CN110514777A - A kind of method that a variety of sugar, sugar alcohols and alcohols quickly detect simultaneously in beer - Google Patents
A kind of method that a variety of sugar, sugar alcohols and alcohols quickly detect simultaneously in beer Download PDFInfo
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- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
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- 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
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
- G01N2030/8809—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample
- G01N2030/884—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample organic compounds
Abstract
The invention discloses a variety of sugar in a kind of beer, the method that sugar alcohol and alcohols quickly detect simultaneously, belong to analytical chemistry field, the present invention uses integrated pulsed amperometric-chromatography of ions, by optimizing pre-treatment detection method, research influences the empirical factor of component separation, it establishes disposable while detecting 23 kinds of carbohydrates in beer, sugar alcohol, alcohols (2, 3- butanediol, ethyl alcohol, methanol, glycerine, antierythrite, xylitol, fucose, arabite, sorbierite, trehalose, ribitol, mannitol, 2-deoxy-D-glucose, mannose, melibiose, glucose, maltitol, fructose, lactose, ribose, sucrose, gossypose, maltose) method, it solves to carbohydrate in beer, the technical problem that sugar alcohol and alcohols multicomponent are accurately analyzed, this method is quick, accurately, it is sensitive, it realizes more Classification is multi-component to be analyzed simultaneously, makes important contribution to beer component detection.
Description
Technical field
The invention belongs to analytical chemistry fields, and in particular to a variety of sugar, sugar alcohols and alcohols quickly inspection simultaneously in a kind of beer
The method of survey.
Background technique
Beer is using malt and hops as raw material, and alcohol made of brewing after gelatinization, saccharification, liquid state fermentation is drunk
Expect, the ingredients such as multivitamin, amino acid, carbohydrate, glycitols are contained in beer.Saccharide compound is polyhydroxyl aldehydes or ketones
And its derivative, it is the energy substance of human life activity, is the important component of numerous food product and beverage.Sugar alcohol is the aldehyde of carbohydrate
Substance after base or ketone group are reduced has prevention sugar usually by the corresponding sugared sweetener generated by catalytic hydrogenation
The advantages that urine is sick, heat is low, in good taste.Alcohols is the important component in certain fermented foods, and it is strong that certain alcohols are beneficial to human body
Health, but certain alcohols such as butanediol have certain toxicity.The analysis of carbohydrate is always one of the difficult point of analytical chemistry, mesh
Regulation in preceding national food safety standard " prepackaged food nutritional labeling general rule ", it is necessary to which clearly mark is eaten in the label of food
The energy of product, the i.e. content of carbohydrate.Property and effect based on sugar alcohol and alcohols in certain food, these two types of components contain
The detection of amount is also extremely important.
Sugar in beer, sugar alcohol and alcohols are its important component parts, the size of content directly concerning the quality of beer and
Quality.Currently, the analysis method of carbohydrate, sugar alcohol, alcohols mainly has liquid chromatography, Liquid Chromatography/Mass Spectrometry, gas chromatography, enzyme electricity
Pole method, the chromatography of ions.Liquid chromatography facilitates general, but sensitivity is low, difficult for the sample detection of complex matrices.Gas phase
Chromatography high sensitivity, but need to derive, quantitative repeatability is poor, and discomfort is fit to do accurate quantitative analysis.Enzyme Electrode is general only
A kind of carbohydrate is detected, there is preferable specificity, but not can be carried out multicomponent while detecting.
Currently, although the method that people detect sugar a variety of in beer, sugar alcohol and alcohols simultaneously possesses some special knowledge, but in mesh
The group only detected to certain a kind of component (such as simple carbohydrate or alcohols) or simultaneously that can be retrieved in preceding data bank
Dosis refracta is less (only the sugar to 10 kinds or so and sugar alcohol are analyzed simultaneously), is not able to satisfy growing detection demand and therefore grinds
Study carefully and establish good, high sensitivity a variety of sugar of a kind of strong applicability, selectivity, the method that sugar alcohols and alcohols detect simultaneously, has
Important realistic meaning and application value.
