CN113466383A - Method for screening organic volatile risk substances in contact material of wine - Google Patents
Method for screening organic volatile risk substances in contact material of wine Download PDFInfo
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- CN113466383A CN113466383A CN202110834351.2A CN202110834351A CN113466383A CN 113466383 A CN113466383 A CN 113466383A CN 202110834351 A CN202110834351 A CN 202110834351A CN 113466383 A CN113466383 A CN 113466383A
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- 230000008685 targeting Effects 0.000 claims 1
- 238000011156 evaluation Methods 0.000 abstract description 3
- 235000020097 white wine Nutrition 0.000 abstract 1
- DOIRQSBPFJWKBE-UHFFFAOYSA-N dibutyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 description 22
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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
- G01N30/62—Detectors specially adapted therefor
- G01N30/72—Mass spectrometers
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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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- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
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Abstract
The application discloses a method for screening organic volatile risk substances in a contact material of wine, which comprises the following steps: soaking the contact material of wine in the migration liquid; adding an extracting solution into the soaked migration solution for extraction, and taking the extracted extracting solution as a sample solution; analyzing the sample liquid by adopting a gas chromatography-mass spectrometry detection method; and screening whether the sample liquid contains organic volatile risk substances according to the analysis result. According to the method, the risk screening can be performed on the organic volatile substances in the contact material of the wine quickly, safely and stably, and the contact material of the wine containing the organic volatile risk substances can be screened by performing gas chromatography-mass spectrometry detection analysis on the migration liquid after the contact material of the wine is soaked, so that the transportation safety of the wine such as white wine is improved, and effective thinking and direction are provided for safety evaluation of food contact materials.
Description
Technical Field
The application relates to the field of food safety detection, in particular to a screening method for organic volatile risk substances in a contact material of wine.
Background
Wine can come into contact with various materials in the production process and the packaged finished products, including transportation pipelines made of high polymer materials or stainless steel, wine bottles, packaging bottle caps, textile fabrics, paper and the like. These contact materials which come into contact with wine are produced by adding specific compounds or metal ions to the material during its production in order to increase its properties, such as plasticity, rigidity, ductility, oxidation resistance, etc.
After these materials are contacted with a solution having good dissolution properties, some of the free materials may slowly migrate into the solution. For example, stainless steel dissolves metal ions, and transportation pipelines and bottle caps made of high molecular polymer materials contain relatively high content of volatile organic compounds.
Wines, such as white spirits, are an alcoholic beverage and are also good solvents. Some organic volatile substances in the conveying pipeline materials, the wine bottles and the bottle caps are easy to migrate into the white spirit after contacting the white spirit, so that the quality of the white spirit is changed. Some volatile organic compounds have adverse effects on human health and have potential food safety hazards. Mainly comprises plastic plasticizer (dibutyl phthalate DBP), benzene series, naphthalene series and other organic hidden trouble substances. These substances have adverse effects on human body such as physiological toxicity, fetal teratogenicity, and neurotoxicity. Food safety accidents in China are frequent, firstly, because of illegal behaviors of bad merchants, and secondly, because China lacks sufficient research and evaluation on safety problems of food contact materials. At present, most of the screening methods for substances in the contact material of the wine are targeted screening methods, only the screening method for metal ions is provided, and the research on the screening method for organic volatile risk substances in the contact material of the wine is lacked.
Disclosure of Invention
The application aims to provide a screening method for organic volatile risk substances in contact materials of wine, which can quickly and safely screen the organic volatile risk substances in the contact materials of the wine.
In order to achieve the above purpose, the technical solution adopted by the present application is as follows:
in some embodiments, the method of the present application comprises the steps of: soaking the contact material of wine in the migration liquid; adding an extracting solution into the soaked migration solution for extraction, and taking the extracted extracting solution as a sample solution; analyzing the sample liquid by adopting a gas chromatography-mass spectrometry detection method; and screening whether the sample liquid contains organic volatile risk substances according to the analysis result.
In some embodiments, the method further comprises: the contact material is weighed and the surface area of the contact material is calculated, the volume of the migrated liquid being adapted to the mass and surface area of the contact material.
In some embodiments, the mass of the contact material is between 2g and 10 g.
In some embodiments, the mass of the contact material is 5 g.
