CN104028005B - A kind of membrane extraction method of enrichment Dietary Ethyl Carbamate in Wine - Google Patents
A kind of membrane extraction method of enrichment Dietary Ethyl Carbamate in Wine Download PDFInfo
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- CN104028005B CN104028005B CN201410259517.2A CN201410259517A CN104028005B CN 104028005 B CN104028005 B CN 104028005B CN 201410259517 A CN201410259517 A CN 201410259517A CN 104028005 B CN104028005 B CN 104028005B
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Abstract
The invention belongs to chemical substance in wine samples and detect pretreatment technology method, a kind of particularly membrane extraction method of enrichment Dietary Ethyl Carbamate in Wine.The present invention uses hollow fiber membrane extraction assembly to extract grape wine, enrichment urethanes wherein; Wherein, the wine samples through pre-treatment flows in the pipe inside (tube side) of hollow-fibre membrane, and extraction organic solvent flows in the pipe outside (shell side) of hollow-fibre membrane.The method of the inventive method membrane extraction carries out fast enriching to urethanes in fermentating wine, to meet quick, trace detection demand, improves qualitative and quantitative analysis sensitivity.The invention has the advantages that the new method providing harmful substance urethanes in a kind of fast enriching grape wine, for its content accurate quantitative analysis provides effective pre-treating method.
Description
Technical field
The invention belongs to chemical substance in wine samples and detect pretreatment technology method, a kind of particularly membrane extraction method of enrichment Dietary Ethyl Carbamate in Wine.
Background technology
Urethanes is pick-me-up (as grape wine, applejack, yellow rice wine, pure mellow wine etc.) one of spontaneous accessory substance in fermentation or storage process.Arginine in liquor-making raw material is decomposed into urea and ornithine by metabolism of yeasts brewageing in sweat, and urea constantly accumulates and the phase is discharged in wine in a large number after fermentation, and urea and ethanol spontaneous reaction generate urethanes.Therefore, fermentation alcohol beverage is one of mankind's main source taking in urethanes.Urethanes is just found to have carcinogenicity as far back as the sixties in last century five.The late nineteen eighties, countries in the world researcher detects urethanes in the alcoholic beverage such as Spirit, brandy, whiskey, grape wine, and confirms its carcinogenicity further.Research shows, urethanes is a kind of multidigit point carcinogenic substance, can cause the diseases such as lung cancer, lymph cancer, liver cancer, cutaneum carcinoma.2007, the international cancer research institution of the World Health Organization assessed urethanes, and formally it was promoted to 2A class carcinogenic substance by 2B class, dangerous on an equal basis with acrylamide.External a lot of country (as Canadian, Japanese etc.) has formulated the limit standard of urethanes in alcoholic beverage, and the scope of limiting the quantity of the kind according to wine is often raised to a few hectogamma from ten micrograms and does not often rise not etc.
The detection method that urethanes is conventional to have after GC-MS, tablets by HPLC-MS and fluorescent derivatization HPLC fluorometric etc.These analytical methods need to carry out more loaded down with trivial details pre-treatment to sample before detecting, and the urethanes in extraction, concentrating sample realizes the target improving detection sensitivity.Pre-treating method conventional at present has SPE, column chromatography and multistage liquid-liquid extraction etc.These sample-pretreating methods are length consuming time usually, complex operation, and loss is comparatively large, and the rate of recovery is low, thus affect the urethanes in fermented wine beverage accurate, efficiently measure.
