CN115825277A - Method for rapidly detecting methanol in wine - Google Patents
Method for rapidly detecting methanol in wine Download PDFInfo
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- CN115825277A CN115825277A CN202211586004.3A CN202211586004A CN115825277A CN 115825277 A CN115825277 A CN 115825277A CN 202211586004 A CN202211586004 A CN 202211586004A CN 115825277 A CN115825277 A CN 115825277A
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Abstract
The invention provides a method for quickly detecting methanol in wine, belonging to the technical field of analysis and detection. The invention comprises the following steps: s1, preparing a sample to be detected and a standard solution; s2, setting a gas chromatography condition and a headspace sampling condition; s3, drawing a standard curve according to the peak area and the concentration of the standard working solution; and S4, obtaining the content of the methanol in the sample to be detected according to the standard curve. The method for rapidly detecting the methanol in the wine provided by the invention has the characteristics of simple and rapid operation, small required sample amount and the like, and is also suitable for detecting the content of the methanol in the wine with complex matrix.
Description
Technical Field
The invention relates to the technical field of analysis and detection, in particular to a method for quickly detecting methanol in wine.
Background
Methanol is also known as industrial alcohol, is a highly toxic substance and can be absorbed by respiratory tract, gastrointestinal tract and skin to cause poisoning. The fake wine and the poor wine contain high-concentration methanol, if the fake wine and the poor wine are drunk, binocular blindness can be caused slightly, death can be caused seriously, and the methanol is one of important hygienic indexes. Because a certain amount of methanol is introduced or generated in the raw materials and the brewing process of the white spirit, for example, the raw materials contain pectin, lignin and other substances, and the methanol is generated in the production processes of hydrolysis, fermentation and the like. However, because the boiling points of methanol and ethanol are close and difficult to separate, and methanol is colorless, tasteless, highly volatile and the like, and can be mixed with water and ethanol and generally cannot be identified by visual inspection, the establishment of an effective rapid analysis and detection method for methanol in white spirit is very necessary.
The existing methods for detecting methanol in white spirit have defects of different degrees, for example, GB5009.266-2016 (determination of methanol in national standard food for food safety) national standard methods have the defects of long sample detection time consumption, incapability of well separating other flavor components in the white spirit, and unsuitability for analysis and detection of batch samples; although the method for detecting the content of the methanol in the white spirit by adopting the colorimetric method is simple in required equipment, the method is complicated to operate, long in required time, difficult to completely dissolve during grinding, easy to cause errors in preparation concentration, and easy to scald operators due to carelessness because water with the temperature of 80 ℃ needs to be poured into a mortar frequently in the operation process.
The patent with the application number of 201811172734.2 discloses a method for rapidly detecting the content of methanol in wine, and the patent uses butyl acetate as an internal standard, uses an HP-INNOPWAX column and achieves the technical effect of rapidly detecting the content of methanol in wine through a gas chromatography. However, the method has the defects of long detection time, high requirement on the professional performance of operators, high detection cost and the like.
Disclosure of Invention
In view of the above, the present invention provides a method for rapidly detecting methanol in wine, comprising the following steps:
s1, preparing a sample to be detected and a standard solution
S1.1, preparation of a tert-amyl alcohol standard solution: precisely weighing 1.0100g of tert-amyl alcohol, diluting to 50ml with 40% ethanol solution to obtain 2% tert-amyl alcohol standard stock solution, and sealing and storing at 0-4 deg.C;
s1.2, preparing a methanol standard solution: accurately weighing 0.5703g of methanol, diluting with 40% ethanol solution to 50ml, preparing 11.406g/L of methanol standard stock solution, and hermetically storing at 0-4 ℃; respectively sucking 0.01mL, 0.05mL, 0.10mL, 0.20mL, 0.40mL and 0.80mL of methanol standard stock solutions into 6 10mL volumetric flasks, metering the volume to 10mL by using 40% ethanol solution, respectively adding 0.1mL of the 2% tert-amyl alcohol standard stock solution obtained in the step S1.1 after uniformly mixing to prepare a concentration gradient required by a standard curve, and preparing the concentration gradient for use;
s1.3, preparation of sample to be detected
Adding 0.1ml of tert-amyl alcohol standard stock solution with the concentration of 2% into 10ml of a sample to be detected, uniformly mixing, filtering by a filter membrane, putting 1-3ml into a headspace sample injection bottle, and detecting by a gas chromatograph;
s2, gas chromatography conditions
Adopting an Agilent 6890B gas chromatograph, an FID detector, a capillary chromatographic column DB-WAX of 30m × 0.25mm × 0.25 μm, starting temperature programming from 38 ℃, keeping for 8min, raising the temperature to 220 ℃ at the rate of 20 ℃/min, keeping for 5min, keeping the temperature of a sample inlet at 180 ℃, keeping the temperature of the detector at 250 ℃, keeping the split ratio of 40: 1, taking nitrogen as carrier gas, and keeping the flow rate of the nitrogen in the column at 1.5mL/min; injecting sample by a headspace sample injector, wherein the equilibrium temperature is 90 ℃, and the equilibrium time is 25min;
s3, making of standard curve
Measuring chromatographic peak areas of internal standard methanol and internal standard tert-amyl alcohol by using a gas chromatograph, and drawing a standard curve by using the concentration of methanol series standard working solution as a horizontal coordinate and the ratio of the chromatographic peak areas of methanol and tert-amyl alcohol as a vertical coordinate;
s4, determination of sample
Injecting the sample to be detected in the headspace sample injection bottle into a gas chromatograph, determining the nature by retention time, simultaneously recording the ratio of the chromatographic peak areas of methanol and tertiary amyl alcohol, and obtaining the concentration of the methanol in the sample to be detected according to a standard curve.
