CN104614329B - The rapid assay methods of 5 hydroxymethyl furfural contents in gluconate dehydratase reaction solution - Google Patents
The rapid assay methods of 5 hydroxymethyl furfural contents in gluconate dehydratase reaction solution Download PDFInfo
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- hydroxymethyl furfural
- gluconate dehydratase
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- NOEGNKMFWQHSLB-UHFFFAOYSA-N 5-hydroxymethylfurfural Chemical compound OCC1=CC=C(C=O)O1 NOEGNKMFWQHSLB-UHFFFAOYSA-N 0.000 title claims abstract description 60
- 238000006243 chemical reaction Methods 0.000 title claims abstract description 41
- 108091022917 Gluconate dehydratase Proteins 0.000 title claims abstract description 33
- RJGBSYZFOCAGQY-UHFFFAOYSA-N hydroxymethylfurfural Natural products COC1=CC=C(C=O)O1 RJGBSYZFOCAGQY-UHFFFAOYSA-N 0.000 title claims abstract description 27
- 238000003556 assay Methods 0.000 title claims abstract description 11
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims abstract description 26
- 239000008103 glucose Substances 0.000 claims abstract description 23
- 239000007788 liquid Substances 0.000 claims abstract description 19
- 238000010521 absorption reaction Methods 0.000 claims abstract description 13
- 238000002835 absorbance Methods 0.000 claims abstract description 11
- 238000002360 preparation method Methods 0.000 claims abstract description 10
- 238000001514 detection method Methods 0.000 claims abstract description 8
- 239000002608 ionic liquid Substances 0.000 claims abstract description 6
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims description 33
- FHDQNOXQSTVAIC-UHFFFAOYSA-M 1-butyl-3-methylimidazol-3-ium;chloride Chemical compound [Cl-].CCCCN1C=C[N+](C)=C1 FHDQNOXQSTVAIC-UHFFFAOYSA-M 0.000 claims description 19
- 238000007789 sealing Methods 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical group Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims description 6
- 239000005457 ice water Substances 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 230000004044 response Effects 0.000 claims description 4
- 229910021554 Chromium(II) chloride Inorganic materials 0.000 claims description 3
- 229910021556 Chromium(III) chloride Inorganic materials 0.000 claims description 3
- 229910006069 SO3H Inorganic materials 0.000 claims description 3
- 229910021536 Zeolite Inorganic materials 0.000 claims description 3
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 3
- 239000003054 catalyst Substances 0.000 claims description 3
- QSWDMMVNRMROPK-UHFFFAOYSA-K chromium(3+) trichloride Chemical compound [Cl-].[Cl-].[Cl-].[Cr+3] QSWDMMVNRMROPK-UHFFFAOYSA-K 0.000 claims description 3
- 239000011636 chromium(III) chloride Substances 0.000 claims description 3
- 239000010457 zeolite Substances 0.000 claims description 3
- 238000005119 centrifugation Methods 0.000 claims description 2
- XBWRJSSJWDOUSJ-UHFFFAOYSA-L chromium(ii) chloride Chemical compound Cl[Cr]Cl XBWRJSSJWDOUSJ-UHFFFAOYSA-L 0.000 claims description 2
- 238000010790 dilution Methods 0.000 claims description 2
- 239000012895 dilution Substances 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- KAIPKTYOBMEXRR-UHFFFAOYSA-N 1-butyl-3-methyl-2h-imidazole Chemical compound CCCCN1CN(C)C=C1 KAIPKTYOBMEXRR-UHFFFAOYSA-N 0.000 claims 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 9
- 230000008569 process Effects 0.000 abstract description 3
- 238000012360 testing method Methods 0.000 abstract description 3
- 238000005259 measurement Methods 0.000 abstract description 2
- CETXOEGRUBXUAL-UHFFFAOYSA-N 3-(hydroxymethyl)furan-2-carbaldehyde Chemical class OCC=1C=COC=1C=O CETXOEGRUBXUAL-UHFFFAOYSA-N 0.000 abstract 2
- 230000003247 decreasing effect Effects 0.000 description 6
- 238000004128 high performance liquid chromatography Methods 0.000 description 6
- 230000018044 dehydration Effects 0.000 description 5
- 238000006297 dehydration reaction Methods 0.000 description 5
- 238000004817 gas chromatography Methods 0.000 description 5
- 239000003643 water by type Substances 0.000 description 5
- 239000000126 substance Substances 0.000 description 4
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 4
- 241000219095 Vitis Species 0.000 description 3
- 235000009754 Vitis X bourquina Nutrition 0.000 description 3
- 235000012333 Vitis X labruscana Nutrition 0.000 description 3
- 235000014787 Vitis vinifera Nutrition 0.000 description 3
- 238000000862 absorption spectrum Methods 0.000 description 2
- 238000013459 approach Methods 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- HYBBIBNJHNGZAN-UHFFFAOYSA-N furfural Chemical compound O=CC1=CC=CO1 HYBBIBNJHNGZAN-UHFFFAOYSA-N 0.000 description 2
- GAEKPEKOJKCEMS-UHFFFAOYSA-N gamma-valerolactone Chemical compound CC1CCC(=O)O1 GAEKPEKOJKCEMS-UHFFFAOYSA-N 0.000 description 2
