CN104422708A - Method for identifying quality of yellow rice wine by using low-field nuclear magnetic resonance - Google Patents
Method for identifying quality of yellow rice wine by using low-field nuclear magnetic resonance Download PDFInfo
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Abstract
A method for identifying the quality of yellow rice wine by using low-field nuclear magnetic resonance comprises the following steps: a, preparing a set of adulteration yellow rice wine samples with different adulteration materials and different weight percentages of the adulteration materials, respectively carrying out low-field nuclear magnetic resonance detection, and thus obtaining test data of all the adulteration yellow rice wine samples; and carrying out low-field nuclear magnetic resonance detection on genuine yellow rice wine, to obtain test data of the genuine yellow rice wine, and establishing a yellow rice wine quality database; and b, carrying out low-field nuclear magnetic resonance detection of to-be-detected yellow rice wine, to obtain test data of the to-be-detected yellow rice wine, carrying out analysis comparison of the test data with the test data in the yellow rice wine quality database, and determining whether the to-be-tested yellow rice wine is adulteration yellow rice wine. The adopted method is fast in identification speed, accurate in identification results, good in repeatability, and good in stability, does not need to invade to the interior of the samples during identification of the samples, and has no pollution and no damage to the samples.
Description
Technical field
The present invention relates to a kind of food detection method, particularly a kind of method utilizing low-field nuclear magnetic resonance to differentiate yellow rice wine quality.
Background technology
Yellow rice wine is that the grain brewageed for raw material with rice, milled glutinous broomcorn millet spills, and general alcohol content is 14% ~ 20%, belongs to low brewed wine.Yellow rice wine is the gorgeous traditional culture legacy of the Chinese nation, and it is with a long history, with beer, grape wine be called that ancient wine is brewageed greatly in the world three.Yellow rice wine is nutritious, is a kind ofly to integrate the brewed wine enjoyed and keep healthy, and can be used for has culinary art, has the effects such as medicinal concurrently, meets the trend of world's alcoholic drink development, is thus classified as the alcoholic drink given special assistance to and develop by country.
But, while yellow rice wine industry is flourish, also occur that a lot of illegal retailer palms off the famous brand name of famous-brand and high-quality enterprise or shoddy phenomenon; What is more, and some lawless persons are adulterated to yellow rice wine, doping (water mixing, mix ethanol, mix methyl alcohol etc.), after carrying out blending process, sell, therefrom reap staggering profits with knockout price.These lawbreaking activitiess are serious impact market both, again reduces the trusting degree of consumer to yellow rice wine product, have impact on the sound development of rice wine industry.For the counterfeit and shoddy goods that market exists, generally only rely on subjective appreciation, the method affects comparatively large by experience and subjective factor, accuracy is difficult to ensure.Therefore, how quick, accurate, real-time mensuration is carried out to yellow rice wine quality, to reduce costs, improve the quality of products, increase economic benefit, expand brand advantage all have great importance.
Low-field nuclear magnetic resonance technology is mainly analyzed the longitudinal relaxation time (T1) of detected object, T2 (T2), coefficient of diffusion and CPMG (Carr-Purcell-Meiboom-Gill) echo data, utilize low-field nuclear magnetic resonance technology can the component such as moisture, grease and alcohol in instrument effectively, in yellow rice wine, water O-H base and ethanol C-H base be the physical basis producing resonance relaxation spectrum.Compared with traditional detection technique, low-field nuclear magnetic resonance technology (LF-NMR) detect sample fast, harmless, in real time, without the need to any chemical reagent, and cheap (market price is about 1/3 of above-mentioned instrument).Low-field nuclear magnetic resonance technology is the pseudo-new technology of one very potential yellow rice wine quality Quick Measuring.。
In sum, research is a kind of can simple and quick, detection technique method accurately to the adulterated doping of yellow rice wine, and tool is of great significance.
