CN108226367A - The detection method of glycerine in a kind of beer - Google Patents
The detection method of glycerine in a kind of beer Download PDFInfo
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- CN108226367A CN108226367A CN201711473484.1A CN201711473484A CN108226367A CN 108226367 A CN108226367 A CN 108226367A CN 201711473484 A CN201711473484 A CN 201711473484A CN 108226367 A CN108226367 A CN 108226367A
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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Abstract
The present invention proposes a kind of detection method of glycerine in beer, belongs to beer detection technique field, and this method safety and environmental protection, accuracy and reproducibility are all preferable, effective detection means in can regulating and controlling as Beer Brewage.The technical solution includes standard working solution preparation, sample solution preparation, liquid-phase chromatographic analysis and Specification Curve of Increasing and result calculates four steps.The present invention can be applied in beer in the detection of glycerine.
Description
Technical field
The invention belongs to a kind of detection methods of glycerine in beer detection technique field more particularly to beer.
Background technology
Content of the glycerine in beer is only second to ethyl alcohol and carbon dioxide, is the important flavor substances for forming beer wine body
Matter, itself has sweet taste and toughness.Glycerine can also act synergistically with other flavor substances, offset the bad mouths such as astringent taste
Sense assigns beer full, mellow, coordination feature.In addition, glycerine, which also has, adjusts yeast cells osmotic pressure, cell is maintained
The important function of the redox equilibrium of matter.Based on its significance to beer flavor and fermentation process of glycerine, having very much must
It is detected.
These methods such as the detection for the glycerine in beer, densimetry, titration, capillary gas chromatography
Suitable for the inspection to glycerine sterling, but it is harsh to the purity requirement of sample, such as the sample that capillary gas chromatography was applicable in
Product purity cannot be below 95%, therefore, it is very big detect difficulty.Glycerine belongs to not volatile compound, is more suitable for adopting
It is detected with liquid chromatogram.But in the existing method using liquid chromatographic detection glycerine, mostly using nh 2 column method, stream
Dynamic phase uses acetonitrile, and toxicity is larger, is unfavorable for environmental protection and testing cost is high.
Invention content
The present invention provides a kind of detection method of glycerine in beer, this method safety and environmental protection, accuracy and reproducibility
All preferably, effective detection means in can regulating and controlling as Beer Brewage.
In order to achieve the above object, the present invention provides a kind of detection method of glycerine in beer, include the following steps：
1) prepared by standard working solution：
The glycerine standard working solution with 8 grades of concentration gradients is prepared respectively, and concentration range is：0.58g/L-
41.81g/L by prepared standard working solution by 0.22 μm of membrane filtration, is dispensed in 2ml centrifuge tubes, freezen protective, detection
Before be restored to room temperature and shake up；
2) prepared by sample solution：
Beer fermentation liquid is poured into the funnel equipped with fast grade filter paper, collects filtrate, and filtrate is passed through into 0.22 μm of film mistake
Filter；Alternatively, after finished beer is deaerated, by 0.22 μm of membrane filtration；
3) liquid-phase chromatographic analysis：
Hydrogen ion type gel chromatographic columns are equipped with to made testing sample solution and standard working solution using liquid chromatograph
It is analyzed, obtains related chromatogram；
4) Specification Curve of Increasing and result calculate.
Preferably, the hydrogen ion type gel chromatographic columns are 300 × 7.8mm of Rezex ROA.
Preferably, the liquid phase chromatogram condition of glycerine is：Detector temperature：40℃；Column oven temperature：60℃；Flow velocity：
0.6ml/min；Run time：25 minutes；Mobile phase：85% phosphoric acid of 0.36mL is added in ultra-pure water, is settled to 1L, is passed through
0.22 μm of membrane filtration, ultrasound degassing 5 minutes.
Preferably, the preparation method of standard working solution：Glycerine standard items are accurately weighed with electronic balance
2.0905g adds in ultra-pure water stirring and dissolving, is settled to 25mL, obtains the glycerin solution of a concentration of 83.62g/L.
