CN108535395A - A method of using 32 kinds of free fatties in UPLC-QTof Rapid Simultaneous Determination health liquors - Google Patents
A method of using 32 kinds of free fatties in UPLC-QTof Rapid Simultaneous Determination health liquors Download PDFInfo
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Abstract
The invention discloses a kind of methods of 32 kinds of free fatties in QTof Rapid Simultaneous Determination health liquors using UPLC, wine sample to be measured closes chromatography using the ultra high efficiency equipped with QTof detectors after pre-treatment and is detected, obtain the chromatogram of sample to be tested, qualitative analysis is carried out according to selection ion to sample to be tested, quantitative analysis is then carried out to sample to be tested according to the standard curve of 32 kinds of free fatties.The method of the present invention is simple and quick, accurately and reliably, reproducible.
Description
Technical field
The present invention relates to a kind of method of 32 kinds of free fatties in Rapid Simultaneous Determination health liquor using UPLC-QTof,
Belong to detection and analysis technical field.
Background technology
Free fatty and the aliphatic acid for constituting complex lipid all play some key effects in metabolism --- as
Main metabolic fuel (storage and transport energy), the essential ingredient of all cell membranes and the gene regulation factor.In addition, meals
Lipid in food can provide polyunsaturated fatty acid, and this kind of aliphatic acid is that powerful local action metabolite (such as spend by class
Raw acid) precursor.Common plant and animal material aliphatic acid is even number chain, and every chain contains 16 to 24 carbon atoms, and is arrived with 0
6 double bonds.But always have countless exceptions in the Nature, practically even there is also the odd numbers of up to nearly 100 carbon atoms
Carbon and even-carbon fatty acid.In addition, double bond can be cis- (Z) and trans- (E) configuration, it is possible to have various other structures are special
Sign, including branch point, ring, oxygen-containing functional group etc..
It is a complicated job that free fatty (FFA) is detached from biomaterial, it is necessary to pay attention to preventing at any time or use up
Amount reduces the influence of hydrolase.After completing separation, aliphatic acid can be analyzed by typical chromatographic process, all be made at present
With Gas Chromatography-mass Spectrometry (GC/MS) and Liquid Chromatography-Tandem Mass Spectrometry (LC/MS/MS).But these methods suffer from respectively
From shortcoming.For example, GC methods need to perform the derivatization in aliphatic acid, to hydrolyze and be converted into methyl esters, this process is not
It only takes, and there is also the risks that aliphatic acid is reset during derivatization so that can not determine that the ester of formation is to come from FFA
Or complete complex lipid.In addition, for high molecular weight (>C24 for low volatility very-long-chain fatty acid), even if
After fatty acid methyl ester (FAME) derivatization, GC/MS analyses still remain problem.In LC/MS methods, although need not be into
Row sample derivatization, but the sample preparation procedure before operation is time-consuming and laborious, and the toxic organic solvent used is expensive, place
Reason expense is also very high.And in typical reverse phase (RP) LC/MS analyses, then it must will be steamed containing the organic extract of all lipids
It is dry, it reuses the better sample introduction solvent of compatibility and is redissolved.In consideration of it, a kind of easy, quick, cheap Separation of Fatty Acids and
Assay method is extremely urgent.
Invention content
In order to avoid above-mentioned existing deficiencies in the technology, the present invention is intended to provide a kind of using UPLC-QTof
The method of 32 kinds of free fatties in Rapid Simultaneous Determination health liquor.32 kinds of free fatties of the present invention be butyric acid, caproic acid,
Octanoic acid, capric acid, hendecanoic acid, lauric acid, tridecanoic acid, myristic acid, pentadecanoic acid, palmitic acid, Heptadecanoic acide, stearic acid,
Arachidic acid, behenic acid, physeteric acid, palmitoleic acid, 10- heptadecenoic acids, gamma-Linolenic acid, leukotrienes, linoleic acid, oleic acid, anti-oil
Acid, arachidonic acid, homologous gamma-Linolenic acid, 11-14-17- eicosatrienoic acids, 11-14- eicosadienoic acids, 11- 20
Carbon enoic acid, docosahexaenoic acid, two dodecadienoic acids, erucic acid and nervonic acid.The method of the present invention is a kind of quick, high pass
Amount is detached with efficient FFA and analysis method, uses the ultra high efficiency with mass spectral analysis and closes phase chromatography (UPC2), can be to protect
The accurate judgement, quick detection of free fatyy acids provide scientific basis in strong wine.