Summary of the invention
Object of the present invention, is just to solve the problem, and provides a kind of method utilizing low-field nuclear magnetic resonance to differentiate yellow rice wine quality.
The object of the present invention is achieved like this: a kind of method utilizing low-field nuclear magnetic resonance to differentiate yellow rice wine quality, comprises the following steps:
The foundation in a, yellow rice wine qualitative data storehouse
Prepare a set of difference mix pseudo-material and different mix pseudo-substance weight percentage composition mix pseudo-yellow rice wine sample, carry out low-field nuclear magnetic resonance detection respectively, respectively mixed the test data of pseudo-yellow rice wine sample; And low-field nuclear magnetic resonance detection is carried out to certified products yellow rice wine, obtain the test data of certified products yellow rice wine; Test data and yellow rice wine quality are set up correlativity, sets up yellow rice wine qualitative data storehouse;
The quartile length of b, yellow rice wine to be measured
Low-field nuclear magnetic resonance detection is carried out to yellow rice wine to be measured, obtain the test data of yellow rice wine to be measured, test data in test data and yellow rice wine qualitative data storehouse is carried out com-parison and analysis, determine that whether yellow rice wine to be measured is for mixing pseudo-yellow rice wine, mix pseudo-yellow rice wine in this way, determine to mix the kind of pseudo-material further and mix pseudo-substance weight percentage composition.
Mixing pseudo-material described in step a is one in water, ethanol, methyl alcohol, described in mix pseudo-substance weight percentage composition be 1-9% and 10-90%, within the scope of 1-9%, percentage composition gradient is 1%, and within the scope of 10-90%, percentage composition gradient is 5%.
Described test data comprises the initial time T of first peak
21, the second peak initial time T
22, the 3rd peak initial time T
23, first peak peak area percent S
21, the second peak peak area percent S
22, the 3rd peak peak area percent S
23and single component relaxation time T
2W.
Described when to mix pseudo-material be water, it is 4% that lowest detection mixes pseudo-substance weight percentage composition; Described when to mix pseudo-material be ethanol, it is 3% that lowest detection mixes pseudo-substance weight percentage composition; Described when to mix pseudo-material be methyl alcohol, it is 4% that lowest detection mixes pseudo-substance weight percentage composition.
The present invention has the following advantages and feature:
The method has the following advantages:
1, differentiate that speed is fast, identification result is accurate;
2, reproducible, good stability;
Do not need to invade sample interior when 3, differentiating sample, sample is not produced and pollutes and destroy;
4, the scene being easy to realize Yellow Wine quality is differentiated, for the testing of each Yellow Wine product quality provides authentic communication, in the quality control and evaluation of yellow rice wine, has larger application potential.
Accompanying drawing explanation
Fig. 1 is the T of pure material (yellow rice wine, water, methyl alcohol, ethanol)
2relaxation collection of illustrative plates;
Fig. 2 is for mixing the T of pseudo-water (0%--30%)
2relaxation collection of illustrative plates;
Fig. 3 is peak initial time and mixes the pseudo-correlativity measuring (0%--30%);
Fig. 4 is peak area percent and mixes the pseudo-correlativity measuring (0%--30%).
Embodiment
The method of yellow rice wine quality is to utilize low-field nuclear magnetic resonance to differentiate, first determine the instrument parameter (mainly correlation parameter being detected to the cpmg sequence row of instrument) that low-field nuclear magnetic resonance instrument is applicable to, guarantee that the free induction index die-away curve decay that LF-NMR relaxation detects is complete.
