CN106404956A - Method for detecting four organic acids in wine and/or fruit wine at same time through high performance liquid chromatography-tandem mass spectrometry internal standard method and application of method - Google Patents
Method for detecting four organic acids in wine and/or fruit wine at same time through high performance liquid chromatography-tandem mass spectrometry internal standard method and application of method Download PDFInfo
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Abstract
The invention discloses a method for detecting four organic acids in wine and/or fruit wine at the same time through a high performance liquid chromatography-tandem mass spectrometry internal standard method and application of the method and belongs to the field of organic acid detection and application. High performance liquid chromatography and mass spectrometry are combined, detection conditions of chromatography and mass spectrometry are optimized, and the wine or the fruit wine is simply treated and then directly measured, so that content of tartaric acid, malic acid, succinic acid and citric acid can be detected quantitatively. The method is low in detection limit, high in selectivity, simple and quick in pretreatment, free of loss in the process, high in detection sensitivity, accurate and reliable in detection result and capable of realizing quick and accurate detection of the four organic acids, and technical support is provided for quickly identifying blended fake wine and fruit wine, protecting dining table safety of consumers and maintaining healthy development of wine market.
Description
Technical field
The present invention relates to one kind detects grape wine and/or fruit wine based on high performance liquid chromatography-tandem mass internal standard method simultaneously
In four kinds of organic acids method, belong to organic acid detection and applied technical field.
Background technology
Fast development with China's economy and growth in the living standard, have the grape wine of long history and cultural deposits
Increasingly liked by people with fruit wine, gone on the daily dining table of common people.It is by the tune to acid-base balance in human body
Section, makes the physiologically active of various enzymes be achieved, thus promoting the metabolic in vivo body being normally carried out, being conducive to drinking person
Body health.But, have illegal retailer to see in the market lucrative, using raw materials such as food coloring, edible alcohol, sweeteners
Blend making fake wine, such fake wine is luxurious high-end and atmospheric and price is very high from the appearance, several units can be only by one bottle of cost, and excessive
Take in food coloring or sweetener can increase burden of liver and damage the healthy of consumer.Therefore, for protection consumer's
Dining table safety and the sound development safeguarding grape wine and fruit wine market, set up a kind of quick discriminating and blend littlefruit grape herb wine and fruit wine
Method has great importance.
Grape wine is considerably complicated with the composition in fruit wine, and wherein organic acid is important component, is impact grape wine and fruit wine
Local flavor and wine product quality key factor, be also one of the important indicator differentiating product quality.High-quality grape wine and fruit
The kinds of organic acids of wine and content are mainly affected by fermentation, have up to tens kinds organic acid ginsengs in whole sweat
With reaction, the four kinds of acid of content highest are tartaric acid (tartaric acid, content 1.5～2.5g/L), malic acid (malic
Acid, content 1.5～3.0g/L), butanedioic acid (succinic acid, content 0.6～1.5g/L) and citric acid (citric
Acid, content 0.10～0.15g/L).Fake producer, in order to keep local flavor and the mouthfeel of grape wine and fruit wine, generally only adds a large amount of
Citric acid blent.Therefore, in national standard《Grape wine》(GB 15037-2006)、《Wild grape wine》(GB/T
The maximum level of citric acid is all defined in 27586-2011).Due in wine blend and without tartaric acid, malic acid and amber
Amber these three materials of acid, therefore, the detection to these three compositions being capable of auxiliary judgment wine blend or fruit wine.
Detection with regard to organic acid has multiple methods, in field of food, in addition to high performance liquid chromatography, also thin-layer chromatography
The chromatograph joint used method of method, gas chromatography, makings, capillary electrophoresis and high performance liquid chromatography-tandem mass method (HPLC-MS/
MS) etc..Thin-layered chromatography accuracy is poor, can only qualitative or sxemiquantitative；Before gas chromatography and the chromatograph joint used method of makings
Process and need to be derived organic acid by the method for esterification, step complexity is loaded down with trivial details；Capillary electrophoresis technique method sensitivity is low,
Reappearance is poor.?《Grape wine, fruit wine universaling analysis method》(GB/T15038-2006) define in and utilize high-efficient liquid phase color
The method that spectral technology measures organic acid, but the activation of solid-phase extraction column to be carried out in the pretreatment process of the method, elute and receive
Collection sample, very loaded down with trivial details, and the pigment in wine also can disturb the detection of organic acid, the degree of accuracy is low.The shortcoming of above analysis method,
As loaded down with trivial details in pretreatment process, accuracy and poor sensitivity and problem etc. that can not be completely quantitative, limit these methods in detection
Application in organic acid in grape wine and fruit wine.In addition although HPLC-MS/MS method can be used for measuring organic acid in fruits and vegetables, but
Have no report using the method that HPLC-MS/MS method measures organic acid in grape wine and/or fruit wine.Therefore, set up a kind of simple,
Quickly, accurately in detection grape wine and/or fruit wine organic acid method, for differentiate to blend littlefruit grape herb wine and fruit wine have important
Practical value.