The method that the present invention uses 32 kinds of free fatties in UPLC-QTof Rapid Simultaneous Determination health liquors, including it is as follows
Step：
Step 1：Pre-treatment
20~50mL wine samples to be measured are measured in 50mL plastic centrifuge tubes, ethyl alcohol is removed using nitrogen evaporator, wait for that Liquid Residue is surplus
Remaining 1~2ml when stop nitrogen and blow, the Liquid Residue after alcohol will be gone to be transferred in 5mL volumetric flasks, with dichloromethane constant volume, through 0.22 μm
Syringe filter filters, and obtains sample to be tested；
Step 2：The drafting of standard curve
Take 32 kinds of mixing standard liquid (FFA correct mixtures：The saturation FFA standard items of various C8 containing even number of carbon atoms to C24
Purchased from Sigma companies；The complex model mixture of different FFA standard items (GLC-85, FFA form) is purchased from Nu-Chek Prep)
It is prepared with chloroform and obtains 1mg/mL storing solutions, then diluted with chloroform and obtain 0.1mg/mL work mixed solution (32 kinds of free fat
The concentration of fat acid is 0.1mg/mL)；The hybrid standard work that gained work mixed solution obtains various concentration is diluted with chloroform
Solution closes chromatography using the ultra high efficiency equipped with QTof detectors and is detected, corresponding to its institute with the peak area of determinand
Mass concentration carry out linear regression, the equation of linear regression of 32 kinds of free fatties is obtained, corresponding to each equation of linear regression
Curve, the standard curve of as corresponding free fatty；
It is dense to obtain 5 differences by a concentration of 5~1000ng/mL of hybrid standard working solution described in step 2, at least dilution
The point value of degree.
Detection parameters setting in step 2 is as follows：
The testing conditions setting that ultra high efficiency closes chromatography is as follows：
Chromatographic column is 2.1x 150mm, 1.8 μm of HSS C18SB chromatographic columns；
Column temperature is 3~50 DEG C；
Sample room temperature is 10~20 DEG C
Mobile phase：A phases are carbon dioxide, and B phases are 0.1% formic acid solution of methanol；
Flow velocity is 0.2~0.5mL/min；
Type of elution is gradient elution；Parameters of gradient elution is set as：When 0min, the volume fraction of Mobile phase B is 5~
10%；By 0min to 5.0min, the volume fraction of Mobile phase B rises to 20~25% from 5~10%；By 5.0min to 5.1min,
The volume fraction of Mobile phase B rises to 40~50% from 20~25%, keeps to 6.0min；By 6.0min to 8.0min, Mobile phase B
Volume fraction be down to 5~10% from 40~50%, and keep balance 1min.
Sample size is 0.5~5 μ L；
Detection time is 3~8min；
Compensate liquid：Methanol (contains 0.1% ammonium hydroxide), 0.20~0.6mL/min of flow velocity；
Current divider：Four-way (1/16 PEEK pipes)；
The testing conditions setting of MS is as follows：
Mass spectrograph：QTof
Ionization pattern：ESI-
Capillary voltage：1.0KV
Orifice potential：30V
Source temperature：100℃
Desolventizing stripping temperature：500℃
Taper hole gas flow rate：10L/h
Desolventizing steam flow speed：600L/h
Acquisition range：50-600m/Z
Neutral mass number and mass number see the table below shown in 1：
Table 1：32 kinds of free fatty mass numbers and corresponding retention time
Step 3：The detection of wine sample to be measured
1.0~the 2.0mL of sample to be tested for taking step 1 to obtain, is detected by the testing conditions of step 2, and acquisition waits for test sample
The chromatogram of product carries out qualitative analysis to sample to be tested according to selection ion, then bent according to the standard of 32 kinds of free fatties
Line carries out quantitative analysis to sample to be tested.
