CN107655988A - A kind of method for detecting ketose and amino sugar simultaneously using gaschromatographic mass spectrometric analysis method - Google Patents
A kind of method for detecting ketose and amino sugar simultaneously using gaschromatographic mass spectrometric analysis method Download PDFInfo
- Publication number
- CN107655988A CN107655988A CN201710813087.8A CN201710813087A CN107655988A CN 107655988 A CN107655988 A CN 107655988A CN 201710813087 A CN201710813087 A CN 201710813087A CN 107655988 A CN107655988 A CN 107655988A
- Authority
- CN
- China
- Prior art keywords
- monose
- ketose
- amino sugar
- solution
- sugar
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- 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
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The invention discloses a kind of method for detecting ketose and amino sugar simultaneously using gaschromatographic mass spectrometric analysis method.This method carries out Thiolation and silicon etherificate to the ketose in sample and mixing monose standard solution and amino sugar by ethyl mercaptan trifluoroacetic acid and HMDS trimethyl silane system and derived, reaction product is after dichloromethane or chloroform extraction, organic layer is detected by GC MS, with the ratio between the peak area of the mixing monose standard solution of various concentrations and internal standard peak area for ordinate, standard curve is established as abscissa using the concentration of every kind of monose, with the content of monose in inner mark method ration sample solution.This method has the advantages that specificity is strong, reproducible, separating degree is good, reliable results, it is possible to achieve detection to ketose in Chinese medicine and amino sugar and quantitative.In addition, this method also can detect glucuronic acid, galacturonic acid, glucose, galactolipin, mannose, rhamnose, fucose, arabinose and xylose.
Description
Technical field
It is more particularly to a kind of to utilize gas chromatography-mass spectrum point the present invention relates to a kind of method for detecting ketose and amino sugar
The method that analysis method detects ketose and amino sugar simultaneously.The invention belongs to chemical analysis and detection technique field.
Background technology
GC-MS (Gas Chromatograph-Mass Spectrometer), it is gas-chromatography and mass spectrometric hyphenated technique.
GC-MS makes the chemical group of complexity can be separated by the use of gas-chromatography as mass spectrographic sampling system；Inspection is used as by the use of mass spectrograph
Survey device and carry out qualitative and quantitative analysis.Test sample is separated into one-component through GC, same with carrier gas by its different retention time
When flow out chromatographic column, by molecular separator interface, remove carrier gas, retained fraction is ionized into MS instrument ion guns, sample
Constitutional changes are ion, are detected through analysis, are recorded as MS figures.Gas chromatograph is equivalent to mass spectrograph sampling system in GC-MS, and
Mass spectrograph is then the detector of gas-chromatography, is organically combined the two by interface.It is indiscriminate that GC-MS methods have been widely used in medicine
With the internal Pharmaceutical Analysis such as monitoring, drug-testing, clinical disease diagnosis, pharmacokinetic studies.
Although disclosing GC-MS detection methods in the prior art passes through ethyl mercaptan-trifluoroacetic acid and HMDS-three
Methyl-monosilane system derives to monose and uronic acid.But this method is not applied to amino sugar and ketose at present.
The present invention first using ethyl mercaptan-trifluoroacetic acid and HMDS-trimethyl silane system to ketose and
Amino sugar is derived, GC-MS detections, and derivative reagent condition is optimized by single factor exploration experiment.And should
Method is applied to the detection of free ketose and amino sugar in Chinese medicine, is the further further investigation based theoretical of Chinese medicine.
The content of the invention
It is same by using gas chromatography-mass spectrometry analysis method (GC-MS detection methods) it is an object of the invention to provide one kind
When detect saccharon sugar and amino sugar method.
