CN111965264A - Solid phase micro-extraction analysis method - Google Patents
Solid phase micro-extraction analysis method Download PDFInfo
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- CN111965264A CN111965264A CN201910417820.3A CN201910417820A CN111965264A CN 111965264 A CN111965264 A CN 111965264A CN 201910417820 A CN201910417820 A CN 201910417820A CN 111965264 A CN111965264 A CN 111965264A
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- 238000002470 solid-phase micro-extraction Methods 0.000 title claims abstract description 55
- 238000004458 analytical method Methods 0.000 title claims abstract description 28
- 238000010438 heat treatment Methods 0.000 claims abstract description 22
- 239000000126 substance Substances 0.000 claims abstract description 17
- 238000004587 chromatography analysis Methods 0.000 claims abstract description 11
- 238000001816 cooling Methods 0.000 claims abstract description 9
- 239000012071 phase Substances 0.000 claims abstract description 8
- 238000005516 engineering process Methods 0.000 claims abstract description 3
- 238000000605 extraction Methods 0.000 claims description 23
- 239000000796 flavoring agent Substances 0.000 claims description 7
- 235000019634 flavors Nutrition 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 7
- 238000005070 sampling Methods 0.000 claims description 7
- 235000002637 Nicotiana tabacum Nutrition 0.000 claims description 6
- 238000003795 desorption Methods 0.000 claims description 6
- 244000269722 Thea sinensis Species 0.000 claims description 4
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 claims description 3
- 235000013305 food Nutrition 0.000 claims description 2
- 238000004817 gas chromatography Methods 0.000 claims description 2
- 244000061176 Nicotiana tabacum Species 0.000 claims 1
- 238000003556 assay Methods 0.000 claims 1
- 238000004811 liquid chromatography Methods 0.000 claims 1
- 238000004895 liquid chromatography mass spectrometry Methods 0.000 claims 1
- 238000002347 injection Methods 0.000 abstract description 20
- 239000007924 injection Substances 0.000 abstract description 20
- 238000009835 boiling Methods 0.000 abstract description 8
- 238000005336 cracking Methods 0.000 abstract description 4
- 238000004821 distillation Methods 0.000 abstract description 4
- 238000012544 monitoring process Methods 0.000 abstract description 3
- 239000000284 extract Substances 0.000 abstract description 2
- 239000000523 sample Substances 0.000 description 49
- 239000007789 gas Substances 0.000 description 16
- 238000011534 incubation Methods 0.000 description 7
- 238000001319 headspace solid-phase micro-extraction Methods 0.000 description 6
- 241000208125 Nicotiana Species 0.000 description 5
- 239000013068 control sample Substances 0.000 description 5
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- IANQTJSKSUMEQM-UHFFFAOYSA-N 1-benzofuran Chemical compound C1=CC=C2OC=CC2=C1 IANQTJSKSUMEQM-UHFFFAOYSA-N 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 244000068988 Glycine max Species 0.000 description 2
- 235000010469 Glycine max Nutrition 0.000 description 2
- 235000019764 Soybean Meal Nutrition 0.000 description 2
- 239000004205 dimethyl polysiloxane Substances 0.000 description 2
- 235000013870 dimethyl polysiloxane Nutrition 0.000 description 2
- 239000004519 grease Substances 0.000 description 2
- 238000004949 mass spectrometry Methods 0.000 description 2
- 238000001819 mass spectrum Methods 0.000 description 2
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000005086 pumping Methods 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 239000004455 soybean meal Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 239000012491 analyte Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 210000004907 gland Anatomy 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 239000005457 ice water Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002808 molecular sieve Substances 0.000 description 1
- CXQXSVUQTKDNFP-UHFFFAOYSA-N octamethyltrisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)O[Si](C)(C)C CXQXSVUQTKDNFP-UHFFFAOYSA-N 0.000 description 1
- 238000004987 plasma desorption mass spectroscopy Methods 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 230000003068 static effect Effects 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
-
- 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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N30/12—Preparation by evaporation
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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
- G01N2030/062—Preparation extracting sample from raw material
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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
- G01N30/12—Preparation by evaporation
- G01N2030/126—Preparation by evaporation evaporating sample
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- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
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- General Health & Medical Sciences (AREA)
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Abstract
The invention relates to a solid phase micro-extraction analysis method, which comprises the steps of heating a closed container which is filled with a substance to be analyzed and is in a negative pressure state in the interior for 1-15min in an environment of 120-300 ℃, taking out the closed container, and cooling the closed container to 60-120 ℃; extracting gas phase components in the closed container by adopting a solid phase microextraction technology to obtain an analysis sample; the obtained analysis sample was subjected to chromatography, and data was collected. The invention carries out high-temperature heat treatment on the sample under the negative pressure state, extracts the aroma components in the distillation cracking zone in the sample, locks the aroma components in the vacuum headspace sample injection bottle, and then carries out conventional solid phase microextraction, can break through the temperature limit of the solid phase microextraction, realizes the sample with high boiling point at the lower temperature of the solid phase microextraction, has simple and easy operation, is easy to realize on-line monitoring, and can open up a new path for the solid phase microextraction.