In some embodiments, the surface area of the contact material is 5cm2～25cm2。
In some embodiments, the surface area of the contact material is 15cm2。
In some embodiments, the volume of the migration solution is 100ml to 1000 ml.
In some embodiments, the volume of the migrating liquid is 200ml to 500 ml.
In some embodiments, soaking is followed by resting.
In some embodiments, the temperature of standing is 25 ℃.
In some embodiments, the period of standing is 2 to 15 days.
In some embodiments, the length of standing is 10 days.
In some embodiments, the migrating liquid is an aqueous ethanol solution.
In some embodiments, the ethanol in the aqueous ethanol solution is chromatographic grade ethanol.
In some embodiments, the volume fraction of the aqueous ethanol solution is between 30% and 80%.
In some embodiments, the volume fraction of the aqueous ethanol solution is 45% to 55%.
In some embodiments, the volume fraction of the aqueous ethanol solution is 53%.
In some embodiments, the non-soaked migration fluid is left as a blank control.
In some embodiments, the extraction solution is an organic solvent.
In some embodiments, the extraction liquid is at least one of a n-hexane solvent, a cyclohexane solvent, a benzene solvent, a toluene solvent, an ethyl acetate solvent, a chloroform solvent.
In some embodiments, the extraction solution is a n-hexane solution.
In some embodiments, the volume of organic solvent is 1ml to 20 ml.
In some embodiments, the volume of organic solvent is from 2ml to 10 ml.
In some embodiments, the volume of organic solvent is 2 ml.
In some embodiments, the extraction is followed by shaking.
In some embodiments, the oscillation is performed using a vortex oscillator.
In some embodiments, the power of the oscillation is 300W.
In some embodiments, the duration of the shaking is 10min to 30 min.
In some embodiments, the duration of the shaking is 15min to 20 min.
In some embodiments, the duration of the oscillation is 15 min.
In some embodiments, the sample fluid is analyzed using a gas chromatograph-mass spectrometer.
In some embodiments, the gas chromatography conditions of the gas chromatography mass spectrometer comprise: the carrier gas is He, the flow rate is 1 mL/min-1.5 mL/min, a non-split mode is adopted, the chromatographic column is HP-5MS (30m multiplied by 0.25mm i.d.. times.0.25 mu m), the temperature rising program is that the initial temperature of the chromatographic column is 40-60 ℃, the temperature is kept for 0 min-2 min, the temperature is raised to 200 ℃ at the speed of 5-10 ℃/min, the temperature is not kept, the temperature is raised to 250 ℃ at the speed of 2-5 ℃/min, the temperature is not kept, the temperature is raised to 300 ℃ at the speed of 10 ℃/min-20 ℃/min, and the temperature is kept for 2 min-10 min.
In some embodiments, the gas chromatography conditions of the gas chromatography mass spectrometer comprise: the carrier gas is He, and the flow rate is 1 mL/min; in non-split mode, the column was HP-5MS (30 m.times.0.25 mm i.d.. times.0.25 μm), temperature program: the initial temperature of the chromatographic column is 40-60 ℃, the chromatographic column is kept for 0-2 min, the temperature is raised to 200 ℃ at the speed of 5-10 ℃/min, the chromatographic column is not kept, the temperature is raised to 250 ℃ at the speed of 2-5 ℃/min, the chromatographic column is not kept, the temperature is raised to 300 ℃ at the speed of 10-20 ℃/min, and the chromatographic column is kept for 2-10 min.
In some embodiments, the mass spectrometry conditions of the gas chromatograph-mass spectrometer comprise: EI ionization source, electron energy is 70eV, ion source temperature is 230 ℃, and the full sweep range is 35.00 amu-450.00 amu.
In some embodiments, the mass spectrometry conditions of the gas chromatograph-mass spectrometer comprise: EI ionization source, electron energy is 70eV, ion source temperature is 230 ℃, and the full sweep range is 35.00 amu-450.00 amu.
In some embodiments, screening the sample fluid for organic volatile risk substances based on the analysis result comprises: and comparing the standard ion fragment pattern in the pattern library with the pattern of the sample liquid according to the retention time, and screening whether the sample liquid contains the organic volatile risk substances represented by the standard ion fragment pattern.