In order to achieve the above object, present invention employs following technological means：
A kind of method for detecting ketose and amino sugar simultaneously using gas chromatography-mass spectrometry analysis method of the present invention, the party
Method is by ethyl mercaptan-trifluoroacetic acid and HMDS-trimethyl silane system to sample and mixing monose standard items
Monose in solution carries out Thiolation and silicon etherificate and derived, and ethyl mercaptan-silicon etherificate that ketose and amino sugar is prepared derives
Product, for reaction product after dichloromethane or chloroform extraction, organic layer passes through gas chromatography-mass spectrometry analysis method (GC-
MS) detected, with the ratio between the peak area of the mixing monose standard solution of various concentrations and internal standard peak area for ordinate, with
The concentration of every kind of monose be abscissa establish standard curve, with the ketose in inner mark method ration sample solution and amino sugar and other
The content of monose, a kind of ketose and a kind of amino sugar are comprised at least in described mixing monose standard solution.
Reaction product after derivative extracts through dichloromethane or chloroform soln, and organic layer, which contains, to be detected by GC-MS
Ketose and amino sugar ethyl mercaptan-silicon etherificate derivative products, therefore the undetectable amino sugar of existing method can be detected.
Wherein, it is preferred that the chromatographic condition of described gas chromatography-mass spectrum is：Using Agilent 7890A-5975C gas
Matter combined instrument, using DB-5 capillary columns, temperature programming, 80 DEG C of column temperature, with 2.5 DEG C/min to 190 DEG C, with 2 DEG C/min to 252
DEG C, with 250 DEG C/min to 300 DEG C, helium makees carrier gas, 250 DEG C of injector temperature, column flow rate 1.2mL/min, EI (70eV), connects
250 DEG C of temperature of mouth, 230 DEG C of ion source temperature, scanning range:M/z50-550, scan rate:2.5scan/s.
Wherein, it is preferred that by ethyl mercaptan-trifluoroacetic acid and HMDS-trimethyl silane system to ketose
Carrying out concrete operation step derived from Thiolation and silicon etherificate with amino sugar is：Measure the sample solution of same volume and mix
Monose standard solution is closed, is concentrated to dryness respectively, adds the mixed solution of ethyl mercaptan and trifluoroacetic acid, 20-25 DEG C of sealing is carried out
Thiolation reaction 10-50min, volatilize naturally in fume hood；Pyridinium dissolution is added, adds HMDS and front three
Base chlorosilane, 50-90 DEG C of water-bath, silicon etherification reaction 10-50min is carried out, after reaction, add the water of dichloromethane or chloroform
Solution, vibrate, centrifugation, remove a layer organic layer solution, can directly carry out gas chromatography-mass spectrometry analysis.
Wherein, it is preferred that the time of Thiolation reaction is 10min.
Wherein, it is preferred that the volume ratio of ethyl mercaptan and trifluoroacetic acid is 2:1.
Wherein, it is preferred that the volume ratio of HMDS and trim,ethylchlorosilane is 3:1.
Wherein, it is preferred that after adding HMDS and trim,ethylchlorosilane, 70 DEG C of water-baths, it is anti-to carry out silicon etherificate
Answer 30min.
Wherein, it is preferred that be designated as erythrite in described.
Wherein, it is preferred that neutral sugar and/or uronic acid are also included in described mixing monose standard solution；Described
Other monose include neutral sugar and/or uronic acid.
Compared to prior art, the beneficial effects of the invention are as follows：
(1) present invention improves over existing deriving method, and derivatization conditions have been carried out with the optimization of single factor test, sample passes through
Ethyl mercaptan-trifluoroacetic acid and HMDS-trimethyl silane system derive to ketose and amino sugar, reaction product
Through dichloromethane or chloroform extraction, organic layer, which contains, to be etherified by ethyl mercaptan-silicon of the GC-MS ketoses detected and amino sugar
Derivative products, therefore the unmeasured amino sugar of existing method is can detect that, and the detection of ketose and amino sugar, lack always special
The method of attribute.
(2) present invention uses gas chromatography-mass spectrography (GC-MS) technology, and the n-alkane in applied analysis thing is to list
Sugared retention index (RI) is determined, it was confirmed that retention index can do good qualitative analysis to ketose and amino sugar.
