CN109490428A - The rapid detection method of methanol content in a kind of wine - Google Patents
The rapid detection method of methanol content in a kind of wine Download PDFInfo
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- CN109490428A CN109490428A CN201811172734.2A CN201811172734A CN109490428A CN 109490428 A CN109490428 A CN 109490428A CN 201811172734 A CN201811172734 A CN 201811172734A CN 109490428 A CN109490428 A CN 109490428A
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- methanol
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- wine
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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
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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
Abstract
The invention discloses a kind of rapid detection methods of methanol content in wine, the detection method of the methanol content of offer can directly, quickly detect the content of methanol in wine compared with national standard, it is easy to operate, accuracy is high, stability is good, the rate of recovery is good, for analyzing batch sample, it can be improved working efficiency, economize on resources, while when enterprise's high-volume is produced, the purpose monitored rapidly can be played to product quality, it being capable of timely Instructing manufacture；Methanol and other interference components can also be efficiently separated, have the advantages that preparation, high sensitivity and reproducible, and the present invention other than providing to the detection method of methanol content in white wine, additionally provide detection method to methanol content in alcohol, assembled alcoholic drinks and fermented wine, applicability is wide, method is simple, is worthy to be popularized.
Description
Technical field
The present invention relates to a kind of quick detection sides of methanol content in food processing field technical field more particularly to wine
Method.
Background technique
Methanol is that white wine generates during the fermentation, is decomposed for methyl ester in pectic substance in raw material and auxiliary material.First
Alcohol itself toxicity with higher, it puts aside in human body, slow poisoning, headache can also be caused to dislike even if a small amount of methanol
The heart, eye-blurred, 5~10 mL can cause to blind, serious to nervous system especially optic nerve lesion.Methanol content is wine
One of the important indicator of class product health supervision detection, the content of strict control methanol in wine ensures food safety, and protection disappears
The safety of the person of expense, prevent the fake wine blent with non-edible alcohol, in blue ruin the exceeded poisoning of methanol generation.
Currently, the detection method of methanol content uses GB5009.266-2016 " national food safety standard in detection drinks
The measurement of methanol in food " national standard method, but national standard method detect a sample time-consuming, and in drinks other flavors at
Divide to be separated well, be not suitable for the analysis detection of batch sample, cannot be timely when enterprise's high-volume is produced
Rapidly product quality is monitored.Therefore it provides in a kind of wine methanol content rapid detection method, to can batch
, quick and accurate detection the advantages of going out methanol content, being consumed when reaching batch detection, shortening, this is food-processing industry
The hot issue of research.
Summary of the invention
It is an object of that present invention to provide a kind of directly fast and accurately gas-chromatography detection method of methanol content in drinks,
Using butyl acetate as internal standard, using HP-INNOPWAX column, while also can other different flavors in quick separating drinks at
Point, finally obtain one kind simply, fast, while the new detection method of accuracy with higher and preferable separating effect,
It is exactly in order to make up the defect of prior art.
The present invention is achieved by the following technical solutions:
The rapid detection method of methanol content in a kind of wine, comprising the following specific steps
(1) ethanol solution that dose volume score is 60%: precision measures ethanol solution 600mL, is settled to 1000mL with water, mixes
It is even；
(2) the butyl acetate solution that dose volume score is 2%: precision draws butyl acetate 2mL, the ethyl alcohol prepared with step (1)
Solution is settled to 100mL, mixes；
(3) preparation of methanol standard solution: weighing methanol 0.10004g in 100mL volumetric flask, with the second prepared in step (1)
Alcoholic solution constant volume, mix, as mother liquor, then take the volumetric flask of 5 50mL, respectively draw 0.5mL, 1mL, 2.5mL, 5mL,
The above-mentioned mother liquor of 7.5mL is settled to scale with the ethanol solution that step (1) is prepared, mixes；
(4) production of methanol standard curve: the methanol standard solution of 5 prepared in step (3) not isoconcentrations is drawn respectively