Compared with prior art, the advantages and positive effects of the present invention are：
1st, this method is detected made testing sample solution using hydrogen ion type gel chromatographic columns, used to flow
Dynamic is mutually weakly acidic aqueous solution, nontoxic, safety and environmental protection and testing cost is cheap.To detect 2000 sample calculating every year, often
A sample is calculated using 15ml acetonitriles, can save mobile phase cost 30L every year, every year can be cost-effective near on reagent
5000 yuan.
2nd, hydrogen ion type gel chromatographic columns are more more durable than nh 2 column used in this method, and use is proper, can continuously make
Use the several years.And nh 2 column is then very fragile, does not notice that Bonded Phase will come off slightly, and column effect is caused drastically to decline and scrap.
3rd, for this method using hydrogen ion type gel chromatographic columns compared to nh 2 column, reproducibility, accuracy are more preferable.This is main
Allowing for need to use acetonitrile and water two-phase to prepare using the mobile phase of nh 2 column, it is necessary to consider volume effect during two mixing
Should, it is difficult to ensure that the ratio prepared every time is all completely the same, this can influence the retention time and peak type of chromatographic peak, influence method
Reproducibility.And as the growth of usage time, the column effect of nh 2 column can constantly decline always, cause to ensure separation effect
Fruit often will according to circumstances adjust the ratio of acetonitrile, this can further reduce the reproducibility and accuracy of method.
Description of the drawings
Fig. 1 is the chromatography stacking chart of glycerine in glycerine standard specimen and beer sample, wherein, in lap, peak area
Big is the glycerine peak in glycerine standard specimen, the small glycerine peak in beer sample of peak area.
Specific embodiment
The technical solution in the embodiment of the present invention will be clearly and completely described below, it is clear that described implementation
Example is only part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, this field is common
Technical staff's all other embodiments obtained without making creative work belong to the model that the present invention protects
It encloses.
Embodiment 1
1) foundation of standard working curve：
Glycerine standard items (purity 100%) 2.0905g is accurately weighed with electronic balance, adds in ultra-pure water stirring and dissolving,
25mL is settled to, obtains the glycerin solution of a concentration of 1. 83.62g/L.This solution of different volumes is measured with surpassing with liquid-transfering gun
Pure water mixes, and obtains diluted glycerin solution step by step, 3. concentration respectively 2. 41.81g/L (2 times of dilution), 27.87g/L (3
Times), the glycerin solution of 4. 20.91g/L (4 times), 5. 13.94g/L (6 times), 6. 6.97g/L (12 times).By it is a concentration of 5.
The glycerin solution of 13.94g/L and 6. 6.97g/L dilute 12 times again, obtain a concentration of 7. 1.162g/L and 8. 0.58g/L the third three
Alcoholic solution.
By the glycerin solution of above-mentioned 8 concentration gradients successively sample detection.Using glycerol concentration as abscissa, chromatography
Peak peak area response obtains equation of linear regression as Y=8.97e+004X+9.05e+003, R as ordinate2=
0.999915.In linear concentration range, the working curve of glycerine is linearly good, is suitble to quantitative analysis.
2) sample pre-treatments：
Beer fermentation liquid is poured into the funnel equipped with fast grade filter paper, collects filtrate, and filtrate is passed through into 0.22 μm of film mistake
Filter；Alternatively, after finished beer is deaerated, by 0.22 μm of membrane filtration.
Meanwhile a certain batch Ao Gute beer that can choose Qingdao Beer Brewery's production is contained as control sample by it in sample
Measure the fixed preceding deemed-to-satisfy4 verification of progress.
3) liquid-phase chromatographic analysis：
Liquid chromatograph：2695 systems of Waters Alliance, Waters Column Heater Module,
2414 differential refraction detectors of Waters and Empower Chromatography Management Systems (Waters, US)；Test condition is：Hydrogen
Ionic gel chromatographic columns 300 × 7.8mm of Rezex ROA (00H-0138-KO)；Detector temperature：40℃；Column oven temperature：
60℃；Flow velocity：0.6ml/min；Run time：25 minutes；Mobile phase：85% phosphoric acid of 0.36mL is added in ultra-pure water, it is fixed
Hold to 1L, through 0.22 μm of membrane filtration, ultrasound degassing 5 minutes.