Content of the invention
The purpose of the present invention is exactly to solve the above problems, providing one kind to utilize high performance liquid chromatography tandem mass spectrum method
The method simultaneously measuring four kinds of organic acids in grape wine and/or fruit wine.The method pre-treatment is simple, detection limit is low, selectivity is good,
Convenient, sensitivity and the degree of accuracy are high, can 4 kinds of organic acids in quick detection grape wine and/or fruit wine, differentiate to blend littlefruit grape herb wine
Or fruit wine, to the dining table of protection consumer, there is safely important using value and practical significance.
To achieve these goals, the present invention adopts the following technical scheme that：
The invention discloses high performance liquid chromatography-tandem mass (HPLC-MS/MS) internal standard method detection grape wine and/or
The application of organic acid in fruit wine.
A kind of high performance liquid chromatography-tandem mass (HPLC-MS/MS) internal standard method detects in grape wine and/or fruit wine simultaneously
The method of four kinds of organic acids, described four kinds of organic acids are tartaric acid, malic acid, butanedioic acid, citric acid.
Preferably, described internal standard method adopts toosendanin is internal standard compound, the study find that using toosendanin as internal standard, it is to four
Plant organic acid noiseless.
Further, the method comprising the steps of：
(1) prepare 4 kinds of organic acid standard liquids and carry out high performance liquid chromatography tandem mass spectrum mensure；
(2) linear relationship and detection limit and the quantitative limit of 4 kinds of organic acids are determined；
(3) pre-process grape wine and/or fruit wine sample and be measured；
(4) content of 4 kinds of organic acids is calculated according to sample detection data.
Preferably, the chromatographic determination condition of step (1) or (3) is：From Agilent Eclipse plus C18 (50 ×
4.6mm, 1.8 μm) chromatographic column, this chromatographic column good separating effect, each compound has reached baseline separation, and because this post is shorter,
Compound flows out comparatively fast, and retention time is short, ideal；
Mobile phase：A phase is 0.15% aqueous formic acid, and B phase is acetonitrile, and the addition of formic acid in the A phase aqueous solution have adjusted acid
Degree, is conducive to the separation of organic acid；Gradient elution program：Gradient elution：0～2.0min, A phase 100%；2.0-2.1min, A phase
100% → 50%, B phase 0 → 50%；2.1-5.0min, A phase each with B phase 50%；5.0-5.1min, A phase 50% → 0；Finally put down
Weighing apparatus 4.9min；
Flow velocity：0.6mL/min；Column temperature：20℃.
Tandem mass spectrum condition determination is：Ionization pattern：Electric spray ion source (ESI), drainage pattern：Reacting prison anion more
(MRM) pattern of survey, is dried gas：High-purity N2, temperature degree is dried：200-350 DEG C, dry gas stream speed：12L/min, atomizing pressure：
30psi, capillary voltage：4000V.
Preferably, under target components MRM pattern, mass spectral analysis parameter is as follows：
Further, described step (1) specifically includes following steps：A series of at least 6 kinds different qualities of accurate formulation are dense
Degree tartaric acid, malic acid, butanedioic acid, citric acid standard working solution, add internal standard compound standard liquid, sample introduction measure obtain
Standard spectrogram.
Further, step (2) specifically includes：The standard spectrogram that step (1) is obtained is respectively with 4 kinds of organic acids and internal standard
The peak area ratio of thing carries out linear regression to the two corresponding concentration proportion, obtains linear relationship regression equation, coefficient correlation
And the range of linearity；With the corresponding concentration of signal to noise ratio (S/N) >=3 as detection limit, the corresponding concentration in (S/N) >=10 is as quantitative limit.
Further, step (3) is specially：Accurately measure grape wine and/or fruit wine Sample Dilution, filter, sample introduction measures
Obtain sample spectrogram.
Further, described step (4) is specially：The sample spectrogram that step (3) is obtained is contrasted with standard spectrogram, qualitative
Determine the species of organic acid, substitute into the content that linear equation quantitatively calculates organic acid simultaneously.
