CN110907584B - Method for detecting alcohol degree of non-alcoholic liquid - Google Patents
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Abstract
The invention provides a method for detecting the alcohol degree of non-alcoholic liquid, and relates to the technical field of alcohol degree detection. The method comprises the steps of preparing an ethanol standard solution and a mobile phase solution; the method comprises the three steps of establishing a standard curve and detecting the alcohol degree of a sample, and detecting the alcohol degree of the non-alcoholic liquid by using a high performance liquid chromatography, wherein the detection limit of the method is 0.1 degree, the detection linear range is 0.1-10 degrees, the linearity is good, the detection result is accurate, the Relative Standard Deviation (RSD) is 0.36-2.33%, the recovery rate is 96.1-103.7%, the used sample amount is small, the generated waste liquid is less, and the operation is simple and rapid.
Description
The technical field is as follows:
the invention relates to the technical field of alcohol degree detection, in particular to an alcohol degree detection method of non-alcoholic liquid.
Background art:
the alcohol degree is used for representing the content of ethanol in a solution, the detection of the alcohol degree is generally applied to alcoholic beverages or foods, and the alcohol degree is one of important indexes for measuring the foods. In recent years, with the development of analytical techniques, some micro-and ultra-micro analytical techniques have come to be applied in the research in the food field, including: gas chromatography, high performance liquid chromatography, nuclear magnetic resonance, gas chromatography-mass spectrometry, gas chromatography-infrared spectrometry, etc. Gas chromatography is most commonly used to detect alcohol levels.
For some non-alcoholic liquids, such as: some liquids such as vinegar, soy sauce, vegetable oil, fruit juice, etc. containing a small amount of ethanol also need to be tested for their alcohol degree. For example, ethanol is an important flavor substance in fermented foods such as seasonings, and different degrees of ethanol can cause different flavors; the aroma component is one of important indexes for evaluating the quality of soy sauce and vinegar, and the ethanol is an important characteristic aroma component of soy sauce and vinegar. Therefore, it is particularly important to measure the alcohol content of these non-alcoholic liquids. Currently, gas chromatography, including packed column gas chromatography, capillary column gas chromatography, and headspace gas chromatography (HSGC), is mostly used to detect the degree of alcohol. Among them, the headspace gas chromatography has a relatively good detection effect, and is a method for analyzing a gas in equilibrium with a liquid (or solid) sample in a closed system by using the gas chromatography. The HSGC method adopts gas sample introduction, avoids the pollution of sample matrixes to a chromatographic column, and can remove the interference of non-volatile matters, so that a spectrogram is simple and interference peaks are few.
Chinese patent CN108572226A discloses a method for measuring the content of ethanol in low-alcoholic beverage based on headspace gas chromatography, the Relative Standard Deviation (RSD) is 0.62%, the recovery rate is 96% -100%, but the method is mainly used for measuring the ethanol in low-alcoholic beverage such as fruit wine, rice wine, beer, grape wine and the like. The research result of 'measuring the content of ethanol in vinegar' of plum brilliant clear (2009) and the like shows that the content of ethanol in vinegar is detected by an HSGC method, the RSD is 1.4-9.7%, and the recovery rate is 91.0-104.9%. Chinese patent CN110007011A discloses a method for detecting the content of ethanol in edible vegetable oil, which also utilizes an HSGC method to detect the content of ethanol, the RSD of the method is 0.930-2.46%, and the recovery rate is 94.3% -100.4%. At present, headspace gas chromatography is basically used for detecting the alcohol degree of non-alcoholic liquid. Because ethanol belongs to a moderate volatile substance, the defect of inaccurate detection result caused by incomplete ethanol volatilization in the detection process of the HSGC method exists, and the defects of large sample amount, more generated waste liquid, complex operation and the like exist.
The invention content is as follows:
in order to solve the technical problems, the invention provides a method for detecting the alcohol degree of non-alcoholic liquid, which utilizes high performance liquid chromatography to detect the alcohol degree of the non-alcoholic liquid, and has the advantages of small sample amount, less generated waste liquid, simple and rapid operation and more accurate detection result.
The invention aims to provide a method for detecting the alcohol degree of non-alcoholic liquid.