In some embodiments, if the sample solution contains the organic volatile risk substance, preparing a standard solution of the organic volatile risk substance, analyzing the standard solution by using a gas chromatography-mass spectrometry method, drawing a standard curve of the standard solution, and determining the concentration of the organic volatile risk substance in the sample solution according to the standard curve.
In some embodiments, the contact material is a material that is contacted during wine production and/or transportation.
In some embodiments, the contact material is a metallic material, a ceramic material, glass, plastic, a woven cloth, or an altar paper.
In some embodiments, the contact material is plastic or a woven cloth.
In some embodiments, the wine is white spirit.
In some embodiments, the white spirit is Maotai-flavor white spirit or a round of Maotai-flavor white spirit.
In some embodiments, the screening is a non-targeted screening, the organic volatile risk substance comprises a known organic volatile risk substance and/or an unknown organic volatile risk substance, and the category of the organic volatile risk substance is one or more.
The screening method of some embodiments of the application can rapidly, safely and stably screen risks of known and/or unknown organic volatile substances in the contact material of the wine, and can screen the contact material of the wine containing organic risk substances by performing gas chromatography-mass spectrometry detection analysis on the migration liquid of the contact material soaked in the wine, so that the transportation safety of the wine is improved, and effective screening thought and direction are provided for safety evaluation of food contact materials.
Drawings
FIG. 1 is a chromatogram of dibutyl phthalate, an organic volatile risk substance, in example 1;
FIG. 2 is a mass spectrum of dibutyl phthalate as an organic volatile risk substance in example 1;
FIG. 3 is a standard curve of dibutyl phthalate, an organic volatile risk substance in example 1.
Detailed Description
The invention is further described below by way of examples, which are not intended to limit the content of the invention further. It should be understood by those skilled in the art that the equivalent substitutions and corresponding modifications made in the present disclosure are within the scope of the present invention.
Main reagents and materials:
ethanol (99.7%) was purchased from Aladdin corporation; methanol (HPLC grade), n-hexane, toluene, cyclohexane, benzene, toluene, chloroform, ethyl acetate (chromatographically pure) were purchased from Tedia, usa.
The main apparatus is as follows:
GC 7890A-MSD 5975C (Agilent, USA) and HP-5MS capillary column 30m × 0.25mm × 0.25 μm (Agilent, USA).
Sample of the contact material of wine: the materials coming from the wine production link and contacting with wine comprise wine transportation pipelines, wine storage tanks, gauze, jar sealing paper and other materials.
The risk screening may be non-targeted screening, the non-targeted screening refers to screening of one or more types of organic volatile risk substances, the organic volatile risk substances can be screened out as long as the materials in contact with the wine contain the organic volatile risk substances, and the screened out volatile risk substances may be known or unknown.
Example 1
Screening of organic volatile risk substances in plastic hoses in contact with wine
1. Migration of organic volatile risk substances in plastic tubes in contact with wine
a. Preparing migration liquid: putting 53ml ethanol into a test tube, weighing 47ml deionized water, adding into the test tube, and shaking up to obtain 53% ethanol water solution;
b. and (3) intercepting a section of plastic tube, weighing, calculating the surface area of the plastic tube, taking a transfer liquid with a certain volume according to the mass and the surface area of the plastic tube, soaking the flexible tube in the transfer liquid, and standing for 10 days.
2. Sample preparation
a. After the migration liquid is soaked, measuring 10ml of migration liquid in a test tube, adding 2ml of n-hexane, placing in a vortex oscillator for constant power oscillation for 15min, and measuring 1ml of an upper organic layer in a sample injection bottle to be detected;
b. after processing a 10ml blank control in the same way as for sample preparation, several layers of 1ml were taken in a sample vial to be tested.
3. And carrying out sample injection analysis on the prepared sample liquid and a blank control sample by using a GC-MS combined instrument. The conditions of the GC-MS combined instrument are as follows:
GC conditions were as follows: the carrier gas is He, and the flow rate is 1 mL/min; in non-split mode, the column was HP-5MS (30 m.times.0.25 mm i.d.. times.0.25 μm), temperature program: the initial temperature of the chromatographic column is 40-60 ℃, the chromatographic column is kept for 0-2 min, the temperature is increased to 120 ℃ at the speed of 5-8 ℃/min, the chromatographic column is not kept, the temperature is increased to 300 ℃ at the speed of 15-20 ℃/min, and the chromatographic column is kept for 5-10 min;
MS conditions: the EI ionization source has electron energy of 70eV and ion source temperature of 230 ℃, and the full-scanning range is 35.00-450.00 amu.