Description
Technical Field
The invention relates to a solid phase microextraction analysis method, in particular to a headspace solid phase microextraction analysis method comprising negative pressure high-temperature heat treatment, and relates to an analysis method of volatile components and/or semi-volatile components in a sample.
Background
The solid phase micro-extraction is a novel sample processing mode, the sample is put into a headspace sample injection bottle with a certain volume for heating, so that volatile components are volatilized from the sample, and then a solid phase micro-extraction head is inserted for sampling, extracting, concentrating and injecting the sample into a whole, so that the operation is convenient; has the advantages of high efficiency, simplicity, no damage and the like.
The main factors influencing the solid phase microextraction are: extraction temperature, extraction time, inorganic salts, pH, etc. For the volatilization efficiency of the sample, the higher the extraction incubation temperature is, the more beneficial the volatilization of the volatile components in the sample is, the shorter the extraction time is, and the higher the extraction efficiency is. However, the higher extraction temperature may also cause instability of the analyte, and the desorption temperature of the solid phase micro-extraction head is generally between 120 ℃ and 280 ℃. The increase of the extraction temperature reduces the adsorption speed of the solid phase micro-extraction head and increases the desorption speed, so that the increase of the extraction temperature can cause the simultaneous adsorption and desorption of the solid phase micro-extraction, and the extraction efficiency cannot be increased. Therefore, the solid phase microextraction temperature is generally recommended to be below 100 ℃, but for the analysis of the flavor components of the flavor samples, a higher incubation extraction temperature is often required, and when the incubation temperature is raised to a certain degree, volatile and semi-volatile substances in the headspace bottle are increased, the equilibrium vapor pressure in the headspace bottle is further increased, and particularly when the temperature in the headspace bottle is raised to be above 120 ℃, a cushion on the headspace bottle cap can burst, even if the cushion does not burst, and volatile gas is easy to overflow during the solid phase microextraction, so that the extraction efficiency is reduced.
In order to increase the desorption temperature of the solid phase micro-extraction head, a great deal of research at home and abroad focuses on the reduction of the headspace temperature of the extraction head part, namely, the increase or maintenance of the extraction and incubation temperatures of a sample, but the reduction of the temperature of the headspace part or the extraction head part. For example, Petersen et al (Petersen M B, Poll L. EurFood Res Technol, 1999, 209:251) can cool the coating while heating the sample by adding a liquid carbon dioxide cooling device to the solid phase microextraction handle. So that the temperature of the coating is lower than the temperature of the sample. The method of internal cooling of the extraction fiber can effectively improve the sensitivity and extraction rate of the PME.
Chinese patent No. CN 207351791U discloses a solid phase micro-extraction auxiliary device. The outer side of the auxiliary equipment body is provided with a vacuum layer, and the bottom of the auxiliary equipment body is provided with an annular groove; the auxiliary device has two connected cylindrical cavities throughout the auxiliary device. When the headspace solid-phase microextraction is carried out, a sample bottle is placed in a cup containing water, the heat-preservation auxiliary equipment is covered on the cup, the groove is aligned, and then the solid-phase microextraction is carried out.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a solid phase microextraction analysis method, which utilizes solid phase microextraction to analyze the aroma components in a distillation cracking zone of a flavor sample, breaks through the limitation that the solid phase microextraction cannot realize the extraction of aroma components with high boiling point, and is an analysis method for improving the application range and the analysis efficiency of the solid phase microextraction.