Summary of the invention
The purpose of the present invention is in view of the above shortcomings of the prior art, using integrated pulsed amperometric-chromatography of ions, optimize
Pre-treatment detection method establishes disposable while detecting in beer 23 kinds by the research of the influence factor separated to component
The method of carbohydrate, sugar alcohol and alcohols, this method is quick, simplicity, high sensitivity, stability are good, realizes quickly analysis and green
Analysis solves the technical issues of sugar, sugar alcohol and alcohols Simultaneous Analysis for Multicomponent in beer.
In order to achieve the above objectives, the invention discloses 23 kinds of sugar, sugar alcohol and alcohols in a kind of beer simultaneously detect method,
Its detecting step is as follows；
Step 1: the configuration of mixed standard solution:
By 2,3- butanediol, ethyl alcohol, methanol, glycerine, antierythrite, xylitol, fucose, arabite, sorbierite, sea
Algae sugar, ribitol, mannitol, 2-deoxy-D-glucose, mannose, melibiose, glucose, maltitol, fructose, lactose,
Ribose, sucrose, gossypose, maltose standard solution configure mixed standard solution as needed；
Step 2: sample to be tested pre-treatment:
Beer measuring samples are ultrasonically treated 30 min(and remove removing carbon dioxide), 0.100 g of beer measuring samples is taken, is added ultrapure
About 150 mL of water shakes up and stands 15 min, and adjusting dilution pH value to 5.0~6.5 is fully transferred in 200 mL volumetric flasks,
Scale is settled to using ultrapure water, shakes up, stand 15 min, takes 10.0 mL solution, first after preactivated IC-H10 column
(heavy-metal ion removal), finally after preactivated IC-RP column, discards preceding 3 mL after 0.22 μm of water phase filter membrane, receives
Collect back segment clear liquid, to upper machine testing.
Step 3: ion chromatography condition and multistage gradient elute condition
Chromatography column: DionexCarboPacTM MA1 (4 × 250 mm)；
Guard column: DionexCarboPacTM MA1 (4 × 50 mm)；
Working electrode: Gold；
Reference electrode: AgCl electrode；
Mobile phase: A:1000 mmol/L NaOH solution, B: ultrapure water；
Flow velocity: 0.45 mL/min；
Column temperature: 29 DEG C；
Sample volume: 10 μ L；
Multistage gradient elutes condition:
Multistage gradient rinse procedures are as follows: when 0.0-75.0 min, leacheate NaOH concentration is 480.0 mmol/L；75.0-80.0
Min, leacheate NaOH concentration are 480.0-600.0 mmol/L；80.0-105.0 min, leacheate NaOH concentration is 600.0
mmol/L；105.0-110.0 min, leacheate NaOH concentration is 600.0-480.0 mmol/L；110.0-120.0 min, leaching
Washing lotion NaOH concentration is 480.0 mmol/L；See Table 1 for details.
1 ion chromatography of table elutes condition
Step 4: calibration curve is drawn:
The chromatographiccondition and multistage gradient that the mixed standard solution configured in step 1 is provided according to step 3 elute item
Part is detected using ion chromatograph, using constituent mass concentration to be measured as abscissa, using component peak area to be measured as ordinate,
To draw calibration curve, quantified by external standard method；
Step 5: the detection of sample solution:
Chromatographiccondition and multistage gradient elution condition that gained clear liquid in step 2 is provided according to step 3 are used into ion
Chromatograph is detected, and calculated result；
Step 6: result calculates:
By result measured by step 4 mixed standard solution come calculated result measured by aligning step five, to calculate institute
Survey each component content in beer.
As preferred；Above-mentioned solution uses the ultrapure water that resistivity is 18.2 M Ω cm to prepare.
The utility model has the advantages that
1, sugar, sugar alcohol and alcohols multi-component material detect simultaneously in beer, are always the technical problem of this analysis field, the present invention
It is disposable to determine 23 kinds of sugar, sugar alcohol and alcohols in beer simultaneously, detection working efficiency greatly improved, reduce detection manpower
Material resources cost, with good economic efficiency and social application value.