Preferably, the pore size of the filter in step S1.3 is 0.22. Mu.m.
Preferably, the sample to be tested in step S1.3 includes any one of distilled liquor, compound liquor and fermented liquor.
Preferably, when the sample to be detected is prepared wine or fermented wine, the sample to be detected needs to be distilled and then a distillate is taken for measurement, so that the problems that the impurity is excessive and a detection instrument is polluted are avoided.
Tests prove that the method for quickly detecting the methanol in the wine has higher detection sensitivity, accuracy and precision and is suitable for measuring the content of the methanol in a large batch of wine samples.
Compared with the prior art, the invention has the following beneficial effects:
1. the method for quickly detecting the methanol in the wine is not only suitable for quickly detecting the methanol content in the distilled wine of non-complex matrix samples such as white wine, whisky and brandy, but also suitable for quickly detecting the methanol content in the complex matrix prepared wine, and meets the quality requirement of batch detection no matter the color of the sample is dark and light.
2. The method for rapidly detecting the methanol in the wine provided by the invention has the characteristics of simple and rapid operation, small required sample amount and the like.
3. The invention adopts a headspace sampling method, strictly limits the heating temperature and the balance time of headspace sampling, further ensures that organic components are volatilized to the maximum extent under the condition of less water evaporation amount, so that the organic components enter a gas chromatograph along with gas, and also strictly limits a temperature rise program, so that different organic components are better separated.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be clearly and completely described below. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The test methods or test methods described in the following examples are conventional methods unless otherwise specified; the starting materials and auxiliaries are, unless specified otherwise, either obtained from customary commercial sources or prepared in customary manner.
Example 1
A method for rapidly detecting methanol in wine comprises the following specific steps:
s1, preparing white spirit samples and standard solutions
S1.1, preparation of a tert-amyl alcohol standard solution: precisely weighing 1.0100g of tert-amyl alcohol, diluting to 50ml with 40% ethanol solution to obtain 2% tert-amyl alcohol standard stock solution, and storing at 4 deg.C under sealed condition;
s1.2, preparing a methanol standard solution: precisely weighing 0.5703g of methanol, metering the volume to 50ml by using a 40% ethanol solution, preparing 11.406g/L of methanol standard stock solution, and storing the stock solution in a sealing way at 4 ℃; respectively sucking 0.01mL, 0.05mL, 0.10mL, 0.20mL, 0.40mL and 0.80mL of methanol standard stock solutions into 6 volumetric flasks with 10mL, fixing the volume to 10mL by using 40% ethanol solution, respectively adding 0.1mL of the 2% tert-amyl alcohol standard stock solution in the step S1.1 after uniformly mixing to prepare a concentration gradient required by a standard curve, and preparing the solution for use;
s1.3, preparation of white spirit sample
Adding 0.1ml of tert-amyl alcohol standard stock solution with the concentration of 2% into a 10ml white spirit sample, uniformly mixing, filtering by a filter membrane with the aperture of 0.22 mu m, putting 1ml into a headspace sample injection bottle, and detecting by a gas chromatograph;
s2, gas chromatography conditions
Adopting an Agilent 6890B gas chromatograph, an FID detector, a capillary chromatographic column DB-WAX of 30m × 0.25mm × 0.25 μm, starting temperature programming from 38 ℃, keeping for 8min, raising the temperature to 220 ℃ at the rate of 20 ℃/min, keeping for 5min, keeping the temperature of a sample inlet at 180 ℃, keeping the temperature of the detector at 250 ℃, keeping the split ratio of 40: 1, taking nitrogen as carrier gas, and keeping the flow rate of the nitrogen in the column at 1.5mL/min; injecting sample by a headspace sample injector, wherein the equilibrium temperature is 90 ℃, and the equilibrium time is 25min;
s3, making of standard curve
Measuring chromatographic peak areas of internal standard methanol and internal standard tert-amyl alcohol by using a gas chromatograph, and drawing a standard curve by using the concentration of methanol series standard working solution as a horizontal coordinate and the ratio of the chromatographic peak areas of methanol and tert-amyl alcohol as a vertical coordinate;
s4, determination of sample
And (3) injecting the white spirit sample in the headspace sampling bottle into a gas chromatograph, determining the nature of the retention time, recording the ratio of the chromatographic peak areas of the methanol and the tertiary amyl alcohol, and obtaining the concentration of the methanol in the white spirit sample according to a standard curve.