The invention provides a method for detecting the alcohol degree of non-alcoholic liquid, which comprises the following steps:
s1, preparation of a solution: (1) ethanol standard solution: preparing 0.1%, 0.2%, 0.5%, 1%, 2%, 5% and 10% ethanol solution by volume percentage with absolute ethanol and double distilled water at 20 ℃;
(2) preparation of mobile phase solution: preparing a mobile phase solution with the mass percent of 2-4:1:95-97 by using acetone, sodium chloride and double distilled water;
s2, establishing a standard curve: performing reversed-phase high performance liquid chromatography on the ethanol standard solution prepared in 5 mu l S1, and drawing a standard curve by taking a peak area as a vertical coordinate and taking an alcoholicity as a horizontal coordinate;
s3 detection of sample alcoholicity: filtering a sample to be detected by using a filter membrane, taking 5 mu l of the filtered sample to be detected to perform reversed-phase high performance liquid chromatography determination, and calculating the alcoholicity of the sample to be detected according to a standard curve drawn by S2;
the conditions of the reversed phase liquid chromatography determination are as follows: the mobile phase is the mobile phase solution prepared in S1; the flow rate is 0.7-1.0 mL/min; the detection wavelength is 233 nm; the column temperature is 28-32 ℃.
Preferably, the preparation of the mobile phase solution comprises the following steps: acetone, sodium chloride and double distilled water are used for preparing a mobile phase solution with the mass percentage of 3:1: 96.
Preferably, the flow rate is 0.8 mL/min.
Preferably, the column temperature is 30 ℃.
Preferably, the filter described in S3 is a 0.22 μm filter.
Specifically, the method for detecting the alcohol degree of the non-alcoholic liquid comprises the following steps:
s1, preparation of a solution: (1) ethanol standard solution: accurately weighing absolute ethyl alcohol and double distilled water with constant temperature of 20 ℃ to prepare 0.1%, 0.2%, 0.5%, 1%, 2%, 5% and 10% of ethanol solution with alcohol degrees of 0.1, 0.2, 0.5, 1, 2, 5 and 10 degrees respectively;
(2) preparation of mobile phase solution: preparing a mobile phase solution with the mass percentage of 2-4:1:95-97 by using chromatographic pure acetone, sodium chloride and double distilled water at room temperature;
s2, establishing a standard curve: sampling and detecting an ethanol standard solution prepared in 5 mu l S1, wherein the mobile phase is the mobile phase solution prepared in S1, the flow rate is 0.7-1.0mL/min, the detection wavelength is 233nm, the column temperature is 28-32 ℃, performing reversed phase high performance liquid chromatography, and drawing a standard curve by taking the peak area as the ordinate and the alcoholicity as the abscissa;
s3 detection of sample alcoholicity: filtering a sample to be detected by a filter membrane of 0.22 mu m, taking 5 mu l of the filtered sample to be detected, loading and detecting, wherein the mobile phase is the mobile phase solution prepared in S1, the flow rate is 0.7-1.0mL/min, the detection wavelength is 233nm, the column temperature is 28-32 ℃, carrying out reversed phase high performance liquid chromatography determination, and calculating the alcohol degree of the sample to be detected according to a standard curve drawn by S2.
The invention has the beneficial effects that:
the invention provides a method for detecting the alcohol degree of non-alcoholic liquid, which utilizes a high performance liquid chromatography to detect the alcohol degree of the non-alcoholic liquid, wherein the detection limit of the method is 0.1 degree, the detection linear range is 0.1-10 degrees, the linearity is good, the detection result is accurate, the Relative Standard Deviation (RSD) is 0.36-2.33%, the recovery rate is 96.1-103.7%, the used sample amount is small, the generated waste liquid is small, and the operation is simple and rapid.
Detailed Description
In order to make the technical means, the original characteristics, the achieved purposes and the effects of the invention easily understood, the invention is further explained with the following embodiments, but the following embodiments are only the preferred embodiments of the invention, and not all embodiments. Based on the embodiments in the implementation, other embodiments obtained by those skilled in the art without any creative efforts belong to the protection scope of the present invention.
The experimental procedures in the following examples are conventional ones unless otherwise specified, and the drugs, reagents and the like used in the following examples are commercially available, and acetone and ethanol used therein are chromatographic grade reagents.
The instrument used in the invention: LC-20AD type high performance liquid chromatograph (Shimadzu, Japan) equipped with Diamonsil reverse phase C18Chromatography column (150 mm × 4.6.6 mm, 5 μm, Dikma).
