CN104007191A - Method for determining content of tetramethylpyrazine in white liquor - Google Patents
Method for determining content of tetramethylpyrazine in white liquor Download PDFInfo
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- CN104007191A CN104007191A CN201410166445.7A CN201410166445A CN104007191A CN 104007191 A CN104007191 A CN 104007191A CN 201410166445 A CN201410166445 A CN 201410166445A CN 104007191 A CN104007191 A CN 104007191A
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Abstract
The invention discloses a method for determining the content of tetramethylpyrazine in white liquor. The method comprises the following steps: setting relevant chromatographic detection conditions on a liquid chromatograph, introducing and determining prepared tetramethylpyrazine series standard solutions with different concentrations under the set chromatographic detection conditions, making a tetramethylpyrazine standard curve by treating the tetramethylpyrazine concentration of the introduced standard solutions as an ordinate and the determined peak area as an abscissa, introducing and determining a liquor sample to be determined under same chromatographic detection conditions, and outputting tetramethylpyrazine content data, that is, loading in the tetramethylpyrazine standard curve. A verification experiment result shows that the minimum quantitative limit of the method is 0.09mg/L, the linear correlation coefficient is greater than 0.999, the tetramethylpyrazine recovery rate is 94.67-100.33%, and the relative standard deviation is below 3.5%, so the method has the advantages of feasibility, reliability, high accuracy, simple and fast operation, low requirements on instrument conditions, and convenient popularization application.
Description
Technical field
The present invention relates to a kind of method of measuring Tetramethylpyrazine content in white wine, belong to Liquor Analysis detection technique field.
Technical background
In recent years, along with social progress and expanding economy, people are more and more higher to the requirement of quality of life.White wine, as Chinese traditional zymotic product, is a part indispensable on common people's dining table already.Excavate the bioactive ingredients (the healthy functions factor) in China white wine, science guide consumption person health is drunk, and promotes white wine industry to promote, and has been the problem of Chinese scholars broad research.Other countries' Spirit relatively, the flavor and fragrance substance content in China white wine can be rated as the first in the world.Wherein pyrazine compounds, as important flavor and fragrance substance, is more and more subject to people's attention and pays close attention to.It has obtained scholar's generally approval in the industry as the healthy functions factor important in white wine.
Pyrazine compounds is the general name of a class containing Isosorbide-5-Nitrae-diazine female ring compound, is extensively present in nature and fermented food, has and is similar to the pleasant fragrance of frying nut, barbecue, and fragrance thoroughly loose property is good, and other fragrance is had and set off by contrast significantly and superposition.Tetramethylpyrazine, has another name called ligustrazine, is a kind of important pyrazine compound.It,, as the main active alkaloid composition of Chinese crude drug rhizome of chuanxiong rhizome, has special pharmacological action simultaneously.Research shows, Tetramethylpyrazine has hemangiectasis, change blood circulation, the functions such as (preventing the damage of alcohol to stomach lining and liver) of protecting liver.In Maotai-flavor, hold concurrently odor type and distilled spirit with sesame flavour, be rich in pyrazine class material, particularly Tetramethylpyrazine, it is mainly produced by microbial metabolism and Maillard reaction, is the health flavor components in China white wine, for " responsible drinking, good for health " provides foundation.
In recent years, mainly contain for the research of Tetramethylpyrazine detection method in white wine: the Xu Yan of Southern Yangtze University, model essay carry out liquid-liquid extraction for philosophy, head space micro-extraction detects the pyrazine compound in white wine in conjunction with GC-MS and solid-phase microextraction in conjunction with the method for gas chromatography; Yu Xiao etc. utilize improved Liebich acidization extraction to measure the pyrazine compound in white wine in conjunction with GS-MS; Wang Li etc. have set up with the pyrazine class material in gas chromatography-mass spectrum-ion scan coupling technique detection white wine; Ren Xuekun etc. utilize GC-External Standard method to detect the Tetramethylpyrazine in white wine.But the research that detects Tetramethylpyrazine in white wine based on liquid chromatography technology also still belongs to blank at present.
Summary of the invention
The object of the present invention is to provide the method for Tetramethylpyrazine content in a kind of feasible, reliable and mensuration white wine that accuracy is high.