In a kind of high performance liquid chromatography-tandem mass (HPLC-MS/MS) quick detection grape wine and/or fruit wine 4 kinds organic
The method of acid is differentiating the application of wine blend and fruit wine.
Beneficial effects of the present invention are：The present invention utilizes high performance liquid chromatography-tandem mass (HPLC-MS/MS) side first
Method detection grape wine and/or fruit wine and its tartaric acid, malic acid, butanedioic acid, 4 kinds of organic acids of citric acid.By optimize chromatogram and
Mass Spectrometer Method condition, makes 4 kinds of organic acids flow out from chromatographic column soon, retention time is short, realizes 4 kinds of sour quick separating, and
The chromatographic peak arriving is symmetrical, improves sensitivity and the degree of accuracy of detection；And the method detection sour to 4 kinds has higher selection
Property, all far below 4 kinds of sour contents in grape wine or fruit wine, the organic acid that can measure low concentration contains for detection limit and quantitative limit
Amount, has the advantages that test limit is low, can qualitative, quantitative accurately detect.
Detect that using the HPLC-MS/MS setting up the technology of 4 kinds of organic acids in grape wine and/or fruit wine is qualitative and quantitative
4 kinds of organic acids in detection grape wine and/or fruit wine, it is possible to authenticate wine blend or fruit wine.Eliminate base by adding internal standard
The impact of mass effect, detects that 4 kinds of organic acids can mutually assist discriminating wine blend or fruit wine, makes testing result more simultaneously
Accurately, and because HPLC-MS/MS technology carries out qualitative, quantitative using " double ion to ", it is to avoid the interference of endogenous material
With the possibility that false positive result of determination occurs.The method pre-treatment is simple and quick, process free of losses, and detection sensitivity is high, knot
Fruit accurately and reliably it is achieved that completing the Accurate Determining of 4 kinds of organic acids in 6 minutes, be quick discriminating blend littlefruit grape herb wine and fruit wine,
Protect the dining table safety of consumer and safeguard that Ko-ji insects sound development provides technical support.
Brief description
Fig. 1 is 4 kinds of organic acid typical case's MRM chromatograms；
Fig. 2 is the mass spectrometry parameters optimization figure of 4 kinds of organic acids, and A- optimizes fragmentation voltage, B- optimizing drying temperature degree；
Fig. 3 is 4 kinds of organic acid regression curves, A- tartaric acid, B- malic acid, C- citric acid, D- butanedioic acid.
Specific embodiment
The invention will be further described with embodiment below in conjunction with the accompanying drawings.
Instrument and reagent
Used in experiment, key instrument has：(Agilent is public for Agilent-1200 type quick separating high performance liquid chromatography
Department), 6410 types triplex tandem level Four bar mass spectrum (Agilent company).Acetonitrile (chromatographically pure, Tedia company), formic acid, DL- apple
Acid (purity is more than 99%) is purchased from Chengdu Ke Long chemical reagent factory, and tartaric acid, butanedioic acid (purity is more than 99.5%) are purchased from sky
Jinshi City's big cyclopentadienyl chemical reagent factory, monohydrate potassium (purity is more than 99.8%) recovers the limited public affairs of development in science and technology purchased from Tianjin
Department, toosendanin (internal standard IS, lot number 121464-201102) is purchased from National Institute for Food and Drugs Control.
Experimental technique
The process of sample
Accurately measure grape wine or fruit wine sample 0.1mL in clean 100mL volumetric flask, be diluted to scale, mistake with pure water
0.45 μm of filter membrane, to be measured.The multiple of dilution if measurement result exceeds the range of linearity, can be determined further according to the height of organic acid content
Afterwards, to be measured.
HPLC condition
Chromatographic column：(50mm × 4.6mm, 1.8 μm, U.S. Agilent is public for Agilent Eclipse plus C18 chromatographic column
Department).Mobile phase：A phase is 0.15% aqueous formic acid, and B phase is acetonitrile.Gradient elution：0～2.0min, A phase 100%；2.0-
2.1min, A phase 100% → 50%, B phase 0 → 50%；2.1-5.0min, A phase each with B phase 50%；5.0-5.1min, A phase 50%
→0；Finally balance 4.9min.Flow velocity：0.6mL/min.Column temperature：20 DEG C, sample size：10μL.