Example 1
A method for detecting the alcohol degree of non-alcoholic liquid comprises the following steps:
s1, preparation of a solution: (1) ethanol standard solution: accurately weighing absolute ethyl alcohol and double distilled water with constant temperature of 20 ℃ to prepare 0.1%, 0.2%, 0.5%, 1%, 2%, 5% and 10% of ethanol solution with alcohol degrees of 0.1, 0.2, 0.5, 1, 2, 5 and 10 degrees respectively;
(2) preparation of mobile phase solution: preparing a mobile phase solution with the mass percent of 2:1: 97 by using chromatographic pure acetone, sodium chloride and double distilled water at room temperature;
s2, establishing a standard curve: sampling and detecting an ethanol standard solution prepared in 5 mu l S1, wherein the mobile phase is the mobile phase solution prepared in S1, the flow rate is 0.7mL/min, the detection wavelength is 233nm, the column temperature is 28 ℃, performing reversed phase high performance liquid chromatography, and drawing a standard curve by taking the peak area as the ordinate and the alcoholicity as the abscissa;
s3, detecting the alcohol degree of the vinegar sample: filtering the sample with 0.22 μm filter membrane, sampling 5 μ l of filtered vinegar sample, detecting, wherein the mobile phase is the mobile phase solution prepared in S1, the flow rate is 0.7mL/min, the detection wavelength is 233nm, the column temperature is 28 deg.C, performing reversed-phase high performance liquid chromatography, and calculating the alcoholicity of the sample to be detected according to the standard curve drawn in S2.
Example 2
A method for detecting the alcohol degree of non-alcoholic liquid comprises the following steps:
s1, preparation of a solution: (1) ethanol standard solution: accurately weighing absolute ethyl alcohol and double distilled water with constant temperature of 20 ℃ to prepare 0.1%, 0.2%, 0.5%, 1%, 2%, 5% and 10% of ethanol solution with alcohol degrees of 0.1, 0.2, 0.5, 1, 2, 5 and 10 degrees respectively;
(2) preparation of mobile phase solution: preparing a mobile phase solution with the mass percent of 3:1:96 by using chromatographic pure acetone, sodium chloride and double distilled water at room temperature;
s2, establishing a standard curve: sampling and detecting an ethanol standard solution prepared in 5 mu l S1, wherein the mobile phase is the mobile phase solution prepared in S1, the flow rate is 0.8mL/min, the detection wavelength is 233nm, the column temperature is 30 ℃, performing reversed-phase high performance liquid chromatography, and drawing a standard curve by taking the peak area as the ordinate and the alcoholicity as the abscissa;
s3, detecting the alcohol degree of the vinegar sample: filtering vinegar with 0.22 μm filter membrane, sampling 5 μ l of filtered vinegar, detecting, wherein the mobile phase is the mobile phase solution prepared in S1, the flow rate is 0.8mL/min, the detection wavelength is 233nm, the column temperature is 30 deg.C, performing reversed-phase high performance liquid chromatography, and calculating the alcohol degree of the sample to be detected according to the standard curve drawn by S2.
Example 3
A method for detecting the alcohol degree of non-alcoholic liquid comprises the following steps:
s1, preparation of a solution: (1) ethanol standard solution: accurately weighing absolute ethyl alcohol and double distilled water with constant temperature of 20 ℃ to prepare 0.1%, 0.2%, 0.5%, 1%, 2%, 5% and 10% of ethanol solution with alcohol degrees of 0.1, 0.2, 0.5, 1, 2, 5 and 10 degrees respectively;
(2) preparation of mobile phase solution: preparing a mobile phase solution with the mass percent of 4:1:95 by using chromatographic pure acetone, sodium chloride and double distilled water at room temperature;
s2, establishing a standard curve: sampling and detecting an ethanol standard solution prepared in 5 mu l S1, wherein the mobile phase is the mobile phase solution prepared in S1, the flow rate is 1.0mL/min, the detection wavelength is 233nm, the column temperature is 32 ℃, performing reversed-phase high performance liquid chromatography, and drawing a standard curve by taking the peak area as the ordinate and the alcoholicity as the abscissa;
s3, detecting the alcohol degree of the vinegar sample: filtering vinegar with 0.22 μm filter membrane, sampling 5 μ l of filtered vinegar, detecting, wherein the mobile phase is the mobile phase solution prepared in S1, the flow rate is 1.0mL/min, the detection wavelength is 233nm, the column temperature is 32 deg.C, performing reversed-phase high performance liquid chromatography, and calculating the alcoholicity of the sample to be detected according to the standard curve drawn in S2.