Then the butyl acetate solution of 0.2mL step (2) preparation is added as internal standard, with the second of step (1) preparation in test tube in 10mL
Alcoholic solution is diluted to a certain concentration, mixes, and carries out chromatography；
(5) in 11 including methanol the mixed mark solution of flavor substance preparation: by flavor substance ethyl hexanoate, ethyl acetate,
Ethyl butyrate, acetic acid, caproic acid, normal propyl alcohol, n-butanol, isoamyl alcohol, acetic acid aldehyde, acetaldehyde and methanol are arrived according to conventional additive amount respectively
In the volumetric flask of 100mL, it is settled to scale with the ethanol solution that step (1) is prepared, mixes and is used as stock solution, draws deposit respectively
Liquid 10mL adds the butyl acetate solution of 0.2mL step (2) preparation as internal standard, and the ethanol solution prepared with step (1) is dilute
It releases to a certain concentration, mixes, carry out chromatography and draw standard curve；
(6) preparation of sample solution: sample solution is drawn into 10mL in test tube, the acetic acid fourth that 0.2mL step (2) are prepared is added
Ester solution dilutes butyl acetate to a certain concentration as internal standard, with the ethanol solution that step (1) is prepared, and mixes；
(7) gas chromatography analysis: analytical conditions for gas chromatography are as follows: HP-INNOPWAX column length 30m, column internal diameter 0.25mm,
0.25 μm of thickness of liquid film, temperature program:, keeping 7min, be warming up to 55 DEG C with 5 DEG C, be warming up to 210 DEG C with 30 DEG C by 40 DEG C of column temperature,
Keep 2min, injector temperature: 200 DEG C, detector temperature: 250 DEG C, gasify room temperature: 240 DEG C, carrier gas: nitrogen flow
0.7mL/min, hydrogen flowing quantity 35mL/min, air mass flow 350mL/min, split ratio 50:1,0.5 μ L of sample volume；
(8) drafting of standard curve and result calculate: starting gas chromatograph, according to the program setting instrument item in step (7)
Part carries out sample introduction operation after waiting instrument stabilizers respectively, the peak area of methanol and other flavor components and butyl acetate is measured, with first
The ratio between alcohol and butyl acetate concentration are abscissa, using the ratio of methanol and butyl acetate chromatographic peak area as ordinate, draw mark
Directrix curve is contrasted with the retention time of methanol and standard specimen and carries out qualitative, utilizes an alignment existing for peak area and methanol content
With inner mark method ration, according to testing result with the standard curve of foundation, methanol content in wine is calculated in sexual intercourse.
The rapid detection method of methanol content in a kind of wine, the concentration of methanol series standard solution in the step (3)
Respectively 10.004mg/L, 20.008mg/L, 50.02mg/L, 100.04mg/L, 150.06mg/L.
The rapid detection method of methanol content in a kind of wine, butyl acetate solution is dilute in the step (4), (5) and (6)
Concentration after releasing is 352mg/L.
The rapid detection method of methanol content in a kind of wine, sample described in step (6) are white wine, alcohol, assembled alcoholic drinks
And fermented wine is any.
The rapid detection method of methanol content, the detection method of the methanol in wine content are in a kind of wine, accurate
10mL Wine Sample is drawn in test tube, 0.2mL2% butyl acetate solution is added as internal standard, the concentration of internal standard solution is 352mg/
L, after instrument stabilizer, 0.5 μ L of sample introduction injects gas chromatograph, and the ratio of the peak area of methanol and butyl acetate is obtained after integral
Value, obtains the content of methanol in wine according to standard curve.
The rapid detection method of methanol content in a kind of wine, the detection method of methanol content is to draw in the alcohol
0.2mL2% butyl acetate solution is added as internal standard in test tube in 10mL alcohol sample, and the concentration of internal standard solution is 352mg/L, to
After instrument stabilizer, 0.5 μ L of sample introduction injects gas chromatograph, and the ratio of the peak area of methanol and butyl acetate, root are obtained after integral
The content of methanol in alcohol is obtained according to standard curve.
The detection method of the rapid detection method of methanol content in a kind of wine, the assembled alcoholic drinks and fermented wine is to prepare
Wine and each 100mL of fermented wine first distill, and the sample 10mL after taking distillation is added 0.2mL2% butyl acetate solution and makees in test tube
Concentration for internal standard, internal standard solution is 352mg/L, and after instrument stabilizer, 0.5 μ L of sample introduction injects gas chromatograph, is obtained after integral
The ratio of the peak area of methanol and butyl acetate obtains the content of methanol in assembled alcoholic drinks and fermented wine according to standard curve.