Standard specimen and sample are detected using above-mentioned liquid-phase chromatographic analysis condition, it is as shown in Figure 1 to obtain chromatogram.
4) method reproducibility index
To same beer sample continuous sample introduction 8 times, glycerine peak area is calculated, obtains method reproducibility index.Such as 1 institute of table
Show.
Table 1
Relative standard deviation is 0.53%, slightly better than the amino column method (0.78%) of document report.
5) recovery of standard addition index
Glycerine standard solution is prepared, a concentration of 11.645g/L takes 0.5ml, 1.0ml, 1.5ml, 2.0ml respectively,
2.5ml is added in 25mL volumetric flasks, and groove is settled to control beer sample.Detection control beer and control beer mark-on respectively
Glycerol content afterwards.Calculate recovery of standard addition.As shown in table 2.
Table 2
Recovery of standard addition 97.7%-100.2%, better than the nh 2 column method (103.9%-116.0%) of document report.
6) in beer sample glycerine measure
The content of glycerine in different category beer is detected according to the method described above, and testing result is as shown in table 3.
Table 3
Beer glycerol content is between 0.6-2.5g/L.Barms are the main factors for influencing glycerol content.
The top fermented beers such as white beer, IPA are generally higher than bottom fermentation beer.
Embodiment 2
IPA Process of Beer Brewing is chosen, from yeast addition until cold storage.According to the method described above in beer fermentation process
For glycerol content into line trace, testing result is as shown in table 4.
Table 4
With reference to 4 data of table it is found that from yeast addition until the 5th day, glycerol content is always in lasting rising, later substantially
Maintain stable state.It can be seen that method provided herein can effectively detect the content of glycerine in beer sample.
Claims (4)
1. the detection method of glycerine in a kind of beer, which is characterized in that include the following steps：
1) prepared by standard working solution：
The glycerine standard working solution with 8 grades of concentration gradients is prepared respectively, and concentration range is：0.58g/L-41.81g/L,
By prepared standard working solution by 0.22 μm of membrane filtration, dispense in 2ml centrifuge tubes, freezen protective is restored to before detection
Room temperature simultaneously shakes up；
2) prepared by sample solution：
Beer fermentation liquid is poured into the funnel equipped with fast grade filter paper, collects filtrate, and filtrate is passed through into 0.22 μm of membrane filtration；Or
Person, after finished beer is deaerated, by 0.22 μm of membrane filtration；
3) liquid-phase chromatographic analysis：
Hydrogen ion type gel chromatographic columns are equipped with using liquid chromatograph to carry out made testing sample solution and standard working solution
Analysis, obtains related chromatogram；
4) Specification Curve of Increasing and result calculate.
2. the detection method of glycerine in beer according to claim 1, which is characterized in that the hydrogen ion type gel color
Spectrum column is 300 × 7.8mm of Rezex ROA.
3. the detection method of glycerine in beer according to claim 1, which is characterized in that the liquid chromatogram item of glycerine
Part is：Detector temperature：40℃；Column oven temperature：60℃；Flow velocity：0.6ml/min；Run time：25 minutes；Mobile phase：It will
85% phosphoric acid of 0.36mL is added in ultra-pure water, is settled to 1L, through 0.22 μm of membrane filtration, ultrasound degassing 5 minutes.
4. the detection method of glycerine in beer according to claim 1, which is characterized in that the preparation of standard working solution
Method：Glycerine standard items 2.0905g is accurately weighed with electronic balance, ultra-pure water stirring and dissolving is added in, is settled to 25mL, obtains
The glycerin solution of a concentration of 83.62g/L.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112730720A (en) * | 2020-12-28 | 2021-04-30 | 湖州中科院应用技术研究与产业化中心 | Liquid phase detection method for vitronectin in cosmetics |
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