(3) method of the invention also can detect neutral sugar and uronic acid, construct powerful a variety of monose composition detection side
Method.Every kind of monose is the chromatogram main peak of single high response, with specificity is strong, reproducible, separating degree is good, reliable results etc.
Advantage.
(4) the inventive method can realize detection to ketose in Chinese medicine and amino sugar and quantitative, can be used for simultaneously
Detect the ketose to dissociate in Chinese medicine.In addition, this method also can detect neutral sugar and uronic acid, such as glucuronic acid, galactolipin
Aldehydic acid, glucose, galactolipin, mannose, rhamnose, fucose, arabinose and xylose.
Brief description of the drawings
Fig. 1 is influence of the Thiolation derivatization reaction time to peak area；
Fig. 2 is influence of the Thiolation derivative reagent total amount to peak area；
Fig. 3 is that silicon is etherified influence of the derivative reagent reaction temperature to peak area；
Fig. 4 is that silicon is etherified influence of the derivative reagent dosage to peak area；
Fig. 5 is standard items GC-MS chromatograms (no dichloromethane/chloroform extraction)；
Fig. 6 is standard items GC-MS chromatograms (dichloromethane/chloroform extraction)；
Fig. 7 is sample GC-MS chromatograms.
Embodiment
Below by embodiment the present invention is described further checking, all embodiments be only used for illustration the present invention,
Do not limit the scope of the invention.Those skilled in the art know the change or equivalent for being done in the claims in the present invention
Change, each falls within protection scope of the present invention.
Embodiment 1 detects the foundation of the GC-MS methods of saccharon sugar and amino sugar
1. instrument and reagent
Agilent7890A-5975C gas chromatograph-mass spectrometers, it is equipped with DB-5 capillary columns (60m × 0.25mm × 0.25 μm)；Mark
Quasi- monose：(sigma is public for fructose (Fru), Glucosamine (GlcN), amine-galactose (GalN), epichitosamine (ManN)
Department)；Wind-weed purified polysaccharide (this laboratory extraction purification)；HMDS (tries a chemical reagent Co., Ltd in Shanghai)；
Trim,ethylchlorosilane (Solution on Chemical Reagents in Shanghai purchase and supply 5-linked chemical plant)；(the limited public affairs of development in science and technology are recovered in Tianjin to pyridine
Department)；Trifluoroacetic acid (Tianjin recovery fine chemistry industry research institute)；Ethyl mercaptan (Shijiazhuang Ji Shi Chemical Co., Ltd.s)；Erythrite
(Beijing Suo Laibao Science and Technology Ltd).
2. experimental method and result
The optimization of 2.2 experimental methods
2.2.1 literature method prepares solution
Precision weighs four kinds of standard monose samples, each 3mg, adds the dissolving of 1mL water.100 μ L mixed solutions are taken, nitrogen blows
It is dry.Add the mixed solution (volume ratio 2 of 100 μ L ethyl mercaptans and trifluoroacetic acid:1), room temperature, sealing, carries out Thiolation reaction
10min, nitrogen drying.100 μ L pyridinium dissolutions are added, add 132 μ L HMDSs and 44 μ L trim,ethylchlorosilanes
Reagent, 70 DEG C of water-baths, carry out silicon etherification reaction 30min.After reaction, 100 μ L water are added, are vibrated, centrifugation, take upper solution, can
Directly carry out gas chromatographic analysis.
2.2.2 improved method prepares solution
Precision weighs four kinds of standard monose samples, each 3mg, adds the dissolving of 1mL water.100 μ L mixed solutions are taken, are concentrated into
It is dry.Add the mixed solution (volume ratio 2 of 100 μ L ethyl mercaptans and trifluoroacetic acid:1), room temperature, sealing, carries out Thiolation reaction
10min, volatilize naturally in fume hood.100 μ L pyridinium dissolutions are added, add 132 μ L HMDSs and 44 μ L front threes
Base chlorosilane reagent (3:1), 70 DEG C of water-baths, silicon etherification reaction 30min is carried out.After reaction, 100 μ L water and appropriate dichloromethane are added
(volume ratio of water and dichloromethane or chloroform is 1 for alkane or chloroform:6), vibrate, centrifugation, remove a layer solution, can be direct
Carry out gas chromatographic analysis.