When carrying out sample comparison by multivariate data analysis, key is to make each sample randomization and at least sample introduction three
It is secondary, to ensure that data analysis is statistically effective.For this research, acquired under MSE patterns in each health liquor
Five repetition sample introductions, which is a kind of agonic Tof acquisition methods, wherein mass spectrograph is touched low when carrying out mixed sweep
It hits and switches between energy and high collision energy.Using TransOmics metabolism group and lipidomics informatics software
(TransOmics Informatics for Metabolomics and Lipidomics, TOIML) carry out data analysis and
FFA is identified.
Following sensitivity test is made to the method for the present invention：Sensitivity test include instrument sensitivity and method it is sensitive
Degree, the detection limit of the sensitivity instrument of instrument indicates, takes the minimum of the mixed standard solution of the free fatty of signal-to-noise ratio >=3
A concentration of instrument detection limit；The quantitative limit of the sensitivity of method method indicates, the free fatty of signal-to-noise ratio >=9 is taken to mix mark
The Cmin of quasi- solution is method quantitative limit.The related data of gained see the table below 2.
Following accuracy and reproducibility experiment are made to the method for the present invention：The same wine sample is selected to be used as blank after pre-treatment
Sample is divided into 3 parts, is separately added into hybrid standard working solution and carries out recovery testu, calculates the rate of recovery；Choose 1 wine sample
Product according to same pre-treating method handle 6, tested respectively, by calculate the range of its relative standard deviation (RSD) come
The reproducibility of discriminatory analysis method.The accuracy of method is indicated with the rate of recovery, is shown in Table 3, the reproducibility of method uses relative standard
Deviation (RSD) indicates, is shown in Table 4.It can be seen that the rate of recovery is in 80~120%, RSD ＜ 10%.
Table 3：The recovery of standard addition experiment of 32 kinds of free fatties
Table 4：The reproducibility experiment of 32 kinds of free fatties
Beneficial effects of the present invention are embodied in：
1, the present invention establishes a kind of side of 32 kinds of free fatties in the Rapid Simultaneous Determination health liquor using UPC2-QTof
Method, can be accurately qualitative, quantitative to 32 kinds of free fatties progress in health liquor, sentences for the accurate of free fatty in wine
Fixed, quick detection provides scientific basis.
2, it is simple and quick, accurate and reliable, repeated to close phase chromatography concatenation QTof mass detectors for ultra high efficiency of the present invention
It is good.
3,2.1x 150mm of the present invention, 1.8 μm of HSS C18SB close phase chromatographic column specially and CO2With methanol as mobile phase
Selection has reached excellent separating effect to 32 kinds of free fatties in wine.
4, the present invention is not necessarily to derivatization, it can be achieved that more simple and quick sample preparation, avoids interfering.
5, extractive with organic solvent can save the time analyzed every time and cost in direct injected to system
6, chromatographic isolation, fast 10 times of speed ratio GC/MS can be completed in three minutes in the present invention.And smaller using toxicity,
More economic CO2As solvent.Faster speed can efficiently analyze larger sample size, to improve the entirety of experiment
Efficiency.
7, detection method of the invention is environmentally friendly " green " technology.The main mobile phase titanium dioxide used in analysis
Carbon comes from the recycling carbon dioxide of other industry releases, and the carbon dioxide used in experiment will not generate new greenhouse gas again
Body.When using the method, the modifying agent (methanol) that each sample introduction is consumed is only 0.9~1.0mL, with similar detection method phase
Than reducing 150~200% organic solvent usage amount.
8, the present invention also has an important feature, is capable of the isomers of separation detection lipid.
9, the present invention can be cost-effective by reducing the use of laboratory consumable.
Description of the drawings
Fig. 1 is the chromatogram of 32 kinds of free fatty standard working solutions.
Specific implementation mode
With reference to specific embodiment, technical solution of the present invention is further elaborated.