4. Screening risk substances, wherein the screening step comprises qualitative and quantitative analysis;
a. and (3) qualitative analysis: and analyzing fragment ion peaks according to retention time, contrasting a standard ion fragment spectrum in a NIST14a.L spectrum library, and then performing qualitative analysis on the risk substances according to the standard.
b. Quantitative analysis: using n-hexane as a solvent, preparing a series of standard solutions of confirmed risk substances, measuring under the same chromatographic-mass spectrometry condition, and making a standard curve; and integrating chromatographic peaks of the sample risk substances, calculating peak areas, and calculating the concentration of the risk substances in the sample according to a standard curve.
And (3) sample determination: shearing a 5g plastic tube sample, soaking in migration liquid with the volume fraction of 53% ethanol, standing for 10 days, then respectively taking 10ml of migration liquid and a blank control sample into the test tube, adding 2ml of n-hexane, oscillating for 30min, standing, clarifying and layering, then taking 1ml of migration liquid and a blank control sample into a sample bottle, and analyzing by using a GC-MS combined instrument. The gas chromatogram of the sample liquid is shown in figure 1, and the reference library is compared, and the risk substance is dibutyl phthalate after screening, and the mass spectrum thereof is shown in figure 2; a standard curve was then prepared as shown in figure 3. The results of molecular formula, peak area and concentration by qualitative and quantitative analysis are shown in table 1.
TABLE 1
| Name (R) | Qualitative ion | Quantitative ion | Peak area | Concentration of |
| Dibutyl phthalate | 149,223 | 149 | 50485 | 5.36ppm |
The organic volatile risk substance in the plastic tube was measured as dibutyl phthalate (DBP), a concentration of 5.36 ppm.
Example 2
Screening of organic volatile risk substances in liquor contact bottle cap
The package of finished liquor is composed of a ceramic bottle body and a plastic bottle cap, and the plastic bottle cap is used as a material for directly contacting the liquor, so that the safety of the plastic bottle cap is very important.
1. Migration of organic volatile risk substances in wine bottle caps
a. Preparing migration liquid: putting 53ml ethanol into a test tube, weighing 47ml deionized water, adding into the test tube, and shaking up to obtain 53% ethanol water solution;
b. weighing the bottle cap, calculating the surface area of the bottle cap, taking a certain volume according to the weight and the area of the bottle cap to obtain transfer liquid, soaking the bottle cap in the transfer liquid, and standing for 10 days.
2. After the migration liquid is soaked, measuring 10ml of migration liquid in a test tube, adding 2ml of n-hexane, placing in a vortex oscillator for constant power oscillation for 15min, and measuring 1ml of an upper organic layer in a sample injection bottle to be detected.
3. And (4) carrying out sample injection analysis on the prepared sample injection sample by using a GC-MS combined instrument. The conditions of the GC-MS combined instrument are as follows:
GC conditions were as follows: the carrier gas is He, and the flow rate is 1 mL/min; in non-split mode, the column was HP-5MS (30 m.times.0.25 mm i.d.. times.0.25 μm), temperature program: the initial temperature of the chromatographic column is 40-60 ℃, the chromatographic column is kept for 0-2 min, the temperature is increased to 120 ℃ at the speed of 5-8 ℃/min, the chromatographic column is not kept, the temperature is increased to 300 ℃ at the speed of 15-20 ℃/min, and the chromatographic column is kept for 5-10 min;
MS conditions: the EI ionization source has electron energy of 70eV and ion source temperature of 230 ℃, and the full-scanning range is 35.00-450.00 amu.
4. Screening risk substances, wherein the screening step comprises qualitative and quantitative analysis;
a. and (3) qualitative analysis: and analyzing fragment ion peaks according to retention time, contrasting a standard ion fragment spectrum in a NIST14a.L spectrum library, and then performing qualitative analysis on the risk substances according to the standard.
b. Quantitative analysis: using n-hexane as a solvent, preparing a series of standard solutions of confirmed risk substances, measuring under the same chromatographic-mass spectrometry condition, and making a standard curve; and integrating chromatographic peaks of the sample risk substances, calculating peak areas, and calculating the concentration of the risk substances in the sample according to a standard curve.