Do not extracted after being derived according to document by 2.2.1 section methods by dichloromethane, neutral sugar, uronic acid can only be detected
And ketose, and amino sugar can not be detected, be derived after improved by 2.2.2 section methods, extracted by dichloromethane, can be with
Amino sugar, ketose, neutral sugar and uronic acid are detected simultaneously, as shown in Figure 5 and Figure 6.And the step for Thiolation derivative is improved,
Volatilized naturally through fume hood, i.e. the saving time can avoid ethyl mercaptan smell from being diffused into laboratory again.In addition, it is further right
Standard items derivatization conditions optimize.
2.2.3 single factor exploration
2.2.3.1 influence of the Thiolation derivative reagent reaction time to abundance
4 kinds of standard monose mixed solutions that the accurate compound concentration of specific steps according to 2.2.2 sections is 0.3mg/mL, mercaptan
Change derivative reagent total amount and fix 100 μ L, the reaction time is respectively 10min, 20min, 30min, 40min and 50min.Can by Fig. 1
Know, after monose sample adds Thiolation derivative reagent, with the rise in Thiolation reaction time, peak response intensity becomes in decline
Gesture, 10min is reacted, Thiolation reaction can be made complete, if overlong time, thiolating reagent (ethyl mercaptan and trifluoro may be caused
Acetic acid) it is oxidized, and lose activity.Therefore, the present invention chooses the Thiolation reaction time as 10min derivative samples.
2.2.3.2 influence of the Thiolation derivative reagent total amount to abundance
It is the 4 of 0.3mg/mL according to the specific steps of 2.2.2 sections and the accurate compound concentration of optimal value of 2.2.3.1 section optimizations
Kind standard monose mixed solution, the Thiolation derivative reagent reaction time is 10min, and derivative reagent total amount is respectively 100 μ L, 200 μ
L, 300 μ L, 400 μ L and 500 μ L.
As shown in Figure 2, after monose sample adds Thiolation derivative reagent, when Thiolation derivative reagent total amount is 100 μ L, peak
Downward trend is presented in response intensity, and concentration is 0.3mg/mL standard monose mixed solution, adds the Thiolation derivative examinations of 100 μ L
Agent, it is sufficient to make Thiolation derivative complete, accordingly, it is determined that the Thiolation derivative reagent total amount of sample is 100 μ L.
2.2.3.3 influence of the silicon etherificate derivative reagent reaction temperature to abundance
It is 0.3mg/mL's according to the specific steps of 2.2.2 sections and the accurate compound concentration of optimal value of Thiolation derivative optimization
The pyridine mixed solution of 4 kinds of standard monose, silicon etherificate derivative reagent HMDS and trim,ethylchlorosilane be 132 μ L and
44 μ L (volume ratios 3:1), derivative reagent reaction temperature is respectively 50 DEG C, 70 DEG C and 90 DEG C.
From the figure 3, it may be seen that after monose sample adds derivative reagent, during 70 DEG C of reaction temperature, peak response intensity highest, make silicon ether
It is complete to change reaction, accordingly, it is determined that sample silicon etherificate derivative reagent reaction temperature is 70 DEG C.
2.2.3.4 influence of the silicon etherificate derivative reagent dosage to abundance
4 kinds of marks for being 0.3mg/mL according to the specific steps of 2.2.2 sections and the accurate compound concentration of optimal value of above optimization
The pyridine mixed solution of quasi- monose, during 70 DEG C of reaction temperature, silicon etherificate derivative reagent HMDS and trimethylchloro-silicane
Alkane (volume ratio 3:1) it is respectively 33 μ L：11μL、66μL：22μL、132μL：44 μ L and 264 μ L:88μL.