The present embodiment is as follows measured 32 kinds of free fatties in certain wine：
1, pre-treatment
Measure 25mL wine samples to be measured in 50mL plastic centrifuge tubes, using nitrogen evaporator remove ethyl alcohol, wait for Liquid Residue residue 1~
Stop nitrogen when 2ml to blow, the Liquid Residue after alcohol will be gone to be transferred in 5mL volumetric flasks, with dichloromethane constant volume, through 0.22 μm of pin type mistake
Filter filters, and obtains sample to be tested；
2, detection parameters are arranged
The testing conditions setting that ultra high efficiency closes chromatography is as follows：
Chromatographic column is 2.1x 150mm, 1.8 μm of HSS C18SB chromatographic columns；
Column temperature is 50 DEG C；
Sample room temperature is 10 DEG C；
Mobile phase：A phases are carbon dioxide, and B phases are 0.1% formic acid solution of methanol；
Flow velocity is 0.23mL/min；
Type of elution is gradient elution；Elution program is as follows：When 0min, the volume fraction of Mobile phase B is 5%；By 0min
Volume fraction to 5.0min, Mobile phase B rises to 25% from 5%；By 5.0min to 5.1min, the volume fraction of Mobile phase B from
25% rises to 50%, keeps to 6.0min；By 6.0min to 8.0min, the volume fraction of Mobile phase B is down to 5% from 50%, and
Keep balance 1min.Specifically, the change curve in gradient elution each stage selects the curve 6 in instrument.
Sample size is 0.5 μ L；
Detection time is 8min；
Compensate liquid：Methanol (contains 0.1% ammonium hydroxide), flow velocity 0.20mL/min；
Current divider：Four-way (1/16 PEEK pipes)；
The testing conditions setting of MS is as follows：
Mass spectrograph：QTof
Ionization pattern：ESI-
Capillary voltage：1.0KV
Orifice potential：30V
Source temperature：100℃
Desolventizing stripping temperature：500℃
Taper hole gas flow rate：10L/h
Desolventizing steam flow speed：600L/h
Acquisition range：50-600m/Z
Neutral mass number and mass number see the above table 1.
3, the drafting of standard curve
Take 32 kinds of mixing standard liquid (FFA correct mixtures：The saturation FFA standard items of various C8 containing even number of carbon atoms to C24
Purchased from Sigma companies；The complex model mixture of different FFA standard items (GLC-85, FFA form) is purchased from Nu-Chek Prep)
It is prepared with chloroform and obtains 1mg/mL storing solutions, then diluted with chloroform and obtain 0.1mg/mL work mixed solution (32 kinds of free fat
The concentration of fat acid is 0.1mg/mL)；The hybrid standard work that gained work mixed solution obtains various concentration is diluted with chloroform
Solution closes chromatography using the ultra high efficiency equipped with QTof detectors and is detected, corresponding to its institute with the peak area of determinand
Mass concentration carry out linear regression, the equation of linear regression of 32 kinds of free fatties is obtained, corresponding to each equation of linear regression
Curve, the standard curve of as corresponding free fatty；
The concentration of the hybrid standard working solution be respectively 5ng/ml, 50ng/ml, 200ng/ml, 500ng/ml,
1000ng/ml。
The corresponding equation of linear regression of 32 kinds of free fatties and correlation coefficient r2It see the table below 2.
Table 2：The equation of linear regression of 32 kinds of free fatties, related coefficient, detection limit, quantitative limit
4, the detection of wine sample to be measured
1.0~the 2.0mL of sample to be tested for taking step 1 to obtain, is detected by the testing conditions of step 2, and acquisition waits for test sample
The chromatogram of product carries out qualitative analysis to sample to be tested according to selection ion, then bent according to the standard of 32 kinds of free fatties
Line carries out quantitative analysis to sample to be tested.
When carrying out sample comparison by multivariate data analysis, key is to make each sample randomization and at least sample introduction three
It is secondary, to ensure that data analysis is statistically effective.For this research, acquired under MSE patterns in each health liquor
Five repetition sample introductions, which is a kind of agonic Tof acquisition methods, wherein mass spectrograph is touched low when carrying out mixed sweep
It hits and switches between energy and high collision energy.Using TransOmics metabolism group and lipidomics informatics software
(TransOmics Informatics for Metabolomics and Lipidomics, TOIML) carry out data analysis and
FFA is identified.
The detection data of 5 this method of table and existing method detection data correction data
It can be seen from the data in Table 5 that the same sample using existing method compared with this method, existing method needs
32 kinds of aliphatic acid could being detected completely using 8 kinds of methods, and detection limit is higher, many trace constituents cannot detect,
And this 32 kinds of aliphatic acid can be detected simultaneously using this method, and the detection limit of this method is relatively low, can be detected using this method
The content that can't detect to existing method, the content more than two methods detection limit be able to detect that using both of which,
The data of two methods detection can absolutely prove this method better than existing in rational error range, by detection data
Method can accurately quantify 32 kinds of aliphatic acid in health liquor.