2,23 kinds of carbohydrates, sugar alcohol, alcohols are the very big work of a technical difficulty in separation detection beer simultaneously.In order to mention
The overall separation degree of high component, compares by many experiments, and present invention selection uses the hydrogen of 480 mmol/L in preceding 75 min
Sodium hydroxide solution carries out isocratic elution, carries out the strength of chromatographic column using the sodium hydroxide solution of 600 mmol/L after 80 min
It rinses, removal influences the chaff interferent of component to be measured, can increase substantially the accuracy of detection.
3, the present invention deeply investigates the multistage gradient elution condition that analyzes, initially elutes concentration, chromatogram column temperature, pH value of solution
The experimental factors such as value have found optimal experimental analysis condition, most by the Influencing Mechanism of the various empirical factors of research analysis
Improves multicomponent while examining the accuracy of time study method to big degree.
4, the present invention passes through the study found that solution ph detects 23 kinds of components in beer simultaneously has great influence, pH
Fluctuation occurs for the measurement content that the variation of value directly results in certain components.By the model for adjusting solution ph to 5.0~6.5
In enclosing, the accuracy and precision of detection can be greatly improved.
5, the present invention analyzes influence of the chromatogram column temperature to detection, and the variation that each degree Celsius of chromatogram column temperature will
It is overlapped certain components.In 29 DEG C of column temperatures, it is able to achieve efficiently separating for 23 kinds of components just.
6, the method for the present invention is easy to operate quick, sensitive and accurate, by simple pre-treatment, can go up machine testing, 23 kinds of groups
Dividing in 70 min can whole appearance.
7, do not use or generate in detection method the solvent toxic to human health, ecological environment,
Reagent, by-product, while consumptive material used is seldom, has green, environmental protection, the technological merit saved.
Detailed description of the invention
Fig. 1 is the chromatography of ions figure of 23 kinds of sugar, sugar alcohol and alcohols mixed standard solution.
Fig. 2 is the chromatography of ions figure of lower standard solution different in flow rate.
Fig. 3 is the chromatography of ions figure of mixed standard solution under different initial eluent concentrations.
Fig. 4 is the chromatography of ions figure of mixed standard solution under different column temperatures.
Fig. 5 is the chromatography of ions figure of 5 kinds of common beer samples.
Corresponding substance: 1. 2,3- butanediols (2,3-Butanediol) is respectively numbered in attached drawing；2. ethyl alcohol
(Alcohol)；3. methanol (Methanol)；4. glycerine (Glycerol)；5. antierythrite (Erythritol)；6. wood
Sugar alcohol (Xylitol)；7. fucose (Fucose)；8. arabite (Arabinitol)；9. sorbierite
(Sorbitol)；10. trehalose (Trehalose)；11. ribitol (Ribitol)；12. mannitol (Mannitol)；13.
2-deoxy-D-glucose (2-Deoxy-D-glucose)；14. mannose (mannose)；15. melibiose (Melibiose)；
16. glucose (Glucose)；17. maltitol (Maltitol)；18. fructose (Fructose)；19. lactose
(Lactose)；20 ribose (Ribose)；21. sucrose (Sucrose)；22. gossypose (Raffinose)；23. maltose
(Maltose).
Specific embodiment
Embodiment one: a kind of method that 23 kinds of sugar, sugar alcohol and alcohols detect simultaneously in beer
1. instrument and reagent
Ion chromatograph (Thermo Scientific company ICS5000+) is equipped with electrochemical detector and autosampler
(AS-SP)；Milli-Q ultrapure water instrument (Millipore company, the U.S.)；(the letter instrument in Shanghai is limited for Ultrasonic Intelligent washer
Company DL-360E)；Electronic balance (Mei Tele company ML802/02)；Experimental water: ultrapure water (resistivity 18.2M Ω .cm)；
Carbohydrate, sugar alcohol, alcohols standard items or standard reagent (purity > 98%)；Sodium hydroxide solution (50%w/w, Fisher
Chemical)；Hydrochloric acid (excellent pure grade)；IC-RP10 column (Agela Technologies)；IC-H10 column (Agela
Technologies).