As shown in Figure 4, after monose sample adds derivative reagent, when derivative reagent HMDS and trimethylchloro-silicane
When alkane is 66 μ L and 22 μ L, peak response intensity highest, accordingly, it is determined that sample silicon is etherified derivative reagent HMDS and three
The volume of methylchlorosilane is 66 μ L and 22 μ L.
In summary, optimal derivatization conditions are：After thiolating reagent total amount is 100 μ L, Thiolation derivatization reaction 10min,
By the pyridine solution that sample preparation is debita spissitudo, silicon etherificate derivatization reaction, silicon etherificate derivative reagent hmds are carried out
Alkane is 66 μ L and 22 μ L with trim,ethylchlorosilane, and 70 DEG C of water-baths derive, and the silicon etherificate derivative time is 30min, can be obtained single
Monose chromatographic peak, and can be with the species and ratio of monose in Accurate Determining herbal polysaccharide.
The preparation of 2.3 samples
2.3.1 in the wind-weed free sugar extraction purification
Rhizoma ane marrhenae 1g is weighed, 10 times of amount distilled water is added, is heated to reflux 2h, in triplicate, filtering, obtain filtrate.
2.3.2 the preparation of analyte derivative
10 μ L sample solution are taken, are concentrated to dryness.Add the mixed solution (volume ratio 2 of 100 μ L ethyl mercaptans and trifluoroacetic acid:
1), room temperature, sealing are reacted 10min, volatilized naturally in fume hood.100 μ L pyridinium dissolutions are added, add the μ L of silicon etherifying reagent 66
HMDS and 22 μ L trim,ethylchlorosilanes, 70 DEG C of water-baths, react 30min.After reaction, 100 μ L water and appropriate are added
Dichloromethane, vibrate, centrifugation, remove a layer solution, can directly carry out gas chromatographic analysis.
2.3.3GC-MS analysis
Using Agilent 7890A-5975C gas chromatograph-mass spectrometers, using the DB-5 capillary columns (μ of 60m × 0.25mm × 0.25
M), temperature programming, 80 DEG C of column temperature, with 2.5 DEG C/min to 190 DEG C, with 2 DEG C/min to 252 DEG C, with 250 DEG C/min to 300 DEG C,
Helium makees carrier gas, 250 DEG C of injector temperature, column flow rate 1.2mL/min.EI (70eV), 250 DEG C of interface temperature, ion source temperature
230 DEG C, scanning range:M/z50-550, scan rate:2.5scan/s.GC-MS is analyzed, with inner mark method ration polysaccharide sample
Monosaccharide component, erythrite is as internal standard compound.
The foundation of 2.4 standard curves
Mixing monose standard items storing solution, GlcN, GalN, ManN and Fru containing 0.6mg/mL are prepared, erythrite is set as
Internal standard compound, its concentration are 0.015mg/mL.Mixing monose is diluted to various concentrations, each monose be followed successively by 0.015mg/mL,
0.03mg/mL, 0.06mg/mL, 0.09mg/mL, 0.12mg/mL, 0.15mg/mL, 0.3mg/mL and 0.6mg/mL.According to
2.3.2 it is vertical with the ratio between monose reference substance peak area during various concentrations and internal standard peak area after the method saved performs the derivatization
Coordinate, linear regression analysis is carried out by abscissa of the concentration of every kind of monose, the results are shown in Table 1.
Table 1：The calibration curve equation and coefficient correlation of 4 kinds of monose
2.5 methodological study
2.5.1 precision test
Precision measures certain density mixing monose standard liquid, after derivatization, by above-mentioned chromatographic condition, continuous sample introduction 5
It is secondary, the ratio of each monosaccharide derivatives peak area and internal standard peak area is determined, as a result the RSD of each peak area is respectively less than 3%, meets point
Analyse basic demand.