Membrane extraction, as the one of membrane separation technique, is a kind of new separation technology combined with liquid-liquid extraction process by membrane separating process.Microporous barrier is placed between material sample liquid and extraction solution by membrane extraction principle exactly, extraction solution promptly soaks into each micropore of film to the wellability of film, and contact with opposite side material sample liquid and form stable boundary layer, separated solute is transferred to extract from material solution through boundary layer.Owing to needing separated solute to carry out mass transfer by micropore, so the dispersion that effectively prevent in level mutually and polymerization.Meanwhile, the liquid-liquid two-phase flow owing to not forming directly contact in membrane extraction moves, so can greatly relax the requirement of the physical property such as density, viscosity, interfacial tension during slective extraction liquid; And process is seldom by the impact of back-mixing and the restriction of liquid flooding condition, selective extraction and accumulation ability also can improve.In addition, hollow fiber membrane extraction has very large mass transfer specific area, and its numerical value is generally about 3000m2m-3, and larger than general extraction contact area 10 ~ 50 times, substantially reduce extraction required time, efficiency is higher.Therefore, hollow fiber membrane extraction has that extractant loss limits less, without liquid flooding, the advantage such as rapidly and efficiently, is widely used in the aspects such as organic matter extraction, metal extraction, biochemical products, pharmaceutical extraction and sample separation enrichment pre-treatment.
Summary of the invention
The object of the invention is to overcome prior art deficiency, a kind of membrane extraction method of enrichment Dietary Ethyl Carbamate in Wine is provided, the method is simple, economical and effective, can be used as the rapid concentration enrichment that sample-pretreating method is applicable to testing sample in industrial online production process.
Technical scheme of the present invention is summarized as follows:
A membrane extraction method for enrichment Dietary Ethyl Carbamate in Wine, uses hollow fiber membrane extraction assembly to extract grape wine, enrichment urethanes wherein; Wherein, the wine samples through pre-treatment flows in the pipe inside (tube side) of hollow-fibre membrane, and extraction organic solvent flows in the pipe outside (shell side) of hollow-fibre membrane.
A membrane extraction method for enrichment Dietary Ethyl Carbamate in Wine, its concrete steps are as follows:
(1) learnt from else's experience pre-treatment containing the wine samples 20 ~ 40 milliliters of urethanes, put into the conical flask of 50 ~ 100 milliliters, promote wine samples with peristaltic pump to circulate in the pipe inside (tube side) of hollow-fibre membrane, flow velocity is 10 ~ 15 ml/min;
(2) get extraction organic solvent 60 ~ 90 milliliters, be placed in 100 ~ 200 milliliters of conical flasks, drive with peristaltic pump and circulate in the pipe outside (shell side) of hollow-fibre membrane, flow velocity is 8 ~ 10 ml/min;
(3) when wine samples and extraction organic solvent start timing when extraction occurs hollow-fibre membrane interracial contact, extraction carries out 10 ~ 15 minutes;
(4) after having extracted, the organic solvent of extraction is concentrated into 10 ~ 20 milliliters and carries out analysis detection, can gas chromatography combined with mass spectrometry be adopted, or after fluorescent derivatization, liquid chromatogram fluorescence detector carries out analysis and measures.
Described organic solvent is carrene, toluene or chloroform.
Described hollow fiber membrane extraction assembly forms by being assembled into by hollow-fibre membrane pipe in the corrosion-resistant material equipment such as stainless steel or glass to build, and described hollow-fibre membrane pipe 20 ~ 100 is one group.
The preparation method of described hollow fiber membrane extraction assembly is as follows:
(1) being averaged external diameter is 0.25 ~ 0.35 millimeter, and length is the hollow-fibre membrane pipe 20 ~ 100 of 200 ~ 350 millimeters is one group;
(2) with volume fraction be 80% ~ 95% ethanol water soak 10 ~ 15 minutes;
(3) hollow-fibre membrane pipe group is assembled in the glass tube with turnover arm, and is cast into hollow fiber membrane extraction assembly.
Described hollow fiber membrane extraction assembly is by Kynoar, and polypropylene or polytetrafluoroethylene (PTFE) hollow fiber polymer membrane material are prepared from, and have solvent resistant, hydrophobicity is good, and resistance to pressure is strong, and specific area is large, and (mass transfer specific area is generally 3000m
2m
-3) feature.
In described wine samples, the concentration of urethanes is 0.5 ~ 120 micrograms per litre.