In order to solve the technical problems, the technical scheme of the invention is as follows:
an analysis method comprising the steps of:
s1, placing the closed container which is filled with the substance to be analyzed and has the interior in a negative pressure state in an environment of 120-300 ℃ for heating for 1-15min, taking out, and cooling to 60-120 ℃;
s2, extracting gas phase components in the closed container by adopting a solid phase microextraction technology to obtain an analysis sample;
s3, carrying out chromatographic analysis on the analysis sample obtained in the S2, and collecting data.
Alternatively, the material to be analyzed is loaded into the closed container and then evacuated by means of a syringe or a vacuum pump.
Further, in S1, the closed container is a headspace sampling bottle. Alternatively, the headspace sampling vials are commercially available.
The headspace sampling bottle is a pressure-resistant cap-rotating type or gland type headspace sampling bottle, preferably a cap-rotating type headspace sampling bottle with the specification of 20 ml.
The pressure in the closed container can be confirmed and adjusted according to the weight and content of the component to be analyzed.
Further, in S1, the pressure in the closed vessel before heating is 50 to 99kPa, preferably 80 to 99 kPa.
Further, in S1, after cooling to 60-120 ℃, the pressure in the closed container is less than 1 standard atmosphere.
Further, the cooling process in S1 is performed in a headspace heating furnace, optionally, for 1-10 min.
S1, heating the sample by a heating furnace such as a headspace heating furnace or other heating devices such as a gas chromatograph-mass spectrometer sample inlet and a gas chromatograph furnace.
On one hand, the cooling process can realize temperature reduction; on the other hand, the device can play a balancing role so that gas phase substances in the closed container are uniformly distributed.
Further, in S2, the solid phase microextraction head was inserted into a closed container and extracted.
Further, in S2, the extraction temperature is 60-120 ℃, preferably 80-100 ℃; the extraction time is 20-120min, preferably 20-60 min.
Further, in S3, the extracted solid phase micro extraction head is inserted into the injection port of the chromatographic analysis instrument, and the thermal desorption is carried out for 2-5min at 200-300 ℃, and the chromatographic analysis instrument is operated and data is collected.
Further, the substance to be analyzed is a flavor substance, preferably, the flavor substance comprises at least one of cut tobacco, tea leaves and food.
Further, the chromatographic analysis comprises at least one of gas chromatographic analysis, gas chromatographic-mass spectrometric analysis, liquid chromatographic analysis and liquid chromatographic-mass spectrometric analysis.
Further, the solid phase micro-extraction is headspace solid phase micro-extraction.
Further, the solid phase micro-extraction comprises on-line solid phase micro-extraction and off-line solid phase micro-extraction.
Further, the solid phase micro-extraction includes on-line analysis and off-line manual analysis.
The invention carries out high-temperature heat treatment on the substance to be analyzed in a negative pressure state, then carries out conventional solid phase micro-extraction, can realize low-temperature extraction on the sample with high boiling point at a lower extraction temperature, is simple and easy to operate, and is easy to realize on-line monitoring.
Because the inside of the closed container is in a negative pressure state, high boiling point components can be converted into gas phase substances only by lower heating temperature, so that volatile and semi-volatile components in the substances to be analyzed can be converted into the gas phase substances more easily, and the requirements on the closed container can be reduced; in addition, the air pressure in the container is less than the atmospheric pressure, so that the volatile gas phase substances do not need to be worried about overflowing to influence the analysis result, and the gas phase components in the distillation cracking zone in the substance to be analyzed are locked in the closed container. Such as coumarone in dried soybean powder, boiling point 173-175 deg.C, this component was not detected in conventional solid phase microextraction, but was detected when the dried soybean powder sample bottle was subjected to vacuum and high temperature treatment.
The invention carries out high-temperature heat treatment on the sample under the negative pressure state, extracts the aroma components in the distillation cracking zone in the sample, locks the aroma components in a closed container such as a headspace sample injection bottle and the like, and then carries out conventional solid phase microextraction, can break through the temperature limit of the solid phase microextraction, realizes the sample with high boiling point at lower solid phase microextraction temperature, has simple and easy operation, is easy to realize on-line monitoring, and can open up a new path for the solid phase microextraction.
Drawings
FIG. 1 is an analytical map of the experimental group (upper curve) and the control group (lower curve) in example 2.
FIG. 2 is an analytical map of the experimental group (upper curve) and the control group (lower curve) in example 3.
FIG. 3 is an analytical map of the experimental group (upper curve) and the control group (lower curve) in example 4.