And (3) sample determination: taking a packaging bottle cap, calculating the surface area, soaking in transfer liquid with the volume fraction of 53% of ethanol, standing for 10 days, taking 10ml of transfer liquid, adding 2ml of n-hexane, oscillating for 30min, standing for clarification and layering, taking 1ml of transfer liquid in a sample injection bottle, and analyzing by using a GC-MS combination instrument. The results show that the undecane contained in the white spirit bottle cap is successfully detected by the method.
Example 3
Screening of organic volatile risk substances in plastic film in liquor brewing process
1. Migration of organic volatile risk substances in plastic film in liquor brewing process
a. Preparing migration liquid: putting 53ml ethanol into a test tube, weighing 47ml deionized water, adding into the test tube, and shaking up to obtain 53% ethanol water solution;
b. shearing part of the plastic film, weighing, calculating the surface area of the plastic film, taking a certain volume according to the mass and the area of the plastic film to obtain transfer liquid, shearing the film, soaking the film in the transfer liquid, and standing for 10 days.
2. After the migration liquid is soaked, measuring 10ml of migration liquid in a test tube, adding 2ml of n-hexane, placing in a vortex oscillator for constant power oscillation for 15min, and measuring 1ml of an upper organic layer in a sample injection bottle to be detected.
3. And (4) carrying out sample injection analysis on the prepared sample injection sample by using a GC-MS combined instrument. The conditions of the GC-MS combined instrument are as follows:
GC conditions were as follows: the carrier gas is He, and the flow rate is 1 mL/min; in non-split mode, the column was HP-5MS (30 m.times.0.25 mm i.d.. times.0.25 μm), temperature program: the initial temperature of the chromatographic column is 40-60 ℃, the chromatographic column is kept for 0-2 min, the temperature is increased to 120 ℃ at the speed of 5-8 ℃/min, the chromatographic column is not kept, the temperature is increased to 300 ℃ at the speed of 15-20 ℃/min, and the chromatographic column is kept for 5-10 min;
MS conditions: the EI ionization source has electron energy of 70eV and ion source temperature of 230 ℃, and the full-scanning range is 35.00-450.00 amu.
4. Screening risk substances, wherein the screening step comprises qualitative and quantitative analysis;
a. and (3) qualitative analysis: and analyzing fragment ion peaks according to retention time, contrasting a standard ion fragment spectrum in a NIST14a.L spectrum library, and then performing qualitative analysis on the risk substances according to the standard.
b. Quantitative analysis: using n-hexane as a solvent, preparing a series of standard solutions of confirmed risk substances, measuring under the same chromatographic-mass spectrometry condition, and making a standard curve; and integrating chromatographic peaks of the sample risk substances, calculating peak areas, and calculating the concentration of the risk substances in the sample according to a standard curve.
And (3) sample determination: shearing a part of plastic film, weighing the mass, calculating the surface area, shearing, soaking in transfer liquid with the volume fraction of 53% ethanol, standing for 10 days, taking 10ml of transfer liquid in a test tube, adding 5ml of n-hexane, oscillating for 30min, standing for clarification and layering, taking 1ml of transfer liquid in a sample injection bottle, and analyzing by using a GC-MS combination instrument. The result shows that the plastic film successfully screened by the invention contains diisobutyl phthalate (DIBP) and dibutyl phthalate (DBP).
Example 4
Screening of organic volatile risk substances in isolation cellar sealing cloth (textile cloth) in liquor brewing process
1. Migration of organic volatile risk substances in isolation cellar sealing cloth in liquor brewing process
a. Preparing migration liquid: putting 53ml ethanol into a test tube, weighing 47ml deionized water, adding into the test tube, and shaking to obtain 53% ethanol water solution.
b. Shearing part of isolation cellar sealing cloth, weighing, calculating the surface area of the plastic film, taking a certain volume according to the mass and the area of the isolation cellar sealing cloth to obtain transfer liquid, soaking the isolation cellar sealing cloth in the transfer liquid, and standing for 10 days.