2. ion chromatography condition
Chromatography column: Dionex CarboPacTMMA1 (4 × 250 mm), guard column: Dionex CarboPacTM MA1
(4×50 mm)；Integrated pulsed amperometric detection；Working electrode: Gold (Au)；Reference electrode: AgCl electrode；Potential waveform:
Gold,Carbo,Quad；Mobile phase: NaOH leacheate；Flow velocity: 0.45 mL/min；Column temperature: 29 DEG C；Sample volume: 10 μ L.Just
Begin elution concentration: 480 mmol/L NaOH solutions.
3. multistage gradient elutes condition
Multistage gradient rinse procedures are as follows: when 0.0-75.0 min, leacheate NaOH concentration is 480.0 mmol/L；75.0-80.0
Min, leacheate NaOH concentration are 480.0-600.0 mmol/L；80.0-105.0 min, leacheate NaOH concentration is 600.0
mmol/L；105.0-110.0 min, leacheate NaOH concentration is 600.0-480.0 mmol/L；110.0-120.0 min, leaching
Washing lotion NaOH concentration is 480.0 mmol/L；See Table 1 for details.
4. the configuration of mixed standard solution
By 2,3- butanediol, ethyl alcohol, methanol, glycerine, antierythrite, xylitol, fucose, arabite, sorbierite, sea
Algae sugar, ribitol, mannitol, 2-deoxy-D-glucose, mannose, melibiose, glucose, maltitol, fructose, lactose, core
Sugar, sucrose, gossypose, maltose standard solution configure certain density mixed standard solution as needed.
5. pre-treating method
About 10 g of beer sample, ultrasonic 30min(is taken to remove removing carbon dioxide).0.10 g of beer measuring samples is accurately taken, is added super
About 150 mL of pure water shakes up and stands 15 min, adjusts the pH value of dilution to 5.0~6.5, be fully transferred to 200 mL volumetric flasks
In, scale is settled to using ultrapure water, shakes up, stand 15 min, takes 10.0 mL solution, first after preactivated IC-H10
Column finally after preactivated IC-RP column, discards preceding 3 mL, back segment clear liquid is collected, to upper after 0.22 μm of water phase filter membrane
Machine testing.
According to above-mentioned experimental analysis condition, 23 kinds of sugar, sugar alcohol and the alcohols of mixed standard solution are detected, detected
As a result as shown in Figure 1.
Embodiment two: influence of the flow velocity to detection
According to the condition of the experimental analysis in embodiment one, the flow velocity of leacheate is successively tested in the case where other conditions are constant
For the component of mixed standard solution under 0.30 mL/min, 0.40 mL/min, 0.45 mL/min, 0.50 mL/min flow conditions
Situation is separated, the chromatography of ions figure of lower mixed standard solution different in flow rate is as shown in Figure 2；It elutes flow velocity and system pressure
Relationship is as shown in table 2.
The relationship of table 2 elution flow velocity and system pressure
Fig. 2 and table 2 are combined it can be concluded that, elution flow velocity it is bigger, system pressure is bigger, and component appearance time is faster, stream
Speed increases to 0.50 mL/min from 0.30 mL/min, and 23 kinds of total appearance times of component are gradually decreased to 62 min by 90 min, and are
System pressure is incrementally increased by 890 psi to 1455 psi.It is seen in fig. 1, that in 0.30 mL/min, system pressure 890
Psi, because flow velocity is low, pressure is smaller, and component peak width is caused to increase, and chromatographic peak sensitivity is decreased obviously.0.40 mL/min flow velocity
When, system pressure reaches 1170 psi, although component sensitivity increases, the total appearance time of component is longer by nearly 80
min.When 0.50 mL/min flow velocity, the total appearance time of component shortens, but the totality point since system pressure is larger, between component
Become smaller from degree, especially component 10 and 11, separating degree is substantially reduced between component 18 and 19.And flow velocity is eluted in 0.45 mL/
When min, initial pressure is 1310 psi, 23 kinds of components in 70 min can whole appearances, and sensitivity and separating degree compare
It is more satisfactory.Therefore, consider that the present invention selects under 0.45 mL/min flow velocity from system stability, separating degree, sensitivity factor
It is tested.