Detailed Description
The invention is further described with reference to specific examples. The following examples are intended to illustrate the invention without further limiting it.
The instrument comprises the following steps: an Aglient 7890N gas chromatograph and an Agilent 5975 type mass spectrum detector; GERSTEL three-in-one (solid phase micro-extraction, static headspace, solution injection) autosampler (GERSTEL, germany); circulating water type vacuum pump (SHZ-DIII), solid phase micro extraction head: 75 μm carbon molecular sieve/polydimethylsiloxane (CAR/PDMS) (SULPLCO, USA), 20mL headspace sample bottles with self-sealing gaskets, condensing units (ice-water mixture);
GC/MS (gas chromatography-mass spectrometry) analysis conditions: gas chromatography parameters: a chromatographic column: HP-5MS capillary column (60.0 m × 250 μm × 0.25 μm), injection inlet temperature of 250 deg.C, carrier gas of high purity helium gas, flow rate of 1.0mL/min, and split ratio of 15: 1; temperature programming: the initial temperature is 80 ℃ and kept for 2min, the temperature is increased to 250 ℃ at the rate of 6 ℃/min and kept for 1min, and then the temperature is increased to 285 ℃ at the rate of 10 ℃/min and kept for 3 min;
mass spectrum parameters: an ionization mode: an electron impact source (EI); ionization energy 70 eV; the ion source temperature is 230 ℃; the temperature of a four-level bar is 150 ℃; the scanning mode is full scanning; the scan range is 35-450 amu.
Example 1
Respectively taking 0.2g of tobacco shreds and putting the tobacco shreds into two 20ml headspace sample bottles, and pumping one headspace sample bottle for several times by using a 25ml syringe with an injection needle until a pumping piston is difficult to pull. Smearing a headspace bottle cushion with vacuum grease to serve as an experimental group; the control sample is not processed, the headspace sample bottle is put into a heating furnace to be heated to 250 ℃ for 3min, the bottle cap of the experimental group is intact, and the soft cap of the headspace sample injection bottle cap of the control sample is burst and bounces out.
Example 2
Respectively putting 0.2g of tobacco shreds into two 20ml headspace sample bottles, connecting one headspace sample bottle to a circulating vacuum pump by using an injector with an injection needle to extract air for several minutes, putting a sample into a heating furnace to heat to 250 ℃ after a vacuum pump pressure gauge is stabilized at 0.1mp, keeping the temperature for 3min, and taking out the headspace sample bottles as an experimental group; the control sample is not treated, and then the headspace sample injection bottle is taken out and put in an incubation furnace at 80 ℃, the balance time is 5min, and the headspace solid phase microextraction time is 50 min. And taking out the solid phase micro-extraction needle, and then carrying out analytic sample injection at a sample injection port of the gas chromatography-mass spectrometer. Compared with a control group, the information of volatile components of the cut tobacco subjected to negative pressure high temperature treatment is obviously rich, and particularly the types and the contents of components with high boiling points are obviously increased (referring to fig. 1, generally, the higher the boiling point of the component, the later the peak time, the judgment can be made accordingly).
Example 3
Respectively putting 0.5g of dry soybean meal into two 20ml headspace sample bottles, connecting one of the headspace sample bottles to a circulating vacuum pump by using an injector with an injection needle to pump air for several minutes, putting a sample into a heating furnace to heat to 250 ℃ after a vacuum pump pressure gauge is stabilized at 0.1mp, keeping the temperature for 3min, and taking out the headspace sample bottles to serve as an experimental group; the control sample is not treated, and then the headspace sample injection bottle is taken out and put in an incubation furnace at 90 ℃, the balance is carried out for 5min, and the headspace solid phase micro-extraction time is 30 min. And taking out the solid phase micro-extraction needle, and then carrying out analytic sample injection at a sample injection port of the gas chromatography-mass spectrometer. Compared with a control group, the relative corresponding abundance of the volatile components of the soybean meal subjected to negative pressure high temperature treatment is obviously enhanced, and the component information is obviously rich.