- 230000003595 spectral effect Effects 0.000 description 2
- 238000002211 ultraviolet spectrum Methods 0.000 description 2
- IQQRAVYLUAZUGX-UHFFFAOYSA-N 1-butyl-3-methylimidazolium Chemical compound CCCCN1C=C[N+](C)=C1 IQQRAVYLUAZUGX-UHFFFAOYSA-N 0.000 description 1
- GSNUFIFRDBKVIE-UHFFFAOYSA-N 2,5-dimethylfuran Chemical class CC1=CC=C(C)O1 GSNUFIFRDBKVIE-UHFFFAOYSA-N 0.000 description 1
- JOOXCMJARBKPKM-UHFFFAOYSA-N 4-oxopentanoic acid Chemical compound CC(=O)CCC(O)=O JOOXCMJARBKPKM-UHFFFAOYSA-N 0.000 description 1
- 239000002028 Biomass Substances 0.000 description 1
- GMEONFUTDYJSNV-UHFFFAOYSA-N Ethyl levulinate Chemical compound CCOC(=O)CCC(C)=O GMEONFUTDYJSNV-UHFFFAOYSA-N 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 150000003851 azoles Chemical class 0.000 description 1
- 239000002551 biofuel Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000000254 damaging effect Effects 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- CHTHALBTIRVDBM-UHFFFAOYSA-N furan-2,5-dicarboxylic acid Chemical class OC(=O)C1=CC=C(C(O)=O)O1 CHTHALBTIRVDBM-UHFFFAOYSA-N 0.000 description 1
- 150000002240 furans Chemical class 0.000 description 1
- 150000002402 hexoses Chemical class 0.000 description 1
- 238000004811 liquid chromatography Methods 0.000 description 1
- 238000010297 mechanical methods and process Methods 0.000 description 1
- 230000005226 mechanical processes and functions Effects 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 125000004108 n-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000007634 remodeling Methods 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 230000001131 transforming effect Effects 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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Abstract
The invention discloses a kind of rapid assay methods of 5 hydroxymethyl furfural contents in gluconate dehydratase reaction solution, comprise the following steps:(1)The preparation of 5 hydroxymethylfurfurals, glucose and ionic liquid standard liquid;(2)The determination of 5 hydroxymethylfurfural maximum absorption wavelengths;(3)The foundation of 5 hydroxymethylfurfural standard curves;(4)The preparation of gluconate dehydratase reaction solution;(5)Maximum absorption wave strong point carries out absorbance detection and calculates its content to 5 hydroxymethylfurfurals in gluconate dehydratase reaction solution.The inventive method instrument is cheap, and testing cost is cheap, and operating process is simple, and detection time is shorter, measurement result accurately and reliably, for the measure of 5 hydroxymethyl furfural contents provides economic, quick, simple, the reliable method of one kind.
Description
Technical field
The invention belongs to biomass chemical catalysis and chemical composition quantitative analysis field, it is related to a kind of assay method, specifically
It is related to a kind of rapid assay methods of 5 hydroxymethyl furfural content in gluconate dehydratase reaction solution.
Background technology
5 hydroxymethyl furfural(HMF)It is a kind of very important platform chemicals, serves many purposes, it can be both prepared
The bio-fuel of various high-quality such as 5- ethoxyl methyls furfural, ethyl levulinate, gamma-valerolactone, 2,5- dimethyl furans
With long chain alkane etc., it is also possible to prepare chemicals such as levulic acid, 2,5- dihydroxymethyls furans, 2, the 5- furans of various high added values
Dicarbaldehyde of muttering and 2,5- furandicarboxylic acids etc..Glucose is to be distributed in nature most extensively and the most abundant hexose of content,
It is to prepare one of the most frequently used and optimal raw materials of HMF.But, there is the pyranoid form structure of special stabilization, institute due to glucose
Conversion ratio with it in water and organic solvent is very low, and then causes the yield of HMF also than relatively low.In recent years, comparatively just
Suitable ionic liquid 1-butyl-3-methyl imidazolium villaumite([BMIM]Cl)Due to excellent physicochemical property, therefore, its conduct
Reaction dissolvent has obtained more and more widely using during transforming glucose dehydration prepares HMF.At present, HMF is in grape
Content in sugared dehydration liquid is measured using gas chromatography and high performance liquid chromatography mostly, but both approaches
Continuous mode need accurate expensive instrument, good experimental situation and well-trained operating personnel, and their behaviour
Make step comparatively laborious, detection time is also long, waste time and energy.In addition, [BMIM] Cl is for gas chromatograph and efficient liquid
Chromatography also has certain damaging action in itself, thus both approaches all have certain answering in actual mechanical process
Use limitation.