Example 2
A method for rapidly detecting methanol in wine comprises the following specific steps:
s1, preparing a wine sample and a standard solution
S1.1, preparation of a tert-amyl alcohol standard solution: precisely weighing 1.0100g of tert-amyl alcohol, diluting to 50ml with 40% ethanol solution to obtain 2% tert-amyl alcohol standard stock solution, and storing at 4 deg.C under sealed condition;
s1.2, preparing a methanol standard solution: precisely weighing 0.5703g of methanol, metering the volume to 50ml by using a 40% ethanol solution, preparing 11.406g/L of methanol standard stock solution, and storing the stock solution in a sealing way at 4 ℃; respectively sucking 0.01mL, 0.05mL, 0.10mL, 0.20mL, 0.40mL and 0.80mL of methanol standard stock solutions into 6 10mL volumetric flasks, metering the volume to 10mL by using 40% ethanol solution, respectively adding 0.1mL of the 2% tert-amyl alcohol standard stock solution obtained in the step S1.1 after uniformly mixing to prepare a concentration gradient required by a standard curve, and preparing the concentration gradient for use;
s1.3, preparation of a sample of the prepared wine
Distilling 100ml of the compound wine to obtain distilled compound wine, adding 0.1ml of tert-amyl alcohol standard stock solution with the concentration of 2% into 10ml of distilled compound wine, uniformly mixing, filtering by a filter membrane with the aperture of 0.22 mu m, taking 2ml of the mixture, placing in a headspace sample injection bottle, and detecting by a gas chromatograph;
s2, gas chromatography conditions
Adopting an Agilent 6890B gas chromatograph, an FID detector, a capillary chromatographic column DB-WAX of 30m × 0.25mm × 0.25 μm, starting temperature programming from 38 ℃, keeping for 8min, raising the temperature to 220 ℃ at the rate of 20 ℃/min, keeping for 5min, keeping the temperature of a sample inlet at 180 ℃, keeping the temperature of the detector at 250 ℃, keeping the split ratio of 40: 1, taking nitrogen as carrier gas, and keeping the flow rate of the nitrogen in the column at 1.5mL/min; injecting sample by a headspace sample injector, wherein the equilibrium temperature is 90 ℃, and the equilibrium time is 25min;
s3, making of standard curve
Measuring chromatographic peak areas of internal standard methanol and internal standard tert-amyl alcohol by using a gas chromatograph, and drawing a standard curve by using the concentration of methanol series standard working solution as a horizontal coordinate and the ratio of the chromatographic peak areas of methanol and tert-amyl alcohol as a vertical coordinate;
s4, determination of sample
And injecting the prepared wine sample in the headspace sampling bottle into a gas chromatograph, determining the nature of the retention time, recording the ratio of the chromatographic peak areas of the methanol and the tertiary amyl alcohol, and obtaining the concentration of the methanol in the prepared wine sample according to a standard curve.