Example 4
Respectively putting 0.5g of dry tea leaves into two 20ml headspace sample bottles, connecting one of the headspace sample bottles to a circulating vacuum pump by using an injector with an injection needle to extract air for several minutes, coating a headspace bottle cushion by using vacuum grease after a vacuum pump pressure gauge is stabilized at 0.1mp, putting a sample into a heating furnace to be heated to 200 ℃, keeping for 2 minutes, then heating to 250 ℃ and keeping for 2 minutes, and taking out the headspace sample bottles to serve as experimental groups; the control sample is not treated, and then the headspace sample injection bottle is taken out and put in an incubation furnace at 90 ℃, the balance time is 10min, and the headspace solid phase micro-extraction time is 40 min. And taking out the solid phase micro-extraction needle, and then carrying out analytic sample injection at a sample injection port of the gas chromatography-mass spectrometer. Compared with a control group, the response information of the volatile components of the tea subjected to negative pressure high temperature treatment is obviously rich, and the component types and the content are obviously increased.
The foregoing examples are set forth to illustrate the present invention more clearly and are not to be construed as limiting the scope of the invention, which is defined in the appended claims to which the invention pertains, as modified in all equivalent forms, by those skilled in the art after reading the present invention.
Claims (9)
1. A solid phase micro-extraction analysis method is characterized by comprising the following steps:
s1, placing the closed container which is filled with the substance to be analyzed and has the interior in a negative pressure state in an environment of 120-300 ℃ for heating for 1-15min, taking out, and cooling to 60-120 ℃;
s2, extracting gas phase components in the closed container by adopting a solid phase microextraction technology to obtain an analysis sample;
s3, carrying out chromatographic analysis on the analysis sample obtained in the S2, and collecting data.
2. The method for solid-phase microextraction analysis according to claim 1, wherein in S1, said closed vessel is a headspace sampling bottle.
3. The method for solid-phase microextraction analysis according to claim 1, wherein in S1, the pressure in the closed vessel before heating is 50 to 99 kPa.
4. The method for solid-phase microextraction analysis according to claim 1, wherein in S1, after cooling to 60-120 ℃, the pressure in the closed container is less than 1 standard atmosphere.
5. The method of claim 1, wherein the solid phase microextraction is performed by inserting the solid phase microextraction head into a closed container in S2.
6. The solid phase microextraction analysis method according to claim 1, wherein in S2, the extraction temperature is 60-120 ℃, preferably 80-100 ℃; the extraction time is 20-120min, preferably 20-60 min.
7. The analysis method as claimed in claim 5, wherein in S3, the extracted solid phase micro extraction head is inserted into the sample inlet of the chromatographic analysis instrument, and the chromatographic analysis instrument is operated and data is collected by thermal desorption at 200-300 ℃ for 2-5 min.
8. The solid phase microextraction analysis method according to any one of claims 1-7, wherein said substance to be analyzed is a flavor substance, preferably said flavor substance comprises at least one of cut tobacco, tea leaves, food.
9. The solid phase microextraction assay of any one of claims 1-7, wherein said chromatographic analysis comprises at least one of gas chromatography, gas chromatography-mass spectrometry, liquid chromatography, and liquid chromatography-mass spectrometry.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114894932A (en) * | 2022-05-07 | 2022-08-12 | 安徽工程大学 | Method for detecting trace amount peculiar smell gas components in automobile textile fabric |
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|---|---|---|---|---|
| CN207440025U (en) * | 2017-11-28 | 2018-06-01 | 谢家理 | The negative pressure extraction piece-rate system of organic pollution in sample |
| CN108593816A (en) * | 2018-04-28 | 2018-09-28 | 江苏中烟工业有限责任公司 | A kind of method and device improving volatile ingredient purging efficiency in tobacco |
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| CN207440025U (en) * | 2017-11-28 | 2018-06-01 | 谢家理 | The negative pressure extraction piece-rate system of organic pollution in sample |
| CN108593816A (en) * | 2018-04-28 | 2018-09-28 | 江苏中烟工业有限责任公司 | A kind of method and device improving volatile ingredient purging efficiency in tobacco |
Non-Patent Citations (3)
| Title |
|---|
| CHANGGOOK LEE 等: "Development of a reduced pressure headspace solid-phase microextraction-gas chromatography/mass spectrometric (rpHSSPME-GC/MS) method and application to aroma analysis", 《ANALYTICAL METHODS》 * |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114894932A (en) * | 2022-05-07 | 2022-08-12 | 安徽工程大学 | Method for detecting trace amount peculiar smell gas components in automobile textile fabric |
| CN114894932B (en) * | 2022-05-07 | 2023-08-01 | 安徽工程大学 | Method for detecting trace odor components in textile fabric for automobile |
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