After instrument parameter is determined, this instrument is utilized to set up a yellow rice wine qualitative data storehouse, specific practice is: prepare a set of difference mix pseudo-material and different mix pseudo-substance weight percentage composition mix pseudo-yellow rice wine sample, carry out low-field nuclear magnetic resonance detection respectively, respectively mixed the test data of pseudo-yellow rice wine sample; And low-field nuclear magnetic resonance detection is carried out to certified products yellow rice wine, obtain the test data of certified products yellow rice wine; Test data and yellow rice wine quality are set up correlativity, sets up yellow rice wine qualitative data storehouse.Above-mentioned test data comprises the initial time T of first peak
21, the second peak initial time T
22, the 3rd peak initial time T
23, first peak peak area percent S
21, the second peak peak area percent S
22, the 3rd peak peak area percent S
23and single component relaxation time T
2W.The pseudo-material of mixing related to is one in water, ethanol, methyl alcohol, and mix pseudo-substance weight percentage composition and get 1-9% and 10-90%, within the scope of 1-9%, percentage composition gradient is 1%, and within the scope of 10-90%, percentage composition gradient is 5%.
After having had yellow rice wine qualitative data storehouse, the quartile length that can carry out yellow rice wine to be measured, specific practice is:
Low-field nuclear magnetic resonance detection is carried out to yellow rice wine to be measured, obtain the test data of yellow rice wine to be measured, test data in test data and yellow rice wine qualitative data storehouse is carried out com-parison and analysis, determine that whether yellow rice wine to be measured is for mixing pseudo-yellow rice wine, mix pseudo-yellow rice wine in this way, determine to mix the kind of pseudo-material further and mix pseudo-substance weight percentage composition.
After testing, when mixing pseudo-material and being water, it is 4% that lowest detection mixes pseudo-substance weight percentage composition; When mixing pseudo-material and being ethanol, it is 3% that lowest detection mixes pseudo-substance weight percentage composition; When mixing pseudo-material and being methyl alcohol, it is 4% that lowest detection mixes pseudo-substance weight percentage composition.
Adopt method of the present invention, the speed of test is fast, consuming time short, once tests and substantially can complete within 4 minutes.
Fig. 1 is the T of pure material (yellow rice wine, water, methyl alcohol, ethanol)
2relaxation collection of illustrative plates, as shown in Figure 1, different pure materials can separate circle of good definition in collection of illustrative plates; The number at its peak, peak initial time, and the area ratio at peak is all different.Fig. 2 is for mixing the T of pseudo-water (0%--30%)
2relaxation collection of illustrative plates, as can be seen from Figure 2, along with the increase of mixing pseudo-massfraction, there is the trend that moves to right clearly at two peaks; Peak initial time pseudo-measures the correlativity of (0%--30%) as shown in Figure 3 with mixing, as shown in Figure 3, along with the increase of mixing pseudo-massfraction, and peak initial time T
21, T
22become large gradually, consistent with the relaxation collection of illustrative plates gained trend that moves to right; Analyze peak area percent and mix the pseudo-correlativity measuring (0%--30%), result as shown in Figure 4, as seen from Figure 4, along with the increase of mixing pseudo-quality mark, first peak area percent S
21increase gradually, and second peak area percent S
22reduce gradually; Mix pseudo-amount 40%-90% rule the same.
In summary, when mixing pseudo-material and being the water of Different Weight percentage composition, at T
2can obviously distinguish in relaxation collection of illustrative plates: increase along with mixing pseudo-quality mark, first peak and second peak move to right along with mixing the increase of pseudo-massfraction; Peak initial time T
21, T
22become large gradually, the peak area percent S at first peak
21increase gradually, the area percentage S at second peak
22in reducing trend gradually.Therefore by detecting the peak initial time of sample, peak area ratio infers whether sample is mixed puppet and had water and mix the weight percentage of pseudo-water.
Other pseudo-material (methyl alcohol, ethanol) of mixing mixes in yellow rice wine, also by analyzing the variation tendency of the area ratio of its peak initial time and peak etc., judges yellow rice wine quality.