2.5.2 replica test
Free sugar need testing solution in 5 parts of wind-weeds of parallel preparation, after derivatization, by above-mentioned chromatographic condition, measure.Obtain confession
In test product after GlcN, GalN, ManN and Fru concentration, calculate RSD and be respectively less than 3%, it is feasible to show that this method is stablized.
2.5.3 stability test
Take free sugar need testing solution in the wind-weed, after derivatization, given respectively after room temperature 0,4,8,12,16,20 and 24h
With measure, as shown in table 2, show that sample is basicly stable within 24h.
Table 2：The effect of 4 kinds of monose average recoveries and matrix
2.6 determination of recovery rates
Free sugar need testing solution in the wind-weed of each sugared content known to 5 parts is taken, monose mixed standard solution is separately added into, presses
After step under " 2.3.2 " item performs the derivatization, sample introduction measure peak area, regression equation is substituted into, calculates average recovery rate, such as table
Shown in 2, show that this method rate of recovery is higher.
The measure of 2.7 samples
The GC-MS collection of illustrative plates of 4 kinds of monose standard items and analyte derivative product is as shown in Fig. 6 and Fig. 7, each monose standard items
Derivative products can separate well, and obtain single chromatogram main peak.The retention time and feature of each monose standard items
Ion is shown in Table 3.The retention index of each monose standard items is shown in Table 4.
Table 3：The characteristic ion of 4 kinds of standard monose
Table 4：The retention index of 4 kinds of standard monose
Claims (10)
1. the method for detecting ketose and amino sugar simultaneously using gas chromatography-mass spectrometry analysis method, it is characterised in that this method is led to
Ethyl mercaptan-trifluoroacetic acid and HMDS-trimethyl silane system are crossed to sample and mixing monose standard solution
In monose carry out Thiolation and silicon etherificate and derive, ethyl mercaptan-silicon etherificate derivative products of ketose and amino sugar are prepared,
After dichloromethane or chloroform extraction, organic layer is carried out reaction product by gas chromatography-mass spectrometry analysis method (GC-MS)
Detection, with the ratio between the peak area of the mixing monose standard solution of various concentrations and internal standard peak area for ordinate, with every kind of list
The concentration of sugar establishes standard curve for abscissa, with the ketose in inner mark method ration sample solution and amino sugar and other monose
Content, a kind of ketose and a kind of amino sugar are comprised at least in described mixing monose standard solution.
2. the method as described in claim 1, it is characterised in that the chromatographic condition of described gas chromatography-mass spectrum is：Using
Agilent 7890A-5975C gas chromatograph-mass spectrometers, using DB-5 capillary columns, temperature programming, 80 DEG C of column temperature, with 2.5 DEG C/min
To 190 DEG C, with 2 DEG C/min to 252 DEG C, with 250 DEG C/min to 300 DEG C, helium makees carrier gas, 250 DEG C of injector temperature, column flow rate
1.2mL/min, EI (70eV), 250 DEG C of interface temperature, 230 DEG C of ion source temperature, scanning range:M/z50-550, scan rate:
2.5scan/s。
3. the method as described in claim 1, it is characterised in that pass through ethyl mercaptan-trifluoroacetic acid and HMDS-three
Methyl-monosilane system carries out concrete operation step derived from Thiolation and silicon etherificate to ketose and amino sugar：Measure same volume
Long-pending sample solution and mixing monose standard solution, is concentrated to dryness, the mixing for adding ethyl mercaptan and trifluoroacetic acid is molten respectively
Liquid, 20-25 DEG C of sealing carry out Thiolation reaction 10-50min, volatilized naturally in fume hood；Pyridinium dissolution is added, adds pregnancy
Base disilazane and trim,ethylchlorosilane, 50-90 DEG C of water-bath, silicon etherification reaction 10-50min is carried out, after reaction, add dichloro
The aqueous solution of methane or chloroform, vibrate, centrifugation, remove a layer organic layer solution, can directly carry out gas chromatography-mass spectrum point
Analysis.