The content of the invention
It is an object of the invention to:A kind of quick measure of 5 hydroxymethyl furfural content in gluconate dehydratase reaction solution is provided
Method, the assay method instrument is cheap, and testing cost is cheap, and operating process is simple, and detection time is shorter, determines knot
Fruit is accurately and reliably.
Technical solution of the invention is that the method is comprised the following steps:
(1)The preparation of 5 hydroxymethyl furfural, glucose and ionic liquid standard liquid;
(2)The determination of 5 hydroxymethyl furfural maximum absorption wavelength;
(3)The foundation of 5 hydroxymethyl furfural standard curve;
(4)The preparation of gluconate dehydratase reaction solution;
(5)Absorbance detection is carried out simultaneously to the 5 hydroxymethyl furfural in gluconate dehydratase reaction solution in maximum absorption wave strong point
Calculate its content.
In step(1)In, the concentration of described 5 hydroxymethyl furfural standard liquid is 0.001 ~ 1 mg/mL;Glucose mark
The concentration of quasi- solution is 0.005 ~ 0.1 mg/mL, and preferred concentration is 0.01 mg/mL;Ionic liquid is 1- butyl -3- methyl miaows
Azoles villaumite([BMIM]Cl), the concentration of its standard liquid is 0.05 ~ 0.2 mg/mL, and preferred concentration is 0.1 mg/mL.
In step(2)In, maximum absorption wave a length of 260 ~ 300 nm of described 5 hydroxymethyl furfural, preferably 284
nm。
In step(4)In, the preparation process of described gluconate dehydratase reaction solution is:By a certain amount of glucose and catalysis
Agent is added in [BMIM] Cl, and heating response certain hour in oil bath pan is placed on after sealing;React after terminating in ice-water bath
In be rapidly decreased to room temperature, add a certain amount of deionized water, be centrifuged after being well mixed, upper strata is gluconate dehydratase reaction solution,
Can be measured after dilution certain multiple.
In the preparation process of gluconate dehydratase reaction solution, the consumption of described [BMIM] Cl is 0.5 ~ 2 g;Described Portugal
The consumption of grape sugar is 50 ~ 150 mg;Described catalyst is AlCl3·6H2O、CrCl2、CrCl3·6H2O、CCC-SO3H、Hβ-
Zeolite (Si/Al=25) or SO4 2-/TiO2-ZrO2In one kind, its consumption be 13.4 ~ 90 mg;Described reaction temperature
It it is 110 ~ 160 °C, the reaction time is 15 ~ 60 min;Described deionized water consumption be 2 ~ 8 mL, centrifugal rotational speed be 5000 ~
10000 rpm, centrifugation time is 5 ~ 10 min;Described extension rate is 5 ~ 2000 times.
The present invention has advantages below:
1)Instrument is cheap, and testing cost is relatively low;
2)Operating process is simple, it is easy to grasp;
3)Detection time is shorter, and detection flux is big;
4)Measurement result accurately and reliably, can be comparable with gas phase and high performance liquid chromatography.
Brief description of the drawings
The uv absorption spectra of Fig. 1 various concentrations HMF.
The uv absorption spectra of Fig. 2 glucose and [BMIM] Cl.
The standard curve of Fig. 3 HMF.
Specific embodiment
With reference to embodiment, the invention will be further described.