The pre-treating method of described wine samples is: take urethanes 0.010 gram, being dissolved into 40 ml volumes marks is in the ethanol water of 12%, be that the ethanol water constant volume of 12% is to 100 milliliters by volume fraction again, configuration concentration is the urethanes standard specimen of 100 mg/litre, getting quantitative urethanes standard specimen respectively with micro liquid sampler joins in wine samples, makes the content of urethanes in wine samples between 0.5 ~ 120 micrograms per litre.
The preparation of hollow fiber membrane extraction assembly:
(1) Pvdf Microporous Hollow Fiber Membrane pipe 20 ~ 80 is one group, soak 10 ~ 15 minutes with the ethanol water that volume fraction is 90%, Pvdf Microporous Hollow Fiber Membrane pipe group is assembled in the glass tube with turnover arm, and is cast into hollow fiber membrane extraction assembly with corrosion-resisting resin;
(2) polypropylene hollow fiber membrane pipe 20 ~ 100 is one group, soak 10 ~ 15 minutes with the ethanol water that volume fraction is 95%, polypropylene hollow fiber membrane pipe group is assembled in the glass tube with turnover arm, and is cast into hollow fiber membrane extraction assembly with corrosion-resisting resin;
(3) polytetrafluoroethylhollow hollow fiber membrane pipe 30 ~ 90 is one group, soak 10 ~ 15 minutes with the ethanol water that volume fraction is 85%, polytetrafluoroethylhollow hollow fiber membrane pipe group is assembled in the glass tube with turnover arm, and is cast into hollow fiber membrane extraction assembly with corrosion-resisting resin.
Beneficial effect of the present invention is:
The advantage of the inventive method is can extracting and enriching urethanes from grape wine rapidly and efficiently by the method for hollow fiber membrane extraction, substantially reduce extraction time, extracting and enriching process can be effectively completed in 15 minutes, whole extraction process organic solvent does not lose substantially, and avoid the phenomenon of emulsification common in traditional liquid-liquid extraction, unsuitable layering, the inventive method extracting and enriching rate of recovery is between 78% ~ 120%, and method is quick, effective, and accuracy rate is good.
Accompanying drawing explanation
Fig. 1 a is hollow fiber membrane extraction mechanism of mass transfer schematic diagram; Fig. 1 b is hollow fiber membrane extraction device operating process schematic diagram;
Number in the figure: 1-wine samples storage device; 2-organic solvent storage device; 3-hollow fiber membrane extraction assembly; 4-bypass return line; 5-pump; 6-Pressure gauge; V
1, V
2-grape wine sample flow control valve; V
3, V
4-organic solvent flow control valve;
Fig. 2 is urethanes rate of recovery contrast block diagram in Kynoar, polypropylene and polytetrafluoroethylene (PTFE) three kinds of unlike material solvent resistant hollow fiber film tube extracting and enriching wine samples.
Detailed description of the invention
The invention provides a kind of membrane extraction method of enrichment Dietary Ethyl Carbamate in Wine, below in conjunction with accompanying drawing with specifically the present invention will be further described.
Embodiment 1
Be averaged external diameter and be about 0.28 millimeter, the Kynoar solvent resistant hydrophobic polymer hollow fiber film tube 60 of long 300 millimeters is one group; Be 95% alcohol immersion 10 minutes by volume fraction, then Pvdf Microporous Hollow Fiber Membrane pipe be assembled in the glass tube with turnover arm, and water with corrosion-resisting resin and build up hollow fiber membrane extraction assembly.Take urethanes 0.010 gram, being dissolved into 40 ml volumes marks is in the ethanol water of 12%, constant volume is to 100 milliliters again, be configured to the urethanes standard specimen that concentration is 100 mg/litre, quantitatively pipetting urethanes standard specimen with micro liquid sampler joins in wine samples, makes the content of urethanes in wine samples be 20 micrograms per litre.Get the wine samples 20 milliliters containing urethanes, put into the conical flask of 50 milliliters, promote wine samples with peristaltic pump and circulate at hollow fiber film tube inside (tube side), flow velocity is 12 ml/min.Get carrene 60 milliliters, be placed in 100 milliliters of conical flasks, drive with peristaltic pump and circulate at hollow fiber film tube outside (shell side), flow velocity is 8 ml/min.When wine samples and extraction organic solvent start timing when extraction occurs hollow-fibre membrane interracial contact, after extraction carries out 11 minutes, organic solvent after extraction is evaporated to 10 milliliters, and adopting gas chromatography combined with mass spectrometry method to measure the rate of recovery is 78%.