2. After the migration liquid is soaked, measuring 10ml of migration liquid in a test tube, adding 2ml of n-hexane, placing in a vortex oscillator for constant power oscillation for 15min, and measuring 1ml of an upper organic layer in a sample injection bottle to be detected.
3. And (4) carrying out sample injection analysis on the prepared sample injection sample by using a GC-MS combined instrument. The conditions of the GC-MS combined instrument are as follows:
GC conditions were as follows: the carrier gas is He, and the flow rate is 1 mL/min; in non-split mode, the column was HP-5MS (30 m.times.0.25 mm i.d.. times.0.25 μm), temperature program: the initial temperature of the chromatographic column is 40-60 ℃, the chromatographic column is kept for 0-2 min, the temperature is increased to 120 ℃ at the speed of 5-8 ℃/min, the chromatographic column is not kept, the temperature is increased to 300 ℃ at the speed of 15-20 ℃/min, and the chromatographic column is kept for 5-10 min;
MS conditions: the EI ionization source has electron energy of 70eV and ion source temperature of 230 ℃, and the full-scanning range is 35.00-450.00 amu.
4. Screening risk substances, wherein the screening step comprises qualitative and quantitative analysis;
a. and (3) qualitative analysis: and analyzing fragment ion peaks according to retention time, contrasting a standard ion fragment spectrum in a NIST14a.L spectrum library, and then performing qualitative analysis on the risk substances according to the standard.
b. Quantitative analysis: using n-hexane as a solvent, preparing a series of standard solutions of confirmed risk substances, measuring under the same chromatographic-mass spectrometry condition, and making a standard curve; and integrating chromatographic peaks of the sample risk substances, calculating peak areas, and calculating the concentration of the risk substances in the sample according to a standard curve.
And (3) sample determination: cutting part of isolation cellar sealing cloth, weighing the mass, calculating the surface area, soaking in transfer liquid with the volume fraction of 53% ethanol, standing for 10 days, taking 10ml of transfer liquid into a test tube, adding 5ml of n-hexane, oscillating for 30min, standing for clarification and layering, taking 1ml of transfer liquid into a sample bottle, and analyzing by using a GC-MS combination instrument. The result shows that the isolation cellar sealing cloth successfully screens the n-tetracosan, the n-pentacosan and the n-heptacosane in the isolation cellar sealing cloth.
The above embodiments are only preferred embodiments of the present application, and the protection scope of the present application is not limited thereto, and any insubstantial changes and substitutions made by those skilled in the art based on the present application are intended to be covered by the present application.
Claims (10)
1. A method for screening organic volatile risk substances in a contact material of wine is characterized by comprising the following steps:
soaking the contact material of wine in the migration liquid;
adding an extracting solution into the soaked migration solution for extraction, and taking the extracted extracting solution as a sample solution;
analyzing the sample liquid by adopting a gas chromatography-mass spectrometry detection method;
and screening whether the sample liquid contains organic volatile risk substances according to the analysis result.
2. The method of claim 1, further comprising: weighing the contact material, and calculating the surface area of the contact material, wherein the volume of the migration liquid is adapted to the mass and the surface area of the contact material;
optionally, the mass of the contact material is 2g to 10 g;
preferably, the mass of the contact material is 5 g;
optionally, the contact material has a surface area of 5cm2～25cm2；
Preferably, the surface area of the contact materialIs 15cm2；
Optionally, the volume of the migration liquid is 100ml to 1000 ml;
preferably, the volume of the migration liquid is 200ml to 500 ml.
Optionally, standing is further included after the soaking;
optionally, the temperature of the standing is 25 ℃;
optionally, the standing time is 2-15 days;
preferably, the length of the standing period is 10 days.
3. The method of claim 1, wherein the migration liquid is an aqueous ethanol solution;
optionally, the ethanol in the ethanol aqueous solution is chromatographic grade ethanol;
optionally, the volume fraction of the ethanol aqueous solution is 30-80%;
optionally, the volume fraction of the ethanol aqueous solution is 45-55%;
optionally, the volume fraction of the aqueous ethanol solution is 53%.
4. The method of claim 1, further comprising: the migration solution not soaked as described was left as a blank control.