4. method as claimed in claim 3, it is characterised in that the reaction product after derivative is molten through dichloromethane or chloroform
Liquid extracts, and organic layer contains can be etherified derivative products by the ethyl mercaptan-silicon of the GC-MS ketoses detected and amino sugar, therefore can be with
Detect the undetectable amino sugar of existing method.
5. method as claimed in claim 3, it is characterised in that the time of Thiolation reaction is 10min.
6. method as claimed in claim 3, it is characterised in that the volume ratio of ethyl mercaptan and trifluoroacetic acid is 2:1.
7. method as claimed in claim 3, it is characterised in that the volume ratio of HMDS and trim,ethylchlorosilane is
3:1。
8. method as claimed in claim 3, it is characterised in that after adding HMDS and trim,ethylchlorosilane, 70
DEG C water-bath, carry out silicon etherification reaction 30min.
9. the method as described in claim 1, it is characterised in that be designated as erythrite in described.
10. the method as described in claim 1, it is characterised in that also comprising neutrality in described mixing monose standard solution
Sugar and/or uronic acid；Other described monose include neutral sugar and/or uronic acid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710813087.8A CN107655988A (en) | 2017-09-11 | 2017-09-11 | A kind of method for detecting ketose and amino sugar simultaneously using gaschromatographic mass spectrometric analysis method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710813087.8A CN107655988A (en) | 2017-09-11 | 2017-09-11 | A kind of method for detecting ketose and amino sugar simultaneously using gaschromatographic mass spectrometric analysis method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107655988A true CN107655988A (en) | 2018-02-02 |
Family
ID=61129599
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710813087.8A Pending CN107655988A (en) | 2017-09-11 | 2017-09-11 | A kind of method for detecting ketose and amino sugar simultaneously using gaschromatographic mass spectrometric analysis method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107655988A (en) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102936235A (en) * | 2012-11-07 | 2013-02-20 | 浙江大学 | Glucuronic acid mercaptol-acetic ester derivative, and preparation method and application thereof |
| CN103645271A (en) * | 2013-12-20 | 2014-03-19 | 四川农业大学 | Method for improving precision and accuracy of trimethylsilyl ether derivatization-GC-MS determination of saccharide and carboxylic acid compounds in aerosol |
| CN103675180A (en) * | 2013-12-05 | 2014-03-26 | 陈东 | Gas chromatography-mass spectrometry detection method for intracellular carbohydrates and amino acids |
| CN103792312A (en) * | 2013-12-05 | 2014-05-14 | 柳州联海科技有限公司 | Method for detecting amino acids and saccharides in fermentation liquor through gas chromatography-mass spectrometry |
| CN104316630A (en) * | 2014-01-17 | 2015-01-28 | 通化华夏药业有限责任公司 | Method for determining content of saccharide components in ixeri sonhifolia injection |
-
2017
- 2017-09-11 CN CN201710813087.8A patent/CN107655988A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102936235A (en) * | 2012-11-07 | 2013-02-20 | 浙江大学 | Glucuronic acid mercaptol-acetic ester derivative, and preparation method and application thereof |
| CN103675180A (en) * | 2013-12-05 | 2014-03-26 | 陈东 | Gas chromatography-mass spectrometry detection method for intracellular carbohydrates and amino acids |
| CN103792312A (en) * | 2013-12-05 | 2014-05-14 | 柳州联海科技有限公司 | Method for detecting amino acids and saccharides in fermentation liquor through gas chromatography-mass spectrometry |
| CN103645271A (en) * | 2013-12-20 | 2014-03-19 | 四川农业大学 | Method for improving precision and accuracy of trimethylsilyl ether derivatization-GC-MS determination of saccharide and carboxylic acid compounds in aerosol |
| CN104316630A (en) * | 2014-01-17 | 2015-01-28 | 通化华夏药业有限责任公司 | Method for determining content of saccharide components in ixeri sonhifolia injection |