Claims (5)
1. a kind of method of 32 kinds of free fatties in Rapid Simultaneous Determination health liquor using UPLC-QTof, it is characterised in that packet
Include following steps：
Step 1：Pre-treatment
Measure 20~50mL wine samples to be measured in 50mL plastic centrifuge tubes, using nitrogen evaporator remove ethyl alcohol, wait for Liquid Residue residue 1~
Stop nitrogen when 2ml to blow, the Liquid Residue after alcohol will be gone to be transferred in 5mL volumetric flasks, with dichloromethane constant volume, through 0.22 μm of pin type mistake
Filter filters, and obtains sample to be tested；
Step 2：The drafting of standard curve
It takes 32 kinds of mixing standard liquids to prepare the storing solution for obtaining 1mg/mL with chloroform respectively, is then diluted with chloroform and obtain 0.1mg/mL
Work mixed solution；With chloroform dilute gained work mixed solution obtain various concentration hybrid standard working solution, using with
There is the ultra high efficiency of QTof detectors to close chromatography to be detected, with the peak area of determinand to its corresponding mass concentration of institute into
Row linear regression obtains the equation of linear regression of 32 kinds of free fatties, the curve corresponding to each equation of linear regression, as phase
Answer the standard curve of free fatty；
Step 3：The detection of wine sample to be measured
1.0~the 2.0mL of sample to be tested for taking step 1 to obtain, is detected by the testing conditions of step 2, obtains sample to be tested
Chromatogram carries out qualitative analysis, then according to the standard curve pair of 32 kinds of free fatties to sample to be tested according to selection ion
Sample to be tested carries out quantitative analysis.
2. according to the method described in claim 1, it is characterized in that：
In step 2, a concentration of 5~1000ng/mL of the hybrid standard working solution, at least dilution obtain 5 various concentrations
Point value.
3. according to the method described in claim 1, it is characterized in that：
In step 2, the testing conditions setting that ultra high efficiency closes chromatography is as follows：
Chromatographic column is 2.1x150mm, 1.8 μm of HSS C18SB chromatographic columns；
Column temperature is 3~50 DEG C；
Sample room temperature is 10~20 DEG C
Mobile phase：A phases are carbon dioxide, and B phases are 0.1% formic acid solution of methanol；
Flow velocity is 0.2~0.5mL/min；
Type of elution is gradient elution；
Sample size is 0.5~5 μ L；
Detection time is 3~8min；
Compensate liquid：Methanol containing 0.1% ammonium hydroxide, 0.20~0.6mL/min of flow velocity；
Current divider：1/16 PEEK four-way pipes.
4. according to the method described in claim 3, it is characterized in that：
Parameters of gradient elution is set as：When 0min, the volume fraction of Mobile phase B is 5~10%；By 0min to 5.0min, flowing
The volume fraction of phase B rises to 20~25% from 5~10%；By 5.0min to 5.1min, the volume fraction of Mobile phase B from 20~
25% rises to 40~50%, keeps to 6.0min；By 6.0min to 8.0min, the volume fraction of Mobile phase B is dropped from 40~50%
To 5~10%, and keep balance 1min.