MS/MS condition
Ion gun：Electric spray ion source (ESI), using anion multiple-reaction monitoring (MRM) pattern, is dried gas：High-purity N2,
Temperature degree is dried：350 DEG C, dry gas stream speed：12L/min, atomizing pressure：30psi, capillary voltage：4000V.Other mass spectrums
Parameter is shown in Table 1.
Mass spectrometry parameters condition under table 1 target components MRM pattern
Chromatographic condition optimizes
When detecting the organic acid in grape wine using HPLC-MS/MS it is most important that selecting optimal chromatographic isolation bar
Part.These conditions include the type of chromatographic column, the pH value of mobile phase, flow velocity and column temperature etc..In the chromatographic column bar determining
Under part, the acid-base value of mobile phase, flow velocity are larger on the separation impact of post effect and chromatographic peak, the too low then disengaging time of flow velocity is long,
Post effect is poor；Column temperature also significantly affects post effect, and column temperature raises the viscosity that can reduce mobile phase and improves mass-transfer efficiency, but too high
Chromatographic column filler can be destroyed again, so the selection of chromatographic condition is considerably complicated, comprehensive numerous Consideration.
First chromatographic column is carried out selecting to investigate, hit and miss experiment Thermo Scientific BDS Hypersil
C18 chromatographic column (100 × 4.6mm, 3 μm, 1# post), Thermo Scientific HILIC XDB-C18 chromatographic column (100 ×
4.6mm, 3 μm, 2# post), 3 sections of chromatograms such as Agilent Eclipse plus C18 chromatographic column (50 × 4.6mm, 1.8 μm, 3# post)
Post.Find that bifurcated peak in malic acid and tartaric acid, and citric acid chromatographic peak drags when using 1# post and 2# post through overtesting
Tail.3# post under identical chromatographic conditions, good separating effect, each compound has reached baseline separation, and because this post is shorter, chemical combination
Logistics goes out comparatively fast, and retention time is short, ideal.
Secondly, the acid-base value of mobile phase, flow velocity and gradient are optimized.By detected object acidity relatively
By force, soluble in water, according to " similar mix " principle, add a certain amount of formic acid to adjust acidity in mobile phase and be conducive to organic acid
Separate, but mobile phase acidity Tai Gaoyi be lost chromatographic column and the detection that is unfavorable for mass spectrum anion, it was found that acetonitrile-
When 0.15% aqueous formic acid system is as mobile phase, chromatographic peak profile is symmetrical.And use mass spectrum ESI condition, the flow velocity of mobile phase
It is usually no more than 0.6mL/min, otherwise because the restriction of gasification and spray condition can greatly reduce sensitivity.100%
During 0.15% aqueous formic acid, tartaric acid is very fast with malic acid appearance, and retention time is respectively 1.01min and 1.38min, and lemon
Lemon acid and butanedioic acid retain relatively by force in the chromatography column, and appearance is slower, therefore on the premise of not affecting separating degree, improve rapidly second
Nitrile ratio, to 50%, makes citric acid quickly flow out with butanedioic acid.
Finally, chromatogram column temperature is optimized.20-60 DEG C of column temperature of setting (60 DEG C of chromatographic column highest tolerable temperature),
It was found that with the rising of temperature, all Compound Retention time shorten, but peak area does not have significant change, and separating degree
It is deteriorated, therefore following experiment adopts 20 DEG C of column temperature.Typical chromatogram is shown in Fig. 1.
MS/MS condition optimizing
Mass Spectrometer Method condition can make sample parent ion obtain maximum transmitted efficiency and daughter ion have in mass spectrum higher
Response intensity, directly affects detection sensitivity and the degree of accuracy, mainly includes to temperature degree, fragmentation voltage and collision energy are dried
Deng optimization.
First, respectively 4 kinds of organic acids are analyzed in scanning-mode it, determine respective molecular ion peak (parent ion)；
Secondly, under the pattern selecting ion detection (SIM), input sample m z, optimize fragmentation voltage
(Fragmentor, 0V～140V), it is ensured that the maximum transmitted efficiency of parent ion, reaches collision cell, specific experiment as far as possible
Result is shown in Fig. 2A；Again, under daughter ion scan pattern, the mass-to-charge ratio of parent ion and different collision energies (0V～40V) are inputted,
Investigate the different impacts to parent ion and daughter ion peak intensity for the collision energy, optimize collision energy during daughter ion maximum intensity,
Determine optimal daughter ion mass-to-charge ratio simultaneously；Finally, setting is dried 200 DEG C -350 DEG C of gas temperature range, investigates under MRM pattern
Temperature degree is dried, concrete outcome is shown in Fig. 2 B during good sensitivity.Test through above, determine optimal fragmentation voltage, collision energy
Parameter is as shown in table 1.The Mass Spectrometry Conditions reference of internal standard toosendanin《Chinese Pharmacopoeia one》(version in 2015) " Fructus meliae toosendan " kind
Regulation under " assay " item.