Example 3
A method for rapidly detecting methanol in wine comprises the following specific steps:
s1, preparing fermented wine samples and standard solutions
S1.1, preparation of a tert-amyl alcohol standard solution: precisely weighing 1.0100g of tert-amyl alcohol, diluting to 50ml with 40% ethanol solution to obtain 2% tert-amyl alcohol standard stock solution, and storing at 4 deg.C under sealed condition;
s1.2, preparing a methanol standard solution: precisely weighing 0.5703g of methanol, metering the volume to 50ml by using a 40% ethanol solution, preparing 11.406g/L of methanol standard stock solution, and storing the stock solution in a sealing way at 4 ℃; respectively sucking 0.01mL, 0.05mL, 0.10mL, 0.20mL, 0.40mL and 0.80mL of methanol standard stock solutions into 6 10mL volumetric flasks, metering the volume to 10mL by using 40% ethanol solution, respectively adding 0.1mL of the 2% tert-amyl alcohol standard stock solution obtained in the step S1.1 after uniformly mixing to prepare a concentration gradient required by a standard curve, and preparing the concentration gradient for use;
s1.3, preparation of fermented wine sample
Distilling 100ml of fermented wine to obtain distilled fermented wine, adding 0.1ml of tert-amyl alcohol standard stock solution with the concentration of 2% into 10ml of distilled fermented wine, uniformly mixing, filtering by a filter membrane with the aperture of 0.22 mu m, taking 3ml of the distilled fermented wine, placing the mixed solution into a headspace sample bottle, and detecting by a gas chromatograph;
s2, gas chromatography conditions
Adopting an Agilent 6890B gas chromatograph, an FID detector, a capillary chromatographic column DB-WAX with the thickness of 30m multiplied by 0.25mm multiplied by 0.25 mu m, starting the temperature programming from 38 ℃ at the initial temperature, keeping for 8min, heating to 220 ℃ at the speed of 20 ℃/min, keeping for 5min, keeping the temperature of a sample inlet at 180 ℃, keeping the temperature of the detector at 250 ℃, and dividing ratio of 40: 1, taking nitrogen as carrier gas, and keeping the flow rate of the nitrogen in the column at 1.5mL/min; injecting sample by a headspace sample injector, wherein the equilibrium temperature is 90 ℃, and the equilibrium time is 25min;
s3, making of standard curve
Measuring chromatographic peak areas of internal standard methanol and internal standard tert-amyl alcohol by using a gas chromatograph, and drawing a standard curve by using the concentration of methanol series standard working solution as a horizontal coordinate and the ratio of the chromatographic peak areas of methanol and tert-amyl alcohol as a vertical coordinate;
s4, determination of sample
And injecting the fermented wine sample in the headspace sample injection bottle into a gas chromatograph, determining the nature of the retention time, recording the ratio of the chromatographic peak areas of methanol and tertiary amyl alcohol, and obtaining the concentration of the methanol in the fermented wine sample according to a standard curve.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (4)
1. A method for rapidly detecting methanol in wine is characterized by comprising the following steps:
s1, preparing a sample to be detected and a standard solution
S1.1, preparation of a tert-amyl alcohol standard solution: precisely weighing 1.0100g of tert-amyl alcohol, diluting to 50ml with 40% ethanol solution to obtain 2% tert-amyl alcohol standard stock solution, and sealing and storing at 0-4 deg.C;
s1.2, preparing a methanol standard solution: precisely weighing 0.5703g of methanol, metering the volume to 50ml by using a 40% ethanol solution, preparing 11.406g/L of methanol standard stock solution, and hermetically storing at 0-4 ℃; respectively sucking 0.01mL, 0.05mL, 0.10mL, 0.20mL, 0.40mL and 0.80mL of methanol standard stock solutions into 6 10mL volumetric flasks, metering the volume to 10mL by using 40% ethanol solution, respectively adding 0.1mL of the 2% tert-amyl alcohol standard stock solution obtained in the step S1.1 after uniformly mixing to prepare a concentration gradient required by a standard curve, and preparing the concentration gradient for use;
s1.3, preparation of sample to be detected
Adding 0.1ml of tert-amyl alcohol standard stock solution with the concentration of 2% into 10ml of a sample to be detected, uniformly mixing, filtering by a filter membrane, putting 1-3ml into a headspace sample injection bottle, and detecting by a gas chromatograph;
s2, gas chromatography conditions
Adopting an Agilent 6890B gas chromatograph, an FID detector, a capillary chromatographic column DB-WAX with the thickness of 30m multiplied by 0.25mm multiplied by 0.25 mu m, starting the temperature programming from 38 ℃ at the initial temperature, keeping for 8min, heating to 220 ℃ at the speed of 20 ℃/min, keeping for 5min, keeping the temperature of a sample inlet at 180 ℃, keeping the temperature of the detector at 250 ℃, and dividing ratio of 40: 1, taking nitrogen as carrier gas, and keeping the flow rate of the nitrogen in the column at 1.5mL/min; injecting sample by a headspace sample injector, wherein the equilibrium temperature is 90 ℃, and the equilibrium time is 25min;
s3, making of standard curve
Measuring chromatographic peak areas of internal standard methanol and internal standard tert-amyl alcohol by using a gas chromatograph, and drawing a standard curve by using the concentration of methanol series standard working solution as a horizontal coordinate and the ratio of the chromatographic peak areas of methanol and tert-amyl alcohol as a vertical coordinate;
s4, determination of sample
Injecting the sample to be detected in the headspace sample injection bottle into a gas chromatograph, determining the nature by retention time, simultaneously recording the ratio of the chromatographic peak areas of methanol and tertiary amyl alcohol, and obtaining the concentration of the methanol in the sample to be detected according to a standard curve.
2. The method for rapid detection of methanol in wine as claimed in claim 1, wherein the pore size of the filter membrane in step S1.3 is 0.22 μm.
3. The method for rapidly detecting methanol in wine according to claim 1, wherein the sample to be detected in step S1.3 comprises any one of distilled wine, prepared wine and fermented wine.
4. The method as claimed in claim 3, wherein when the sample is a compound wine or a fermented wine, the distillate is obtained by distilling the sample.
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