Its technical scheme is: a kind of method of measuring Tetramethylpyrazine content in white wine, is characterized in that comprising the steps:
1) preparation Tetramethylpyrazine series standard solution: with the Tetramethylpyrazine standard solution of Tetramethylpyrazine and ethanol dilution preparation variable concentrations;
2) the chromatogram testing conditions of setting liquid chromatograph: mobile phase is Jia Chun ﹕ water (v/v)=35 ﹕ 65, flow velocity is 1mL/min, column temperature is 40 DEG C, chromatographic column is phenomenex Gemini5 μ C18110A (250 × 4.60mm), detection wavelength is 278nm, and sample size is 20 μ L;
3) draw Tetramethylpyrazine typical curve: under the chromatogram testing conditions of above-mentioned setting, after baseline is steady, successively the Tetramethylpyrazine standard solution of variable concentrations sample introduction after membrane filtration is measured, taking the concentration of the Tetramethylpyrazine standard solution of sample introduction as ordinate, the Tetramethylpyrazine peak area of measuring is horizontal ordinate, draws out Tetramethylpyrazine typical curve;
4) mensuration of Tetramethylpyrazine content in white wine: draw white wine wine sample to be measured, after membrane filtration to the sample bottle of liquid chromatograph, under the chromatogram testing conditions of above-mentioned setting, sample introduction is measured, in output wine sample, the content data of Tetramethylpyrazine, is carried in above-mentioned Tetramethylpyrazine typical curve.
Its beneficial effect is: liquid chromatography technology of the present invention is measured the method for Tetramethylpyrazine content in white wine, by adopting liquid phase chromatography to detect the recovery of Tetramethylpyrazine content in white wine wine sample, the verification experimental verification of precision and detectability, its quantitative limit is low to moderate 0.09mg/L, linearly dependent coefficient is greater than 0.999, the recovery of Tetramethylpyrazine is 94.67%～100.33%, relative standard deviation is below 3.5%, illustrate that the present invention adopts liquid chromatography technology, draw out Tetramethylpyrazine typical curve, again by white wine wine sample sample introduction to be measured being measured under the chromatogram testing conditions setting, thereby the method for Tetramethylpyrazine content in mensuration white wine, not only feasibility and good reliability, precision and accuracy are high, and simple and quick, be easy to grasp, instrument and equipment conditional request to distillery is not high, easy to utilize.
Brief description of the drawings
Fig. 1 is Tetramethylpyrazine standard specimen liquid chromatographic detection figure;
Fig. 2 is Tetramethylpyrazine canonical plotting.
Specific implementation method
Embodiment 1.Measure the method for Tetramethylpyrazine content in a surname's wine product
One, preparation Tetramethylpyrazine standard solution:
Tetramethylpyrazine is purchased from SIGMA company of the U.S..Take the Tetramethylpyrazine of 0.5g, be dissolved in the chromatographic grade ethanol of concentration 60%, and constant volume, the Tetramethylpyrazine standard specimen mother liquor of preparation 500mg/L.
By above-mentioned Tetramethylpyrazine standard specimen mother liquor doubling dilution, the Tetramethylpyrazine standard specimen solution (seeing Fig. 1) of preparation 5mg/L.
The Tetramethylpyrazine standard specimen solution that pipettes successively above-mentioned 1mL, 2mL, 4mL, 6mL, 8mL with transfer pipet is in 10mL volumetric flask, be settled to scale, be mixed with 0.5mg/L, 1.0mg/L, 2.0mg/L, 3.0mg/L, 4.0mg/L Tetramethylpyrazine standard solution, stand-by.
Two, set the chromatogram testing conditions of liquid chromatograph: adopt Agilent 1200 liquid chromatographs, set chromatogram testing conditions: mobile phase is Jia Chun ﹕ water (v/v)=35 ﹕ 65, flow velocity is 1mL/min, column temperature is 40 DEG C, chromatographic column is phenomenex Gemini5 μ C18110A (250 × 4.60mm), detection wavelength is 278nm, and sample size is 20 μ L.
Three, draw Tetramethylpyrazine typical curve: under the chromatogram testing conditions of above-mentioned setting, after baseline is steady, Tetramethylpyrazine standard solution to 0.5mg/L, 1.0mg/L, 2.0mg/L, 3.0mg/L, 4.0mg/L variable concentrations successively, after 0.22 μ m membrane filtration, sample introduction is measured, taking the concentration of sample introduction Tetramethylpyrazine standard solution as ordinate, the Tetramethylpyrazine peak area of measuring is horizontal ordinate, draws out Tetramethylpyrazine typical curve (seeing Fig. 2).Curvilinear equation: y=1E-05x+0.0015; Related coefficient: r=0.9996.
Four, the mensuration of Tetramethylpyrazine content in white wine: white wine wine sample to be measured is provided by Anhui Xuan Jiu group.Draw 3mL wine sample to be measured, after 0.22 μ m membrane filtration to the sample bottle of liquid chromatograph, under the same chromatogram testing conditions of above-mentioned setting, sample introduction is measured, the content data of Tetramethylpyrazine in output wine sample, be carried in above-mentioned Tetramethylpyrazine typical curve, the content of measuring Tetramethylpyrazine in this wine sample is 1.27mg/L.
Embodiment 2.Liquid phase chromatography detects the recovery, precision and the detectability test of Tetramethylpyrazine content in a surname's wine wine sample.