The invention has the advantages that the detection method of methanol content provided by the invention directly, can be examined quickly compared with national standard
The content of methanol in wine is surveyed, it is easy to operate, accuracy is high, stability is good, the rate of recovery is good, for analyzing batch sample, Neng Gouti
High working efficiency, economizes on resources, while when enterprise's high-volume is produced, the mesh monitored rapidly can be played to product quality
, it being capable of timely Instructing manufacture；Methanol and other interference components can also be efficiently separated, there is preparation, high sensitivity and repetition
Property good advantage, and the present invention other than providing to the detection method of methanol content in white wine, additionally provide to alcohol, prepare
The detection method of methanol content in wine and fermented wine, applicability is wide, and method is simple, is worthy to be popularized.
Detailed description of the invention
Fig. 1 is the canonical plotting of the application methanol content.
Specific embodiment
The rapid detection method of methanol content in a kind of wine, comprising the following specific steps
(1) ethanol solution that dose volume score is 60%: precision measures ethanol solution 600mL, is settled to 1000mL with water, mixes
It is even；
(2) the butyl acetate solution that dose volume score is 2%: precision draws butyl acetate 2mL, the ethyl alcohol prepared with step (1)
Solution is settled to 100mL, mixes；
(3) preparation of methanol standard solution: weighing methanol 0.10004g in 100mL volumetric flask, with the second prepared in step (1)
Alcoholic solution constant volume, mix, as mother liquor, then take the volumetric flask of 5 50mL, respectively draw 0.5mL, 1mL, 2.5mL, 5mL,
The above-mentioned mother liquor of 7.5mL is settled to scale with the ethanol solution that step (1) is prepared, mixes, the concentration point of methanol series standard solution
It Wei not 10.004mg/L, 20.008mg/L, 50.02mg/L, 100.04mg/L, 150.06mg/L；
(4) production of methanol standard curve: the methanol standard solution of 5 prepared in step (3) not isoconcentrations is drawn respectively
Then the butyl acetate solution of 0.2mL step (2) preparation is added as internal standard, with the second of step (1) preparation in test tube in 10mL
The concentration that alcoholic solution dilutes butyl acetate solution is 352mg/L, mixes, carries out chromatography；
(5) in 11 including methanol the mixed mark solution of flavor substance preparation: by flavor substance ethyl hexanoate, ethyl acetate,
Ethyl butyrate, acetic acid, caproic acid, normal propyl alcohol, n-butanol, isoamyl alcohol, acetic acid aldehyde, acetaldehyde and methanol are arrived according to conventional additive amount respectively
In the volumetric flask of 100mL, it is settled to scale with the ethanol solution that step (1) is prepared, mixes and is used as stock solution, draws deposit respectively
Liquid 10mL adds the butyl acetate solution of 0.2mL step (2) preparation as internal standard, and the ethanol solution prepared with step (1) is dilute
The concentration for releasing butyl acetate solution is 352mg/L, is mixed, and carries out chromatography and draws standard curve；
(6) preparation of sample solution: sample solution is drawn into 10mL in test tube, the acetic acid fourth that 0.2mL step (2) are prepared is added
For ester solution as internal standard, the concentration for the ethanol solution dilution butyl acetate butyl acetate solution prepared with step (1) is 352mg/
L is mixed；
(7) gas chromatography analysis: analytical conditions for gas chromatography are as follows: HPINNOPWAX column length 30m, column internal diameter 0.25mm,
0.25 μm of thickness of liquid film, temperature program:, keeping 7min, be warming up to 55 DEG C with 5 DEG C, be warming up to 210 DEG C with 30 DEG C by 40 DEG C of column temperature,
Keep 2min, injector temperature: 200 DEG C, detector temperature: 250 DEG C, gasify room temperature: 240 DEG C, carrier gas: nitrogen flow
0.7mL/min, hydrogen flowing quantity 35mL/min, air mass flow 350mL/min, split ratio 50:1,0.5 μ L of sample volume；
(8) drafting of standard curve and result calculate: starting gas chromatograph, according to the program setting instrument item in step (7)
Part carries out sample introduction operation after waiting instrument stabilizers respectively, the peak area of methanol and other flavor components and butyl acetate is measured, with first
The ratio between alcohol and butyl acetate concentration are abscissa, using the ratio of methanol and butyl acetate chromatographic peak area as ordinate, draw mark
Directrix curve is contrasted with the retention time of methanol and standard specimen and carries out qualitative, utilizes an alignment existing for peak area and methanol content
With inner mark method ration, according to testing result with the standard curve of foundation, methanol content in wine is calculated in sexual intercourse.
The rapid detection method of methanol content in a kind of wine, sample described in step (6) are white wine, alcohol, assembled alcoholic drinks
And fermented wine is any.