5. according to the method described in claim 1, it is characterized in that：
In step 2, the testing conditions setting of MS is as follows：
Mass spectrograph：QTof
Ionization pattern：ESI-
Capillary voltage：1.0KV
Orifice potential：30V
Source temperature：100℃
Desolventizing stripping temperature：500℃
Taper hole gas flow rate：10L/h
Desolventizing steam flow speed：600L/h
Acquisition range：50-600m/Z.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112147252A (en) * | 2020-09-25 | 2020-12-29 | 安徽瑞思威尔科技有限公司 | UPC2-PDA-Q-Tof/MS detection method for 39 effective components in pseudo-ginseng wine |
| CN112147253A (en) * | 2020-09-25 | 2020-12-29 | 安徽瑞思威尔科技有限公司 | UPC2-PDA-Q-Tof/MS detection method for 42 effective components in ganoderma lucidum wine |
| 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 |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20020192264A1 (en) * | 2000-09-01 | 2002-12-19 | Zemel Michael B. | Materials and methods for the treatment or prevention of obesity |
| CN102539609A (en) * | 2011-12-31 | 2012-07-04 | 青岛啤酒股份有限公司 | Detection method for measuring free fatty acid in beer through methyl esterification in bottle-headspace SPME (solid-phase micro-extraction)-gas chromatography and mass spectrum |
| CN104297381A (en) * | 2014-11-05 | 2015-01-21 | 光明乳业股份有限公司 | Determination method of free medium-chain fatty acid |
| CN105241968A (en) * | 2015-08-31 | 2016-01-13 | 广州金域医学检验中心有限公司 | Method of quickly detecting fatty acid in whole blood red cell |
| CN105866302A (en) * | 2016-06-17 | 2016-08-17 | 安徽古井贡酒股份有限公司 | Method for utilizing ultra-effective bonded phase chromatography to serially connect QDa while quickly detecting seven biogenic amines in white spirit |
| CN105891375A (en) * | 2016-06-17 | 2016-08-24 | 安徽瑞思威尔科技有限公司 | Method using ultra-performance convergence chromatography to fast detect chiral ethyl lactate in Baijiu |
| CN107367468A (en) * | 2017-08-03 | 2017-11-21 | 北京师范大学 | A kind of free fatty acid determination method in edible oil |
| CN107607666A (en) * | 2017-10-12 | 2018-01-19 | 福建省医学科学研究院 | The detection method of organic acid in a kind of biological sample |
-
2018
- 2018-03-12 CN CN201810201947.7A patent/CN108535395B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20020192264A1 (en) * | 2000-09-01 | 2002-12-19 | Zemel Michael B. | Materials and methods for the treatment or prevention of obesity |
| CN102539609A (en) * | 2011-12-31 | 2012-07-04 | 青岛啤酒股份有限公司 | Detection method for measuring free fatty acid in beer through methyl esterification in bottle-headspace SPME (solid-phase micro-extraction)-gas chromatography and mass spectrum |
| CN104297381A (en) * | 2014-11-05 | 2015-01-21 | 光明乳业股份有限公司 | Determination method of free medium-chain fatty acid |
| CN105241968A (en) * | 2015-08-31 | 2016-01-13 | 广州金域医学检验中心有限公司 | Method of quickly detecting fatty acid in whole blood red cell |
| CN105866302A (en) * | 2016-06-17 | 2016-08-17 | 安徽古井贡酒股份有限公司 | Method for utilizing ultra-effective bonded phase chromatography to serially connect QDa while quickly detecting seven biogenic amines in white spirit |
| CN105891375A (en) * | 2016-06-17 | 2016-08-24 | 安徽瑞思威尔科技有限公司 | Method using ultra-performance convergence chromatography to fast detect chiral ethyl lactate in Baijiu |
| CN107367468A (en) * | 2017-08-03 | 2017-11-21 | 北京师范大学 | A kind of free fatty acid determination method in edible oil |
| CN107607666A (en) * | 2017-10-12 | 2018-01-19 | 福建省医学科学研究院 | The detection method of organic acid in a kind of biological sample |
Non-Patent Citations (2)
| Title |
|---|
| 渠淑萍: "超临界流体色谱-质谱在游离脂肪酸及变压器油氧化产物分离检测中的应用研究", 《中国优秀硕士学位论文全文数据库》 * |
| 渠淑萍等: "超高效合相色谱一串联质谱测定地沟油中的游离脂肪酸", 《分析试验室》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN112147252A (en) * | 2020-09-25 | 2020-12-29 | 安徽瑞思威尔科技有限公司 | UPC2-PDA-Q-Tof/MS detection method for 39 effective components in pseudo-ginseng wine |
| CN112147253A (en) * | 2020-09-25 | 2020-12-29 | 安徽瑞思威尔科技有限公司 | UPC2-PDA-Q-Tof/MS detection method for 42 effective components in ganoderma lucidum wine |
| CN112147253B (en) * | 2020-09-25 | 2022-04-01 | 安徽瑞思威尔科技有限公司 | UPC2-PDA-Q-Tof/MS detection method for 42 effective components in ganoderma lucidum wine |
| CN112147252B (en) * | 2020-09-25 | 2022-04-19 | 安徽瑞思威尔科技有限公司 | UPC2-PDA-Q-Tof/MS detection method for 39 effective components in pseudo-ginseng wine |
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