Claims (4)
1. utilize low-field nuclear magnetic resonance to differentiate a method for yellow rice wine quality, it is characterized in that, comprise the following steps:
The foundation in a, yellow rice wine qualitative data storehouse
Prepare a set of difference mix pseudo-material and different mix pseudo-substance weight percentage composition mix pseudo-yellow rice wine sample, carry out low-field nuclear magnetic resonance detection respectively, respectively mixed the test data of pseudo-yellow rice wine sample; And low-field nuclear magnetic resonance detection is carried out to certified products yellow rice wine, obtain the test data of certified products yellow rice wine; Test data and yellow rice wine quality are set up correlativity, sets up yellow rice wine qualitative data storehouse;
The quartile length of b, yellow rice wine to be measured
Low-field nuclear magnetic resonance detection is carried out to yellow rice wine to be measured, obtain the test data of yellow rice wine to be measured, test data in test data and yellow rice wine qualitative data storehouse is carried out com-parison and analysis, determine that whether yellow rice wine to be measured is for mixing pseudo-yellow rice wine, mix pseudo-yellow rice wine in this way, determine to mix the kind of pseudo-material further and mix pseudo-substance weight percentage composition.
2. the method utilizing low-field nuclear magnetic resonance to differentiate yellow rice wine quality according to claim 1, it is characterized in that: mixing pseudo-material described in step a is one in water, ethanol, methyl alcohol, it is described that to mix pseudo-substance weight percentage composition be 1-9% and 10-90%, within the scope of 1-9%, percentage composition gradient is 1%, within the scope of 10-90%, percentage composition gradient is 5%.
3. the method utilizing low-field nuclear magnetic resonance to differentiate yellow rice wine quality according to claim 1, is characterized in that: described test data comprises the initial time T of first peak
21, the second peak initial time T
22, the 3rd peak initial time T
23, first peak peak area percent S
21, the second peak peak area percent S
22, the 3rd peak peak area percent S
23and single component relaxation time T
2W.
4. the method utilizing low-field nuclear magnetic resonance to differentiate yellow rice wine quality according to claim 1, is characterized in that: described in when to mix pseudo-material be water, it is 4% that lowest detection mixes pseudo-substance weight percentage composition; Described when to mix pseudo-material be ethanol, it is 3% that lowest detection mixes pseudo-substance weight percentage composition; Described when to mix pseudo-material be methyl alcohol, it is 4% that lowest detection mixes pseudo-substance weight percentage composition.
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Cited By (2)
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| CN106950243A (en) * | 2017-03-31 | 2017-07-14 | 安徽农业大学 | A kind of method for detecting aged rice |
| CN110849779A (en) * | 2019-12-11 | 2020-02-28 | 湖北省农业科学院农产品加工与核农技术研究所 | Method for rapidly predicting salt content in aquatic product based on spectral imaging technology |
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| CN102749349A (en) * | 2012-06-20 | 2012-10-24 | 山东大学 | Method for testing authenticity of donkey-hide gelatin |
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2013
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| CN102375000A (en) * | 2011-09-19 | 2012-03-14 | 海南椰岛（集团）股份有限公司 | Method for testing coconut island deer tortoise wine based on HNMR (hydrogen-nuclear magnetic resonance)-pattern recognition technique |
| CN102749349A (en) * | 2012-06-20 | 2012-10-24 | 山东大学 | Method for testing authenticity of donkey-hide gelatin |
| CN103344661A (en) * | 2013-07-05 | 2013-10-09 | 上海适济生物科技有限公司 | Method for identifying adulterated oil and gutter oil through hydrogen nuclear magnetic resonance method |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106950243A (en) * | 2017-03-31 | 2017-07-14 | 安徽农业大学 | A kind of method for detecting aged rice |
| CN110849779A (en) * | 2019-12-11 | 2020-02-28 | 湖北省农业科学院农产品加工与核农技术研究所 | Method for rapidly predicting salt content in aquatic product based on spectral imaging technology |
| CN110849779B (en) * | 2019-12-11 | 2022-07-01 | 湖北省农业科学院农产品加工与核农技术研究所 | Method for rapidly predicting salt content in aquatic product based on spectral imaging technology |
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