Embodiment three: multistage gradient elutes influence of the condition to detection
According to the condition of the experimental analysis in embodiment one, it is dense that initial leacheate is successively tested in the case where other conditions are constant
Mixed standard solution component separates situation, hybrid standard to degree under conditions of 450,470,480,490,500 mmol/L respectively
The component separation situation of solution is as shown in Figure 3.
From figure 3, it can be seen that initially elution concentration is in 450 mmol/L, the separation of component 7 and 8, component 19 and 20
Degree is not high, and component 10 and 11 is almost overlapped；For initial elution concentration in 470 mmol/L, the separating degree of component 10 and 11 is not high；Just
When the elution concentration that begins is respectively 490,500 mmol/L, the separating degree of component 14 and 15 is decreased obviously, and component 18 and 19 is not implemented
Separation；And concentration is initially eluted in 480 mmol/L, the overall separation degree of this 23 kinds of components and sensitivity are ideal.Cause
This, considers from overall separating degree, and initial elution 480 mmol/L of concentration of present invention selection is detected.
Example IV: influence of the chromatographic column temperature to detection
According to the condition of the experimental analysis in embodiment one, successively tested in the case where other conditions are constant 26 DEG C, 28 DEG C,
29 DEG C, 30 DEG C, the component of mixed standard solution separates situation under 32 DEG C of chromatographic column temperatures, the component of mixed standard solution separates feelings
Condition is as shown in Figure 4.
Figure 4, it is seen that in 26 DEG C to 32 DEG C temperature ranges, as the temperature rises, the total appearance time of component
Shorten, appearance rate increases.At 26 DEG C, component 10 and 11, the these two pair component of component 17 and 18 are almost overlapped；At 28 DEG C, component
Separating degree between 10 and component 11 is not high；At 30 DEG C, the separating degree between component 18 and 19 is smaller, is not able to satisfy quantitative analysis
Requirement；At 32 DEG C, component 18 and component 19 are completely overlapped, this three pairs of components of component 7 and 8, component 9 and 10, component 14 and 15
Between separating degree it is smaller；At 29 DEG C, the separating degree of 23 kinds of components and sensitivity are ideal.It can be seen that temperature is to 23
Kind component measures simultaneously significant impact, and each degree Celsius of variation, which this may result in two or more components, effectively to divide
From.To sum up, consider that the present invention is chosen under 29 DEG C of column temperatures and carries out in fact from the separating degree of improvement method, sensitivity, selective angle
Test analysis.
Embodiment five: influence of the pH value to detection
According to the condition of the experimental analysis in embodiment one, in the case where other conditions are constant, different pH value are configured in order
The mixed standard solution of the same theory concentration of (2.0-12.0) carries out machine testing, and experimental result confirms, glycerine, rock algae
This 9 kinds of components of sugar, ribitol, mannose, melibiose, glucose, maltitol, ribose, maltose by solution ph influenced compared with
Greatly, other components are influenced smaller by pH value, and different pH value are to glycerine, fucose, ribitol, mannose, melibiose, grape
Sugar, maltitol, ribose, malt sugar detection influence as shown in chart 3.
Influence of 3 solution ph of table to 9 kinds of compound mensuration contents
From table 3 it is observed that there is certain journey under strong acid and strong alkaline condition in glycerine and glucose assays content
The increase of degree, this is because many components (such as strong acid or strong alkali environment) under the conditions of certain pH value, are easy to generate a certain amount of
Glucose, and glycerine is a kind of trihydroxylic alcohol, there are three hydroxyls for tool, under strong acid or basic conditions, it is easier to ionize, examine
Content is surveyed to increase；It is little that fucose, mannose, melibiose, ribose measure changes of contents in acid condition, and is greater than in pH value
Under 8.3 alkaline condition, there is a degree of reduction in measurement content, and in pH value 11.0, measurement contains especially melibiose
64.8% when amount only has neutral；Ribitol is surveyed in the case where pH value is less than 4.1 acid conditions and under alkaline condition of the pH value greater than 8.3
Determine content and certain fluctuation occur, affects quantitative analysis；Under acid and alkaline condition, measurement content maltose occurs
It reduces, this is because maltose is easy to happen the reaction such as hydrolysis at this time.As seen from Table 3, in the mild acid conditions of pH value 5.0-6.5
Under, 9 kinds of compound mensuration changes of contents very littles, fluctuation all within 3.8%, illustrates that component ion concentration is stablized at this time.Therefore,
Comprehensively consider the influence factors such as 23 kinds of component physicochemical characteristic, dissociation degree, sensitivity, the present invention is selected pH value 5.0-6.5's
Mild acid conditions are measured analysis.