1.3 linear relationships and detection limit
Take appropriate tartaric acid, malic acid, butanedioic acid, citric acid standard liquid accurate formulation 0.25,0.5,1.0,2.0,
5.0th, a series of standard working solution of different quality concentration of 10.0 μ g/mL, adds toosendanin standard liquid so that its concentration is
2.0 μ g/mL, by above-mentioned condition, sample introduction measures respectively, with the quota ion peak area internal scalar quantity quasi-molecular ions face of 4 kinds of organic acids
Long-pending ratio is ordinate (Y), and with 4 kinds of organic acid concentrations and internal standard concentration ratio as abscissa, (X) carries out linear regression (linear graph is shown in
Fig. 3 A-D), obtain regression equation, coefficient correlation and the range of linearity；With the corresponding concentration of signal to noise ratio (S/N) >=3 as detection limit,
(S/N) >=10 corresponding concentration, as quantitative limit, obtain tartaric acid, malic acid, butanedioic acid, the detection limit of citric acid and quantitation
Limit, the results are shown in Table 2.As can be seen from the results, in the range of 0.25-10 μ g/mL, the regression coefficient of 4 kinds of organic acids is all higher than
0.99, linearly well, detection limit and quantitative limit, all far below the content in grape wine and fruit wine, therefore, it can by diluted sample
It is measured after product.
The linear equation of 2 four kinds of organic acids of table, the range of linearity, coefficient correlation, quantitative limit and detection limit
Embodiment 2
Wine blend or the discriminating of fruit wine：Using the detection method set up to 10 grape wine commercially
And analyzed after 1 Howthorn Wine sample step process by embodiment 2, measurement result is shown in Table 3.There it can be seen that
4 kinds of organic acids of 1-3# sample all have detection, and content range is 0.104～1.88g/L, and wherein citric acid content corresponds with correspondence
The national standard of execution《Grape wine》(GB 15037-2006)、《Wild grape wine》Maximum level in (GB/T 27586-2011)
Require (dry, half-dried, sweet half mould is not more than 1.0g/L, and sweet type is not more than 2.0g/L).Citric acid content model in other 7 samples
Enclose for 5.06～9.07g/L, exceed the corresponding execution standard that indicates and limit the quantity 2.5～7 times, do not detect tartaric acid, malic acid, amber
Acid, illustrates that product is not by fruit fermenting and producing, suspects for blending fake wine.Whether the method in order to verify foundation is accurate, and
Have detected 2 quality index such as total reducing sugar, sugar-free extract of 4～11# sample and 1 pigment that may illegally add is carmine, knot
Fruit shows that total reducing sugar, sugar-free extract index are not inconsistent standardization requirement yet, and have detected famille rose, further confirms that this 7 samples are
Fake wine.These results suggest that, the method for 4 kinds of organic acids of quick mensure that the present invention sets up is applied to discriminating wine blend and fruit
Wine.
Mensure (the unit of 4 kinds of organic acids in table 3 actual sample：g/L)
Note：N.D.- does not detect
Although the above-mentioned accompanying drawing that combines is described to the specific embodiment of the present invention, not model is protected to the present invention
The restriction enclosed, one of ordinary skill in the art should be understood that on the basis of technical scheme, and those skilled in the art are not
Need to pay the various modifications that creative work can make or deformation still within protection scope of the present invention.
Claims (10)
1. the application of high performance liquid chromatography-tandem mass internal standard method organic acid in detection grape wine and/or fruit wine.
2. a kind of high performance liquid chromatography-tandem mass internal standard method detection grape wine and/or fruit wine mesotartaric acid, malic acid, amber
Acid, the method for 4 kinds of organic acids of citric acid, is characterized in that, comprise the following steps：
(1) prepare 4 kinds of organic acid standard liquids and carry out high performance liquid chromatography tandem mass spectrum detection；
(2) linear relationship and detection limit and the quantitative limit of 4 kinds of organic acids are determined；
(3) pre-process grape wine and/or fruit wine sample and be measured；
(4) content of 4 kinds of organic acids is calculated according to sample detection data.