Embodiment 2
Be averaged external diameter and be about 0.28 millimeter, the polypropylene solvent resistant hydrophobic polymer hollow fiber film tube 60 of long 300 millimeters is one group; Be 95% alcohol immersion 10 minutes by volume fraction, then polypropylene hollow fiber membrane pipe be assembled in the glass tube with turnover arm, and water with corrosion-resisting resin and build up hollow fiber membrane extraction assembly.Take urethanes 0.010 gram, being dissolved into 40 ml volumes marks is in the ethanol water of 12%, constant volume is to 100 milliliters again, be configured to the urethanes standard specimen that concentration is 100 mg/litre, quantitatively pipetting urethanes standard specimen with micro liquid sampler joins in wine samples, makes the content of urethanes in wine samples be 20 micrograms per litre.Get the wine samples 20 milliliters containing urethanes, put into the conical flask of 50 milliliters, promote wine samples with peristaltic pump and circulate at hollow fiber film tube inside (tube side), flow velocity is 12 ml/min.Get carrene 60 milliliters, be placed in 100 milliliters of conical flasks, drive with peristaltic pump and circulate at hollow fiber film tube outside (shell side), flow velocity is 8 ml/min.When wine samples and extraction organic solvent start timing when extraction occurs hollow-fibre membrane interracial contact, after extraction carries out 11 minutes, organic solvent after extraction is evaporated to 10 milliliters, and adopting gas chromatography combined with mass spectrometry method to measure the rate of recovery is 98%.
Embodiment 3
Be averaged external diameter and be about 0.28 millimeter, the polytetrafluoroethylene (PTFE) solvent resistant hydrophobic polymer hollow fiber film tube 60 of long 300 millimeters is one group; Be 95% alcohol immersion 10 minutes by volume fraction, then polytetrafluoroethylhollow hollow fiber membrane pipe be assembled in the glass tube with turnover arm, and water with corrosion-resisting resin and build up hollow fiber membrane extraction assembly.Take urethanes 0.010 gram, being dissolved into 40 ml volumes marks is in the ethanol water of 12%, constant volume is to 100 milliliters again, be configured to the urethanes standard specimen that concentration is 100 mg/litre, quantitatively pipetting urethanes standard specimen with micro liquid sampler joins in wine samples, makes the content of urethanes in wine samples be 20 micrograms per litre.Get the wine samples 20 milliliters containing urethanes, put into the conical flask of 50 milliliters, promote wine samples with peristaltic pump and circulate at hollow fiber film tube inside (tube side), flow velocity is 12 ml/min.Get carrene 60 milliliters, be placed in 100 milliliters of conical flasks, drive with peristaltic pump and circulate at hollow fiber film tube outside (shell side), flow velocity is 8 ml/min.When wine samples and extraction organic solvent start timing when extraction occurs hollow-fibre membrane interracial contact, after extraction carries out 11 minutes, organic solvent after extraction is evaporated to 10 milliliters, and adopting gas chromatography combined with mass spectrometry method to measure the rate of recovery is 78%.