Embodiment six: the range of linearity and detection limit
The mixed standard solution for configuring various concentration uses the laboratory apparatus and chromatographic condition progress calibration curve in embodiment 1
Fitting.The detection limit (S/N=3) that component to be measured is calculated by chromatographic peak signal-to-noise ratio, in the mg/L concentration of 0.10 mg/L~10.0
In range, it is molten 7 various concentration levels (0.10,0.20,0.40,1.0,2.0,4.0,10.0 mg/L) hybrid standard has been carried out
The detection of liquid and linear fit.The results are shown in Table 4 for it.
The range of linearity, linear equation, related coefficient and the detection limit (S/N=3) of the measurement component of table 4
Y: peak area (nC.min), X: mass concentration (mg/L)
From 4 available 23 kinds of composition coefficient Rs of table2All greater than 0.999, wherein there is 18 kinds of component coefficient Rs2
Greater than 0.9995, while the absolute value of the intercept of 23 kinds of composition equations is respectively less than 0.008, this is absolutely proved tests item herein
Under part, measuring method is stable, linear good simultaneously for 23 kinds of components.Other than methanol and ethyl alcohol, other 21 kinds of component detection limits exist
Between 0.0109~0.2069 mg/L.
Embodiment seven: the measurement of the rate of recovery and precision
3 kinds of beer samples are randomly selected, it is respectively 0.20 mg/L, 1.00 that concentration stratification levels are successively added into 3 samples
The mixed standard solution of mg/L, 2.00 mg/L, each concentration level carries out 6 replicate experiments, to verify different beer bases
Matter surveys the rate of recovery and precision of timing method, according to the measurement concentration calculation rate of recovery after substrate concentration, addition concentration and addition.
Table 5 lists the average recovery rate and RSD data of three concentration levels, six Parallel testings.
Table 5 measure component the rate of recovery and precision (RSD) (n=6)
As can be seen from Table 5, in the case where 0.20 mg/L adds concentration level, the rate of recovery of only methanol is 79.70%, but can
Meet food physical and chemical analysis technical requirements (for measurement content less than 0.10 mg/L, the rate of recovery should be 60%~120%).23 kinds of carbohydrates,
The rate of recovery of sugar alcohol, alcohol component in three kinds of matrix under three concentration levels is between 79.70%~107.13%, determination data
RSD is in 1.78%~10.85% range.This absolutely proves that three kinds of matrix, six Parallel testing rate of recovery data results meet food
The requirement of product Physico-chemical tests, the detection method accuracy is high, precision is good.
Embodiment eight: the measurement of actual sample
5 kinds of common beer (beer -1, beer -2, beer -3, dark beer -1, dark beer -2) are successively extracted, according to embodiment one
Intermediate ion chromatographic condition and pre-treatment step have carried out the detection point of 23 kinds of carbohydrates in actual sample, sugar alcohol, alcohol component content
Analysis, Fig. 5 are actual sample measurement chromatography of ions figure, and table 6 is detected components data result
The measurement result (mg/L) of 6 beer sample of table
"-": it is not detected
From in Fig. 5 and table 6 as can be seen that the carbohydrate detected in five kinds of beer, sugar alcohol, alcohol component quantity be successively 12,14,
11,16,15 kind, the type for detecting Hubeiwan in beer is more, content is bigger, and quality is better, measuring result and sample
The practical quality status of product is consistent completely.From the point of view of detecting component, the detection biggish component of content is glycerine, ethyl alcohol, lactose, Portugal
Grape sugar, trehalose, sorbierite, mannitol etc..Carbohydrate, sugar alcohol be more than type in yellow beer from the point of view of beer type, in dark beer
It is abundant.