Comparative example 1
A method for measuring the alcohol content of a non-alcoholic liquid, which is different from example 2 only in that a mobile phase solution is used which is prepared by: at room temperature, a mobile phase solution with the mass percent of 3:97 is prepared by using chromatographic pure acetone and double distilled water.
Comparative example 2
A method for measuring the degree of alcohol in a non-alcoholic liquid, which is different from example 2 only in that the flow rate of a mobile phase in a reversed-phase high-performance liquid chromatography measurement is 1.2 mL/min.
Comparative example 3
A method for measuring the degree of alcohol in a non-alcoholic liquid, which is different from example 2 only in that the column temperature in the reversed-phase high-performance liquid chromatography measurement is 35 ℃.
The non-alcoholic liquids described in examples 1 to 3 and comparative examples 1 to 3 were evaluated for the effect of the alcohol content measuring method, and the results are shown in table 1.
As can be seen from the results in Table 1, the method for detecting the alcohol content of the non-alcoholic liquid provided by the invention has the advantages of good linearity, accurate detection result and detection minimum limit of 0.1 degree; r of the plotted Standard Curve20.9996-0.999; the linear range is 0.1-10 degrees; relative Standard Deviation (RSD) of 0.36% to 2.29%; the recovery rate is 96.1-103.2%. In particular, the detection method described in embodiment 2 of the present inventionThe method has the best effect, and the standard curve is y = 1.0017x + 0.1911.
In addition, the alcohol degree of the non-alcoholic liquid is detected by using soy sauce, vegetable oil, non-alcoholic beverages and the like as samples to be detected and using the alcohol degree detection method of the non-alcoholic liquid provided by the invention, and the detection result shows that R of a drawn standard curve20.9996-0.998; the linear range is 0.1-10 degrees; relative Standard Deviation (RSD) 0.84% -2.33%; the recovery rate is 96.3-103.7%.
The foregoing is a preferred embodiment of the present invention, and is not intended to limit the invention in any way, so that any simple modification and equivalent changes made to the above embodiment without departing from the technical spirit of the present invention should be considered as the protection scope of the present invention.
Claims (5)
1. A method for detecting the alcohol degree of non-alcoholic liquid is characterized by comprising the following steps:
s1, preparation of a solution: (1) ethanol standard solution: preparing 0.1%, 0.2%, 0.5%, 1%, 2%, 5% and 10% ethanol solution by volume percentage with absolute ethanol and double distilled water at 20 ℃;
(2) preparation of mobile phase solution: preparing a mobile phase solution with the mass percent of 2-4:1:95-97 by using acetone, sodium chloride and double distilled water;
s2, establishing a standard curve: performing reversed-phase high performance liquid chromatography on the ethanol standard solution prepared in 5 mu l S1, and drawing a standard curve by taking a peak area as a vertical coordinate and taking an alcoholicity as a horizontal coordinate;
s3 detection of sample alcoholicity: filtering a sample to be detected by using a filter membrane, taking 5 mu l of the filtered sample to be detected to perform reversed-phase high performance liquid chromatography determination, and calculating the alcoholicity of the sample to be detected according to a standard curve drawn by S2;
the conditions of the reversed phase liquid chromatography determination are as follows: the mobile phase is the mobile phase solution prepared in S1; the flow rate is 0.7-1.0 mL/min; the detection wavelength is 233 nm; the column temperature is 28-32 ℃.
2. The method for detecting alcohol content according to claim 1, wherein the mobile phase solution is prepared by: acetone, sodium chloride and double distilled water are used for preparing a mobile phase solution with the mass percentage of 3:1: 96.
3. The method for detecting alcohol degree according to claim 1, wherein the flow rate is 0.8 mL/min.
4. The method for detecting alcohol degree according to claim 1, wherein the column temperature is 30 ℃.
5. The method for detecting alcohol content according to claim 1, wherein the filter of S3 is a 0.22 μm filter.
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Inventor after: Ren Dahong Inventor after: Lin Lizhao Inventor after: Ye Yuemin Inventor after: He Naka Inventor before: Ren Dahong |