Embodiment 4
Be averaged external diameter and be about 0.32 millimeter, the Kynoar solvent resistant hydrophobic polymer hollow fiber film tube 80 of long 280 millimeters is one group; Be 95% alcohol immersion 15 minutes by volume fraction, then Pvdf Microporous Hollow Fiber Membrane pipe be assembled in the glass tube with turnover arm, and water with corrosion-resisting resin and build up hollow fiber membrane extraction assembly.Take urethanes 0.010 gram, being dissolved into 40 ml volumes marks is in the ethanol water of 12%, constant volume is to 100 milliliters again, be configured to the urethanes standard specimen that concentration is 100 mg/litre, quantitatively pipetting urethanes standard specimen with micro liquid sampler joins in wine samples, makes the content of urethanes in wine samples be 40 micrograms per litre.Get the wine samples 30 milliliters containing urethanes, put into the conical flask of 50 milliliters, promote wine samples with peristaltic pump and circulate at hollow fiber film tube inside (tube side), flow velocity is 15 ml/min.Get carrene 80 milliliters, be placed in 200 milliliters of conical flasks, drive with peristaltic pump and circulate at hollow fiber film tube outside (shell side), flow velocity is 10 ml/min.When wine samples and extraction organic solvent start timing when extraction occurs hollow-fibre membrane interracial contact, after extraction carries out 15 minutes, organic solvent after extraction is evaporated to 15 milliliters, and adopting gas chromatography combined with mass spectrometry method to measure the rate of recovery is 88%.
Embodiment 5
Be averaged external diameter and be about 0.32 millimeter, the polypropylene solvent resistant hydrophobic polymer hollow fiber film tube 80 of long 280 millimeters is one group; Be 95% alcohol immersion 15 minutes by volume fraction, then polypropylene hollow fiber membrane pipe be assembled in the glass tube with turnover arm, and water with corrosion-resisting resin and build up hollow fiber membrane extraction assembly.Take urethanes 0.010 gram, being dissolved into 40 ml volumes marks is in the ethanol water of 12%, constant volume is to 100 milliliters again, be configured to the urethanes standard specimen that concentration is 100 mg/litre, quantitatively pipetting urethanes standard specimen with micro liquid sampler joins in wine samples, makes the content of urethanes in wine samples be 40 micrograms per litre.Get the wine samples 30 milliliters containing urethanes, put into the conical flask of 50 milliliters, promote wine samples with peristaltic pump and circulate at hollow fiber film tube inside (tube side), flow velocity is 15 ml/min.Get carrene 80 milliliters, be placed in 200 milliliters of conical flasks, drive with peristaltic pump and circulate at hollow fiber film tube outside (shell side), flow velocity is 10 ml/min.When wine samples and extraction organic solvent start timing when extraction occurs hollow-fibre membrane interracial contact, after extraction carries out 15 minutes, organic solvent after extraction is evaporated to 15 milliliters, and adopting gas chromatography combined with mass spectrometry method to measure the rate of recovery is 112%.
Embodiment 6
Be averaged external diameter and be about 0.32 millimeter, the polytetrafluoroethylene (PTFE) solvent resistant hydrophobic polymer hollow fiber film tube 80 of long 280 millimeters is one group; Be 95% alcohol immersion 15 minutes by volume fraction, then polytetrafluoroethylhollow hollow fiber membrane pipe be assembled in the glass tube with turnover arm, and water with corrosion-resisting resin and build up hollow fiber membrane extraction assembly.Take urethanes 0.010 gram, being dissolved into 40 ml volumes marks is in the ethanol water of 12%, constant volume is to 100 milliliters again, be configured to the urethanes standard specimen that concentration is 100 mg/litre, quantitatively pipetting urethanes standard specimen with micro liquid sampler joins in wine samples, makes the content of urethanes in wine samples be 40 micrograms per litre.Get the wine samples 30 milliliters containing urethanes, put into the conical flask of 50 milliliters, promote wine samples with peristaltic pump and circulate at hollow fiber film tube inside (tube side), flow velocity is 15 ml/min.Get carrene 80 milliliters, be placed in 200 milliliters of conical flasks, drive with peristaltic pump and circulate at hollow fiber film tube outside (shell side), flow velocity is 10 ml/min.When wine samples and extraction organic solvent start timing when extraction occurs hollow-fibre membrane interracial contact, after extraction carries out 15 minutes, organic solvent after extraction is evaporated to 15 milliliters, and adopting gas chromatography combined with mass spectrometry method to measure the rate of recovery is 82%.
Urethanes in the extraction of the inventive method application membrane extraction technology, enriched sample not easily produces emulsification, and easy and simple to handle, the used time is short, can realize continuous extraction; And film component device is reusable, the rate of recovery is better, is applicable to the pre-treating method as production line detects fast.
