of microwave extraction is adopted, the spectrogram of gas chromatography-mass spectrometry of the phthalate esters in the soil is shown in figure 1, the recovery rate of the phthalate esters in the soil reaches 78.5-110.6%, and the precision of a parallel sample is 3.4-8.2%.
The invention is a gas chromatography-mass spectrometry analysis method of phthalate in soil based on microwave extraction, compared with the traditional Soxhlet extraction pretreatment, the microwave extraction pretreatment method has the advantages of high automation degree, time and cost saving, high extraction efficiency and accurate analysis result, and is an efficient pretreatment method; the gas chromatography-mass spectrometer is adopted to carry out analysis and test on the sample, and the analysis accuracy is high, and the method is rapid and sensitive.
The technical means disclosed by the scheme of the invention are not limited to the technical means disclosed by the technical means, and also comprise the technical scheme formed by equivalent replacement of the technical features. The present invention is not limited to the details given herein, but is within the ordinary knowledge of those skilled in the art.
Claims (4)
1. A method for analyzing phthalic acid esters in soil by gas chromatography-mass spectrometry based on microwave extraction is characterized by comprising the following steps:
step one, adding anhydrous sodium sulfate into a collected soil sample, uniformly mixing, dehydrating, grinding and uniformly mixing to obtain a granular mixture;
step two, filling the soil to be detected processed in the step one into a microwave extraction tank, adding a normal hexane/acetone mixed solvent, and extracting by adopting a microwave extraction instrument under the set extraction condition;
step three, filtering the extract obtained in the step two, concentrating, purifying by a solid phase extraction column, and concentrating to be detected;
and step four, putting the liquid to be detected processed in the step three into a gas chromatography-mass spectrometer for analysis.
2. The method for analyzing phthalic acid esters in soil by using gas chromatography and mass spectrometry based on microwave extraction as claimed in claim 1, wherein the gas chromatography analysis conditions in the fourth step are as follows: a chromatographic column: HP-5 MS: 30 m.times.0.25 mm.times.0.25 μm; carrier gas: helium gas; the carrier gas flow is 1.0 mL/min; sample introduction amount: 1 mu L of the solution; sample inlet temperature: 250 ℃; auxiliary temperature: 280 ℃, sample injection mode: split-flow sample introduction, split-flow ratio: 10:1.
3. The method for analyzing phthalates in soil based on microwave extraction gas chromatography-mass spectrometry of claim 1, wherein in the gas chromatography analysis in the fourth step, the temperature of the chromatographic column is raised by the following procedures: the initial temperature was 45 ℃ and after 2 minutes, the temperature was raised to 320 ℃ at 10 ℃/min and held for 5.5 minutes.
4. The method for analyzing phthalic acid esters in soil by using gas chromatography-mass spectrometry based on microwave extraction as claimed in claim 1, wherein the mass spectrometry conditions in the fourth step are as follows: the scanning mode is as follows: fully sweeping; the scanning range is 35-500 amu; ionization energy: 70 eV; the ion source temperature is 250 ℃; temperature of the quadrupole rods: 150 ℃, transmission line temperature: 280 ℃, solvent retardation: for 10 min.
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| CN202011011460.6A CN111929395A (en) | 2020-09-23 | 2020-09-23 | Method for analyzing phthalic acid ester in soil by gas chromatography-mass spectrometry based on microwave extraction |
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| CN202011011460.6A CN111929395A (en) | 2020-09-23 | 2020-09-23 | Method for analyzing phthalic acid ester in soil by gas chromatography-mass spectrometry based on microwave extraction |
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|---|---|---|---|---|
| CN103852535A (en) * | 2014-03-26 | 2014-06-11 | 昆山洛丹伦生物科技有限公司 | Detecting method for phthalate acid in plastic component of electronic element |
| CN107655991A (en) * | 2017-09-21 | 2018-02-02 | 国家烟草质量监督检验中心 | The assay method of 6 kinds of phthalic acid esters in soil |
| CN107703236A (en) * | 2017-09-26 | 2018-02-16 | 广东工业大学 | A kind of extraction detection method of Phthalate Esters In Soil |
| CN108387663A (en) * | 2018-05-28 | 2018-08-10 | 东莞市中鼎检测技术有限公司 | A method of detecting phthalic anhydride content in toy with gas chromatography mass spectrometry |
| CN109946405A (en) * | 2019-04-19 | 2019-06-28 | 贵阳市环境监测中心站 | A method of measurement earth's surface underwater trace O-phthalic esters pollutant |
| CN110068626A (en) * | 2019-05-08 | 2019-07-30 | 东莞市信准检测技术服务有限公司 | The measuring method of phthalic acid ester in toy for children |
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2020
- 2020-09-23 CN CN202011011460.6A patent/CN111929395A/en active Pending
Patent Citations (6)
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|---|---|---|---|---|
| CN103852535A (en) * | 2014-03-26 | 2014-06-11 | 昆山洛丹伦生物科技有限公司 | Detecting method for phthalate acid in plastic component of electronic element |
| CN107655991A (en) * | 2017-09-21 | 2018-02-02 | 国家烟草质量监督检验中心 | The assay method of 6 kinds of phthalic acid esters in soil |
| CN107703236A (en) * | 2017-09-26 | 2018-02-16 | 广东工业大学 | A kind of extraction detection method of Phthalate Esters In Soil |
| CN108387663A (en) * | 2018-05-28 | 2018-08-10 | 东莞市中鼎检测技术有限公司 | A method of detecting phthalic anhydride content in toy with gas chromatography mass spectrometry |
| CN109946405A (en) * | 2019-04-19 | 2019-06-28 | 贵阳市环境监测中心站 | A method of measurement earth's surface underwater trace O-phthalic esters pollutant |
| CN110068626A (en) * | 2019-05-08 | 2019-07-30 | 东莞市信准检测技术服务有限公司 | The measuring method of phthalic acid ester in toy for children |
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Application publication date: 20201113 |