It can be seen that detection baseline stability from actual sample chromatography of ions figure above, peak shape is sharp, is interfered by other substances
It is smaller, this absolutely prove the detection method have good stability, accuracy it is high.In terms of actual sample measurement result, the detection method
It is easy to operate, quick and precisely, it is practical.
The present invention is begged for by the analysis to kinds of experiments influence factors such as initial elution concentration, flow velocity, column temperature, solution ph
By having explored the gradient conditions of 23 kinds of sugar, sugar alcohol and alcohols in beer while measurement, established integrated pulsed amperometric-
The analysis method of 23 kinds of sugar of Simultaneous Determination, sugar alcohol and alcohols.This method is easy, quick, sensitive, accurate, is suitable for
The quick analysis of 23 kinds of sugar, sugar alcohol and alcohols in beer.
Protection content of the invention is not limited to above embodiments, without departing from the spirit and scope of the invention, this
Field technical staff it is conceivable that variation and advantage be all included in the present invention, and with appended claims be protect
Protect range.
Claims (2)
1. a kind of method that a variety of sugar, sugar alcohol and alcohols quickly detect simultaneously in beer, it is characterised in that the following steps are included:
Step 1: the configuration of mixed standard solution:
By 2,3- butanediol, ethyl alcohol, methanol, glycerine, antierythrite, xylitol, fucose, arabite, sorbierite, sea
Algae sugar, ribitol, mannitol, 2-deoxy-D-glucose, mannose, melibiose, glucose, maltitol, fructose, lactose,
Ribose, sucrose, gossypose, maltose standard solution configure mixed standard solution as needed；
Step 2: sample to be tested pre-treatment:
Beer measuring samples are ultrasonically treated 30 min, take 0.100 g of beer measuring samples, about 150 mL of ultrapure water is added, shakes
15 min of even standing adjust dilution pH value to 5.0~6.5, are fully transferred in 200 mL volumetric flasks, using ultrapure water constant volume
It to scale, shakes up, stand 15 min, take 10.0 mL solution, first after preactivated IC-H10 column, after 0.22 μm of water phase
Filter membrane discards preceding 3 mL finally after preactivated IC-RP column, back segment clear liquid is collected, to upper machine testing；
Step 3: ion chromatography condition and multistage gradient elute condition:
Chromatography column: Dionex CarboPacTM MA1 (4 × 250 mm)；
Guard column: Dionex CarboPacTM MA1 (4 × 50 mm)；
Working electrode: Gold；
Reference electrode: AgCl electrode；
Mobile phase: A:1000 mmol/L NaOH solution, B: ultrapure water；
Flow velocity: 0.45 mL/min；
Column temperature: 29 DEG C；
Sample volume: 10 μ L；
Multistage gradient elutes condition
Multistage gradient rinse procedures are as follows: when 0.0-75.0 min, leacheate NaOH concentration is 480.0 mmol/L；75.0-80.0
Min, leacheate NaOH concentration are 480.0-600.0 mmol/L；80.0-105.0 min, leacheate NaOH concentration is 600.0
mmol/L；105.0-110.0 min, leacheate NaOH concentration is 600.0-480.0 mmol/L；110.0-120.0 min, leaching
Washing lotion NaOH concentration is 480.0 mmol/L；Step 4: calibration curve is drawn:
The chromatographiccondition and multistage gradient that the mixed standard solution configured in step 1 is provided according to step 3 elute item
Part is detected using ion chromatograph, using constituent mass concentration to be measured as abscissa, using component peak area to be measured as ordinate,
To draw calibration curve, quantified by external standard method；
Step 5: the detection of sample solution:
Chromatographiccondition and multistage gradient elution condition that gained clear liquid in step 2 is provided according to step 3 are used into ion
Chromatograph is detected, and calculated result；
Step 6: result calculates:
By result measured by step 4 mixed standard solution come calculated result measured by aligning step five, to calculate institute
Survey each component content in beer.
2. the method that a variety of sugar, sugar alcohol and alcohols quickly detect simultaneously in a kind of beer according to claim 1, feature
It is, above-mentioned solution uses the ultrapure water that resistivity is 18.2 M Ω cm to prepare.
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