Claims (7)
1. a membrane extraction method for enrichment Dietary Ethyl Carbamate in Wine, is characterized in that: use hollow fiber membrane extraction assembly to extract grape wine, enrichment urethanes wherein; Wherein, through the wine samples of pre-treatment in the pipe internal flow of hollow-fibre membrane, extraction organic solvent is in the pipe flows outside of hollow-fibre membrane;
Concrete steps are as follows:
(1) learnt from else's experience pre-treatment containing the wine samples 20 ~ 40 milliliters of urethanes, put into the conical flask of 50 ~ 100 milliliters, promote wine samples with peristaltic pump to flow in the pipe inner loop of hollow-fibre membrane, flow velocity is 10 ~ 15 ml/min;
(2) get extraction organic solvent 60 ~ 90 milliliters, be placed in 100 ~ 200 milliliters of conical flasks, drive with peristaltic pump and flow in the pipe outer loop of hollow-fibre membrane, flow velocity is 8 ~ 10 ml/min;
(3) when wine samples and extraction organic solvent start timing when extraction occurs hollow-fibre membrane interracial contact, extraction carries out 10 ~ 15 minutes;
(4), after having extracted, the organic solvent of extraction is concentrated into 10 ~ 20 milliliters and carries out analysis detection.
2. the membrane extraction method of a kind of enrichment Dietary Ethyl Carbamate in Wine according to claim 1, is characterized in that: described organic solvent is carrene, toluene or chloroform.
3. the membrane extraction method of a kind of enrichment Dietary Ethyl Carbamate in Wine according to claim 1, it is characterized in that: described hollow fiber membrane extraction assembly forms by being assembled into by hollow-fibre membrane pipe in corrosion-resistant material equipment to build, and described hollow-fibre membrane pipe 20 ~ 100 is one group.
4. the membrane extraction method of a kind of enrichment Dietary Ethyl Carbamate in Wine according to claim 3, is characterized in that, the preparation method of described hollow fiber membrane extraction assembly is as follows:
(1) being averaged external diameter is 0.25 ~ 0.35 millimeter, and length is the hollow-fibre membrane pipe 20 ~ 100 of 200 ~ 350 millimeters is one group;
(2) with volume fraction be 80% ~ 95% ethanol water soak 10 ~ 15 minutes;
(3) hollow-fibre membrane pipe group is assembled in the glass tube with turnover arm, and is cast into hollow fiber membrane extraction assembly.
5. the membrane extraction method of a kind of enrichment Dietary Ethyl Carbamate in Wine according to any one of claim 3 or 4, it is characterized in that: described hollow fiber membrane extraction assembly is by Kynoar, and polypropylene or polytetrafluoroethylene (PTFE) hollow fiber polymer membrane material are prepared from.
6. the membrane extraction method of a kind of enrichment Dietary Ethyl Carbamate in Wine according to claim 1, is characterized in that: in described wine samples, the concentration of urethanes is 0.5 ~ 120 micrograms per litre.
7. the membrane extraction method of a kind of enrichment Dietary Ethyl Carbamate in Wine according to claim 6, it is characterized in that, the pre-treating method of described wine samples is: take urethanes 0.010 gram, being dissolved into 40 ml volumes marks is in the ethanol water of 12%, be that the ethanol water constant volume of 12% is to 100 milliliters by volume fraction again, configuration concentration is the urethanes standard specimen of 100 mg/litre, getting quantitative urethanes standard specimen respectively with micro liquid sampler joins in wine samples, make the content of urethanes in wine samples between 0.5 ~ 120 micrograms per litre.
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| CN108505214B (en) * | 2018-06-07 | 2020-10-02 | 南京宁高晶测生物科技有限公司 | Preparation method of nanofiber membrane for detecting content of ethyl carbamate |
| CN110302682B (en) * | 2019-06-30 | 2021-10-01 | 浙江工业大学 | Method and device for separating methyl linolenate based on hollow fiber liquid membrane |
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