3. as claimed in claim 2 a kind of high performance liquid chromatography-tandem mass internal standard method detection grape wine and/or fruit wine in
The method of 4 kinds of organic acids, is characterized in that, it is internal standard compound that described internal standard method adopts toosendanin.
4. as claimed in claim 2 a kind of high performance liquid chromatography-tandem mass internal standard method detection grape wine and/or fruit wine in
The method of 4 kinds of organic acids, is characterized in that, the chromatographic determination condition of step (1) or (3) is：Chromatographic column：Agilent Eclipse
Plus C18,50 × 4.6mm, 1.8 μm；
Mobile phase A is the water containing 0.15% formic acid, and Mobile phase B is acetonitrile；Gradient elution program：Gradient elution：0～2.0min, A
Phase 100%；2.0-2.1min, A phase 100% → 50%, B phase 0 → 50%；2.1-5.0min, A phase each with B phase 50%；5.0-
5.1min, A phase 50% → 0；Finally balance 4.9min；
Flow velocity 0.6mL/min；Column temperature：20℃.
5. as claimed in claim 2 a kind of high performance liquid chromatography-tandem mass internal standard method detection grape wine and/or fruit wine in
The method of 4 kinds of organic acids, is characterized in that,
Mass spectroscopy condition is：Ionization pattern：Electric spray ion source,
Drainage pattern：Anion multiple-reaction monitoring pattern,
Gas is dried：High-purity N2, temperature degree is dried：200-350 DEG C,
Atomizing pressure：30psi, capillary voltage：4000V.
6. as claimed in claim 2 a kind of high performance liquid chromatography-tandem mass internal standard method detection grape wine and/or fruit wine in
The method of 4 kinds of organic acids, is characterized in that, described step (1) specifically includes following steps：Accurate formulation a series of at least 6 kinds not
Homogenous quantities concentration tartaric acid, malic acid, butanedioic acid, citric acid standard working solution, add internal standard compound standard liquid, sample introduction
Mensure obtains standard spectrogram.
7. as claimed in claim 2 a kind of high performance liquid chromatography-tandem mass internal standard method detection grape wine and/or fruit wine in
The method of 4 kinds of organic acids, is characterized in that, step (2) specifically includes：The standard spectrogram that step (1) is obtained is organic with 4 kinds respectively
Acid with the peak area ratio of internal standard compound, linear regression is carried out to the two corresponding concentration proportion, obtain linear relationship regression equation,
Coefficient correlation and the range of linearity；With the corresponding concentration in signal to noise ratio >=3 as detection limit, the corresponding concentration in signal to noise ratio >=10 is as quantitation
Limit.
8. as claimed in claim 2 a kind of high performance liquid chromatography-tandem mass internal standard method detection grape wine and/or fruit wine in
The method of 4 kinds of organic acids, is characterized in that, step (3) is specially：Accurately measure grape wine and/or fruit wine Sample Dilution, filter,
Sample introduction measures and obtains sample spectrogram.
9. as claimed in claim 2 a kind of high performance liquid chromatography-tandem mass internal standard method detection grape wine and/or fruit wine in
The method of 4 kinds of organic acids, is characterized in that, described step (4) is specially：The sample spectrogram that obtain step (3) and standard spectrogram
Contrast, the qualitative species determining organic acid, substitute into the content that linear equation quantitatively calculates organic acid simultaneously.
10. a kind of high performance liquid chromatography-tandem mass internal standard method as described in claim 2-9 any one is in detection grape wine
And/or in fruit wine 4 kinds of organic acids method in the application differentiating wine blend and fruit wine.
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| CN112175779A (en) * | 2020-09-24 | 2021-01-05 | 陕西科技大学 | White spirit based on ultrasonic wave and ultraviolet light synergistic ripening acceleration and ripening acceleration method and metabolic flux analysis method thereof |
| CN112175779B (en) * | 2020-09-24 | 2023-04-28 | 陕西科技大学 | White spirit ripening based on ultrasonic wave and ultraviolet light cooperation and ripening method and metabolic flow analysis method thereof |
| CN116879441A (en) * | 2023-07-13 | 2023-10-13 | 合肥工业大学 | Detection method for organic acid in food based on liquid chromatography-mass spectrometry |
| CN117451903A (en) * | 2023-12-25 | 2024-01-26 | 南京市食品药品监督检验院 | Method for simultaneously detecting 14 organic acids in fruit wine |
| CN117451903B (en) * | 2023-12-25 | 2024-02-23 | 南京市食品药品监督检验院 | Method for simultaneously detecting 14 organic acids in fruit wine |
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