5. The method of claim 1, wherein the extraction solution is an organic solvent;
optionally, the extracting solution is at least one of a n-hexane solvent, a cyclohexane solvent, a benzene solvent, a toluene solvent, an ethyl acetate solvent and a chloroform solvent;
preferably, the extracting solution is a normal hexane solvent;
optionally, the volume of the organic solvent is 1ml to 20 ml;
optionally, the volume of the organic solvent is 2ml to 10 ml;
preferably, the volume of the organic solvent is 2 ml.
6. The method of claim 1, further comprising shaking after the extracting;
optionally, the oscillating is performed using a vortex oscillator;
optionally, the oscillating power is 300W;
optionally, the oscillation time is 10min to 30 min;
optionally, the oscillation time is 15min to 20 min;
preferably, the duration of the oscillation is 15 min.
7. The method of claim 1, wherein analyzing the sample fluid using gas chromatography-mass spectrometry comprises: analyzing the sample liquid by using a gas chromatography-mass spectrometer;
optionally, the gas chromatography conditions of the gas chromatography-mass spectrometer comprise: the carrier gas is He, the flow rate is 1 mL/min-1.5 mL/min, a non-shunting mode is adopted, the chromatographic column is HP-5MS (30m multiplied by 0.25mm i.d.. times.0.25 mu m), the temperature rising program is that the initial temperature of the chromatographic column is 40-60 ℃, the temperature is kept for 0 min-2 min, the temperature is raised to 200 ℃ at the speed of 5-10 ℃/min, the temperature is not kept, the temperature is raised to 250 ℃ at the speed of 2-5 ℃/min, the temperature is raised to 300 ℃ at the speed of 10 ℃/min-20 ℃/min, and the temperature is kept for 2 min-10 min;
preferably, the gas chromatography conditions of the gas chromatography-mass spectrometer comprise: the carrier gas is He, and the flow rate is 1 mL/min; in non-split mode, the column was HP-5MS (30 m.times.0.25 mm i.d.. times.0.25 μm), temperature program: the initial temperature of the chromatographic column is 40-60 ℃, the chromatographic column is kept for 0-2 min, the temperature is raised to 200 ℃ at the speed of 5-10 ℃/min, the chromatographic column is not kept, the temperature is raised to 250 ℃ at the speed of 2-5 ℃/min, the chromatographic column is not kept, the temperature is raised to 300 ℃ at the speed of 10-20 ℃/min, and the chromatographic column is kept for 2-10 min;
optionally, the mass spectrometry conditions of the gas chromatography-mass spectrometer comprise: EI ionization source, electron energy is 70eV, ion source temperature is 230 ℃, and the full sweep range is 35.00 amu-450.00 amu;
preferably, the mass spectrum conditions of the gas chromatograph-mass spectrometer comprise: mass spectrum conditions: EI ionization source, electron energy is 70eV, ion source temperature is 230 ℃, and the full sweep range is 35.00 amu-450.00 amu.
8. The method as claimed in claim 1, wherein the screening the sample liquid for organic volatile risk substances according to the analysis result comprises:
and comparing a standard ion fragment pattern in a pattern library with the pattern of the sample liquid according to the retention time, and screening whether the sample liquid contains the organic volatile risk substances represented by the standard ion fragment pattern.
9. The method of claim 8, further comprising:
if the sample liquid contains the organic volatile risk substances, preparing a standard solution of the organic volatile risk substances, analyzing the standard solution by adopting a gas chromatography-mass spectrometry detection method, drawing a standard curve of the standard solution, and determining the concentration of the organic volatile risk substances in the sample liquid according to the standard curve.
10. The method according to any one of claims 1 to 9, wherein the contact material is a material that is contacted during wine production and/or transportation;
optionally, the contact material is a metal material, a ceramic material, glass, plastic, a textile fabric or jar sealing paper;
preferably, the contact material is a plastic or textile cloth;
optionally, the wine is white spirit;
preferably, the liquor is Maotai-flavor liquor or a round of Maotai-flavor liquor;
optionally, the screening is a non-targeting screening, the organic volatile risk substances comprise known organic volatile risk substances and/or unknown organic volatile risk substances, and the types of the organic volatile risk substances are one or more.
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Application publication date: 20211001 |