The rapid detection method of methanol content, the detection method of the methanol in wine content are in a kind of wine, accurate
10mL Wine Sample is drawn in test tube, 0.2mL2% butyl acetate solution is added as internal standard, the concentration of internal standard solution is 352mg/
L, after instrument stabilizer, 0.5 μ L of sample introduction injects gas chromatograph, and the ratio of the peak area of methanol and butyl acetate is obtained after integral
Value, obtains the content of methanol in wine according to standard curve.
The rapid detection method of methanol content in a kind of wine, the detection method of methanol content is to draw in the alcohol
0.2mL2% butyl acetate solution is added as internal standard in test tube in 10mL alcohol sample, and the concentration of internal standard solution is 352mg/L, to
After instrument stabilizer, 0.5 μ L of sample introduction injects gas chromatograph, and the ratio of the peak area of methanol and butyl acetate, root are obtained after integral
The content of methanol in alcohol is obtained according to standard curve.
The detection method of the rapid detection method of methanol content in a kind of wine, the assembled alcoholic drinks and fermented wine is to prepare
Wine and each 100mL of fermented wine first distill, and the sample 10mL after taking distillation is added 0.2mL2% butyl acetate solution and makees in test tube
Concentration for internal standard, internal standard solution is 352mg/L, and after instrument stabilizer, 0.5 μ L of sample introduction injects gas chromatograph, is obtained after integral
The ratio of the peak area of methanol and butyl acetate obtains the content of methanol in assembled alcoholic drinks and fermented wine according to standard curve.
Claims (7)
1. the rapid detection method of methanol content in a kind of wine, which is characterized in that comprising the following specific steps
(1) ethanol solution that dose volume score is 60%: precision measures ethanol solution 600mL, is settled to 1000mL with water, mixes
It is even；
(2) the butyl acetate solution that dose volume score is 2%: precision draws butyl acetate 2mL, the ethyl alcohol prepared with step (1)
Solution is settled to 100mL, mixes；
(3) preparation of methanol standard solution: weighing methanol 0.10004g in 100mL volumetric flask, with the second prepared in step (1)
Alcoholic solution constant volume, mix, as mother liquor, then take the volumetric flask of 5 50mL, respectively draw 0.5mL, 1mL, 2.5mL, 5mL,
The above-mentioned mother liquor of 7.5mL is settled to scale with the ethanol solution that step (1) is prepared, mixes；
(4) production of methanol standard curve: the methanol standard solution of 5 prepared in step (3) not isoconcentrations is drawn respectively
Then the butyl acetate solution of 0.2mL step (2) preparation is added as internal standard, with the second of step (1) preparation in test tube in 10mL
Alcoholic solution is diluted to a certain concentration, mixes, and carries out chromatography；
(5) in 11 including methanol the mixed mark solution of flavor substance preparation: by flavor substance ethyl hexanoate, ethyl acetate,
Ethyl butyrate, acetic acid, caproic acid, normal propyl alcohol, n-butanol, isoamyl alcohol, acetic acid aldehyde, acetaldehyde and methanol are arrived according to conventional additive amount respectively
In the volumetric flask of 100mL, it is settled to scale with the ethanol solution that step (1) is prepared, mixes and is used as stock solution, draws deposit respectively
Liquid 10mL adds the butyl acetate solution of 0.2mL step (2) preparation as internal standard, and the ethanol solution prepared with step (1) is dilute
It releases to a certain concentration, mixes, carry out chromatography and draw standard curve；
(6) preparation of sample solution: sample solution is drawn into 10mL in test tube, the acetic acid fourth that 0.2mL step (2) are prepared is added
Ester solution dilutes butyl acetate to a certain concentration as internal standard, with the ethanol solution that step (1) is prepared, and mixes；
(7) gas chromatography analysis: analytical conditions for gas chromatography are as follows: HP-INNOPWAX column length 30m, column internal diameter 0.25mm,
0.25 μm of thickness of liquid film, temperature program:, keeping 7min, be warming up to 55 DEG C with 5 DEG C, be warming up to 210 DEG C with 30 DEG C by 40 DEG C of column temperature,
Keep 2min, injector temperature: 200 DEG C, detector temperature: 250 DEG C, gasify room temperature: 240 DEG C, carrier gas: nitrogen flow
0.7mL/min, hydrogen flowing quantity 35mL/min, air mass flow 350mL/min, split ratio 50:1,0.5 μ L of sample volume；
(8) drafting of standard curve and result calculate: starting gas chromatograph, according to the program setting instrument item in step (7)
Part carries out sample introduction operation after waiting instrument stabilizers respectively, the peak area of methanol and other flavor components and butyl acetate is measured, with first
The ratio between alcohol and butyl acetate concentration are abscissa, using the ratio of methanol and butyl acetate chromatographic peak area as ordinate, draw mark
Directrix curve is contrasted with the retention time of methanol and standard specimen and carries out qualitative, utilizes an alignment existing for peak area and methanol content
With inner mark method ration, according to testing result with the standard curve of foundation, methanol content in wine is calculated in sexual intercourse.