In the white wine wine sample of above-described embodiment 1, add respectively 0.5mg/L, 1.0mg/L, 2.0mg/L Tetramethylpyrazine standard solution, after membrane filtration to the sample bottle of liquid chromatograph, each test do three times parallel, order according to low concentration to high concentration, sample introduction successively, after wine sample gathers, starts post processor, loading method, Output rusults.Calculate the method and measure the recovery and the relative standard deviation (in table 1) of Tetramethylpyrazine.
The mensuration of the Tetramethylpyrazine recovery in table 1 wine sample
(n=3, the mg/L of unit)
Detection limit: baseline noise value is 0.03mg/L, the baseline noise value of 3 times is 0.09mg/L, the minimum detectability of the method is 0.09mg/L.
Claims (3)
1. measure a method for Tetramethylpyrazine content in white wine, it is characterized in that comprising the steps:
1) preparation Tetramethylpyrazine series standard solution: with the Tetramethylpyrazine standard solution of Tetramethylpyrazine and ethanol dilution preparation variable concentrations;
2) the chromatogram testing conditions of setting liquid chromatograph: mobile phase is Jia Chun ﹕ water (v/v)=35 ﹕ 65, flow velocity is 1mL/min, column temperature is 40 DEG C, chromatographic column is phenomenex Gemini5 μ C18110A (250 × 4.60mm), detection wavelength is 278nm, and sample size is 20 μ L;
3) draw Tetramethylpyrazine typical curve: under the chromatogram testing conditions of above-mentioned setting, after baseline is steady, successively the Tetramethylpyrazine standard solution of variable concentrations sample introduction after membrane filtration is measured, taking the concentration of the Tetramethylpyrazine standard solution of sample introduction as ordinate, the Tetramethylpyrazine peak area of measuring is horizontal ordinate, draws out Tetramethylpyrazine typical curve;
4) mensuration of Tetramethylpyrazine content in white wine: draw white wine wine sample to be measured, after membrane filtration to the sample bottle of liquid chromatograph, under the chromatogram testing conditions of above-mentioned setting, sample introduction is measured, the content data of the Tetramethylpyrazine in output wine sample, is carried in above-mentioned Tetramethylpyrazine typical curve.
2. a kind of method of measuring Tetramethylpyrazine content in white wine according to claim 1, is characterized in that: described ethanol is the chromatographic grade ethanol of concentration 60%.
3. a kind of method of measuring Tetramethylpyrazine content in white wine according to claim 1, is characterized in that: the Tetramethylpyrazine standard solution of described variable concentrations is 0.5mg/L, 1.0mg/L, 2.0mg/L, 3.0mg/L, 4.0mg/L Tetramethylpyrazine standard solution.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105158396A (en) * | 2015-09-18 | 2015-12-16 | 西安科技大学 | Rapid detection method for tetramethylpyrazine |
| CN104977370B (en) * | 2015-02-03 | 2016-09-07 | 江苏今世缘酒业股份有限公司 | A kind of LC-MS quickly detects the method for Pyrazine material in white wine |
| CN105929082A (en) * | 2016-07-14 | 2016-09-07 | 云南中烟工业有限责任公司 | Method for separating and determining pyrazine substances and pyridine substances in saliva |
| CN109917033A (en) * | 2019-03-15 | 2019-06-21 | 贵州茅台酒股份有限公司 | A kind of method of hydroxypyrazine class compound in measurement Maotai-flavor liquor |
| CN113174442A (en) * | 2021-04-28 | 2021-07-27 | 四川大学 | Quantitative detection method for tetramethylpyrazine synthesis key gene expression in Daqu |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104977370B (en) * | 2015-02-03 | 2016-09-07 | 江苏今世缘酒业股份有限公司 | A kind of LC-MS quickly detects the method for Pyrazine material in white wine |
| CN105158396A (en) * | 2015-09-18 | 2015-12-16 | 西安科技大学 | Rapid detection method for tetramethylpyrazine |
| CN105929082A (en) * | 2016-07-14 | 2016-09-07 | 云南中烟工业有限责任公司 | Method for separating and determining pyrazine substances and pyridine substances in saliva |
| CN109917033A (en) * | 2019-03-15 | 2019-06-21 | 贵州茅台酒股份有限公司 | A kind of method of hydroxypyrazine class compound in measurement Maotai-flavor liquor |
| CN109917033B (en) * | 2019-03-15 | 2021-12-14 | 贵州茅台酒股份有限公司 | Method for determining hydroxypyrazine compounds in Maotai-flavor liquor |
| CN113174442A (en) * | 2021-04-28 | 2021-07-27 | 四川大学 | Quantitative detection method for tetramethylpyrazine synthesis key gene expression in Daqu |
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Application publication date: 20140827 |