Non-Patent Citations (5)
| Title |
|---|
| A.I. RUIZ-MATUTE ET AL: "Derivatization of carbohydrates for GC and GC–MS analyses", 《JOURNAL OF CHROMATOGRAPHY B》 * |
| KAZUKI TOEDA ET AL: "Microbial Flocculant from Alcaligenes cupidus KT201", 《AGRICULTURAL AND BIOLOGICAL CHEMISTRY》 * |
| NEIL P. J. PRICE: "Acylic Sugar Derivatives for GC/MS Analysis of 13 C-Enrichment during Carbohydrate Metabolism", 《ANALYTICAL CHEMISTRY》 * |
| V. PITTHARD ET AL: "GC-MS Analysis of Monosaccharide Mixtures as their Diethyldithioacetal Derivatives: Application to Plant Gums Used in Art Works", 《CHROMATOGRAPHIA》 * |
| 宋叶涵 等: "三种色谱法分析鲍鱼生殖腺多糖的单糖组成", 《食品与机械》 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101718752B (en) | Detection method of residual polybrominated diphenyl ether in cosmetics with gas chromatography-mass spectrum method | |
| CN104535664B (en) | A kind of method simultaneously detecting multiple mycotoxin in sesame paste | |
| CN104991017B (en) | Liquid chromatogram-tandem mass spectrometry method for determining isothiazolinone bactericides contained in water-based adhesive | |
| CN103808846A (en) | Series quadrupole-rod gas-chromatographic mass spectrometry detection method for 35 toxic medicaments in urine | |
| CN104297409A (en) | Chiral analysis method for nicotine in tobacco juice of electronic cigarette | |
| CN101852766A (en) | Method for detecting phthalate ester plasticizer in plastic | |
| CN1288439C (en) | Method for detecting tobacco specific nitrosamine by liquid phase chromatography and series mass spectrometry | |
| CN105954402A (en) | Gas chromatography-flame ionization/tandem mass spectrometry detection method of alkaloids in cigarette main stream smoke | |
| CN104267135A (en) | Method for measuring carbonyl compound in electronic cigarette liquid | |
| CN105699503A (en) | Method for simultaneously determining content of sodium, potassium, magnesium and calcium in tobaccos | |
| CN112034084A (en) | Detection method of volatile components in blumea oil and application thereof | |
| CN101813675B (en) | LC-MS/MS analysis method for detecting morphinane alkaloid in whole blood and urine | |
| CN104914184A (en) | Cold trap capturing-gas chromatography/mass spectrum combined detection method for furan in cigarette mainstream smoke | |
| CN105572285A (en) | Method for measuring semi-volatile substances in mainstream smoke of cigarettes | |
| CN103389351B (en) | Method for simultaneously detecting 9 acetylene-terminated hormones by virtue of liquid phase-tandem mass spectrometry | |
| CN103149311B (en) | Measuring method of sesame phenol content in tobacco essence perfume | |
| CN112684068A (en) | Method for measuring content of hydroxy-alpha-sanshool | |
| CN104458934A (en) | Method for detecting water-soluble sugar in tobacco and tobacco products | |
| CN107219311A (en) | A kind of method of aspertoxin in quick measure smokeless tobacco | |
| CN107655988A (en) | A kind of method for detecting ketose and amino sugar simultaneously using gaschromatographic mass spectrometric analysis method | |
| CN104502486B (en) | A kind of apply the method for methyl vanillin and ethyl vanillin in Headspace-solid phase microextraction technical measurement milk powder | |
| CN107462657A (en) | A kind of method for detecting uronic acid and aldose simultaneously using gaschromatographic mass spectrometric analysis method | |
| CN103399111B (en) | Method for selectively measuring ethylene glycol monoethyl ether acetate in dry food packaging paper based on headspace-gas chromatography/mass spectrometry | |
| CN106290627B (en) | The analysis method of nitrosamine burst size in a kind of cigarette smoke | |
| CN108828114A (en) | A kind of method of solid phase microextraction-mass spectrometry on-line preconcentration detection Performance Liquid Chromatography Analysis for Nicotine in Tobacco class compound |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20180202 |