2. the rapid detection method of methanol content in a kind of wine according to claim 1, which is characterized in that the step
(3) in the concentration of methanol series standard solution be respectively 10.004mg/L, 20.008mg/L, 50.02mg/L, 100.04mg/L,
150.06mg/L。
3. the rapid detection method of methanol content in a kind of wine according to claim 1, which is characterized in that the step
(4), the concentration in (5) and (6) after the dilution of butyl acetate solution is 352mg/L.
4. the rapid detection method of methanol content in a kind of wine according to claim 1, which is characterized in that in step (6)
The sample is any of white wine, alcohol, assembled alcoholic drinks and fermented wine.
5. the rapid detection method of methanol content in a kind of wine according to claim 4, which is characterized in that the white wine
The detection method of middle methanol content is that precision draws 10mL Wine Sample in test tube, and 0.2mL2% butyl acetate solution is added and makees
Concentration for internal standard, internal standard solution is 352mg/L, and after instrument stabilizer, 0.5 μ L of sample introduction injects gas chromatograph, is obtained after integral
The ratio of the peak area of methanol and butyl acetate obtains the content of methanol in wine according to standard curve.
6. the rapid detection method of methanol content in a kind of wine according to claim 4, which is characterized in that the alcohol
The detection method of middle methanol content is to draw 10mL alcohol sample in test tube, is added in the conduct of 0.2mL2% butyl acetate solution
The concentration of mark, internal standard solution is 352mg/L, and after instrument stabilizer, 0.5 μ L of sample introduction injects gas chromatograph, obtains methanol after integral
With the ratio of the peak area of butyl acetate, the content of methanol in alcohol is obtained according to standard curve.
7. the rapid detection method of methanol content in a kind of wine according to claim 4, which is characterized in that the preparation
The detection method of wine and fermented wine is that assembled alcoholic drinks and each 100mL of fermented wine first distill, and the sample 10mL after taking distillation is in test tube
In, 0.2mL2% butyl acetate solution is added as internal standard, the concentration of internal standard solution is 352mg/L, after instrument stabilizer, sample introduction 0.5
μ L injects gas chromatograph, and the ratio of the peak area of methanol and butyl acetate is obtained after integral, is prepared according to standard curve
The content of methanol in wine and fermented wine.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110045042A (en) * | 2019-05-22 | 2019-07-23 | 遵义医科大学 | A kind of measuring method of Salted duck egg residual methanol and ethyl alcohol |
| CN110221003A (en) * | 2019-07-18 | 2019-09-10 | 青岛琛蓝海洋生物工程有限公司 | The remaining detection method of ethyl alcohol in a kind of hemostatic material |
| CN112526053A (en) * | 2020-12-29 | 2021-03-19 | 陕西延长石油（集团）有限责任公司 | Method for measuring mixed alcohol and mixed ester in industrial ethanol by gas chromatography internal standard method |
| CN113176326A (en) * | 2021-04-26 | 2021-07-27 | 上汽大众汽车有限公司 | Method for detecting methanol content of cleaning solution |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110045042A (en) * | 2019-05-22 | 2019-07-23 | 遵义医科大学 | A kind of measuring method of Salted duck egg residual methanol and ethyl alcohol |
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| CN112526053A (en) * | 2020-12-29 | 2021-03-19 | 陕西延长石油（集团）有限责任公司 | Method for measuring mixed alcohol and mixed ester in industrial ethanol by gas chromatography internal standard method |
| CN113176326A (en) * | 2021-04-26 | 2021-07-27 | 上汽大众汽车有限公司 | Method for detecting methanol content of cleaning solution |
| CN113176326B (en) * | 2021-04-26 | 2022-08-23 | 上汽大众汽车有限公司 | Method for detecting methanol content of cleaning solution |
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Application publication date: 20190319 |