Embodiment 1:According to 5 hydroxymethyl furfural content in following steps measure gluconate dehydratase reaction solution
(a)It is accurate to prepare the HMF standard liquids of 0.010 mg/mL, and it is diluted to 0.001 respectively, 0.002,
0.004th, 0.006 and 0.008 mg/mL, carries out all band spectral scan respectively on ultraviolet specrophotometer, and scanning result is such as
Shown in Fig. 1;From figure 1 it appears that under various concentrations, the maximal ultraviolet absorption peak of HMF at 284 nm, therefore, really
Fixed 284 nm are the maximum absorption wavelength of HMF;
(b)The glucose standards solution of 0.01 mg/mL and [BMIM] Cl standard liquids of 0.1 mg/mL are prepared respectively,
All band spectral scan is carried out on ultraviolet specrophotometer respectively, scanning result is as shown in Figure 2;From figure 2 it can be seen that grape
Sugar does not have a UV absorption in the wave-length coverage of 200 ~ 400 nm, and the ultraviolet absorption peak of [BMIM] Cl is at 211 nm, grape
The presence of sugar and [BMIM] Cl does not influence on the measure of HMF contents, therefore, determine HMF's using ultraviolet specrophotometer
Content is feasible;
(c)Concentration with HMF as abscissa, with various concentrations under HMF absorbance as ordinate, draw HMF standard
Curve, as shown in Figure 3;From figure 3, it can be seen that the equation of HMF standard curves is y=131.45x+0.0013, R2=0.9998;
(d)By 100 mg glucose and 13.4 mg AlCl3·6H2O is added in 1 g [BMIM] Cl, by it after sealing
It is placed in oil bath pan and 60 min is heated under 110 °C;Reaction is rapidly decreased to room temperature in ice-water bath after terminating, add 4 mL to go
Ionized water, is well mixed;5000 rpm are centrifuged 10 min, and upper strata is gluconate dehydratase reaction solution;
(e)By step(d)In gluconate dehydratase reaction solution dilute 2000 times, then with ultraviolet specrophotometer repeat survey
Determine its absorbance and the relative standard deviation of HMF contents is calculated according to standard curve(RSD);From table 1 it follows that determine
The relative standard deviation of HMF contents is only 1.04%, and this illustrates the ultraviolet spectra for determining HMF contents in glucose response liquid
Method has precision higher;
(f)Take step(d)In the mL of gluconate dehydratase reaction solution 1, add 0.5 ~ 4 mL 1mg/mL HMF standards it is molten
Liquid, constant volume is to 10 mL after mixing and dilutes 200 times again, then determines its absorbance and according to standard with ultraviolet specrophotometer
Curve calculates the TIANZHU XINGNAO Capsul of HMF contents;From Table 2, it can be seen that the TIANZHU XINGNAO Capsul of the HMF contents for determining is 100.45
~ 102.74%, average out to 101.81%, close to 100%, this illustrates the ultraviolet spectra for detecting HMF contents in glucose response liquid
Method has the degree of accuracy higher;
(g)By step(d)Middle gluconate dehydratase reaction solution dilutes 2000,10 and 5 times respectively, then uses uv-spectrophotometric
Meter, gas chromatograph and high performance liquid chromatograph determine the content of HMF;Although from table 3 it is observed that ultraviolet spectroscopy is measured
HMF contents it is more slightly higher than the HMF contents that gas chromatography and high performance liquid chromatography are measured, but ultraviolet spectroscopy with
The mean error of the HMF contents that gas chromatography and high performance liquid chromatography are measured only be respectively 2.53 and 1.96%, 3% with
Interior, this explanation determines HMF contents using ultraviolet spectroscopy can be comparable with gas chromatography and high performance liquid chromatography.
The Precision Experiment of table 1
The TIANZHU XINGNAO Capsul of table 2 is tested
The ultraviolet spectroscopy of table 3, gas chromatography and high performance liquid chromatography compare
Embodiment 2:Step(a-c)With embodiment 1;Then, by 100 mg glucose and 6.9 mg CrCl2It is added to 1 g
In [BMIM] Cl, it is placed on after sealing in oil bath pan and 30 min is heated under 120 °C;Reaction is fast in ice-water bath after terminating
Prompt drop adds 4 mL deionized waters to room temperature, is well mixed;10000 rpm are centrifuged 5 min, and it is anti-that upper strata is gluconate dehydratase
Answer liquid;Above-mentioned gluconate dehydratase reaction solution is diluted 2000 times, its absorbance is determined with ultraviolet specrophotometer, according to embodiment
Standard curve in 1 calculates HMF contents for 46.21 mg.
Embodiment 3:Step(a-c)With embodiment 1;Then, by 100 mg glucose and 14.9 mg CrCl3·6H2O is added
To in 1 g [BMIM] Cl, it is placed on after sealing in oil bath pan and 30 min is heated under 120 °C;React after terminating in frozen water
Room temperature is rapidly decreased in bath, 4 mL deionized waters are added, is well mixed;5000 rpm are centrifuged 10 min, and upper strata is glucose
Dehydration liquid;Above-mentioned gluconate dehydratase reaction solution is diluted 2000 times, its absorbance is determined with ultraviolet specrophotometer, according to
Standard curve in embodiment 1 calculates HMF contents for 50.73 mg.
Embodiment 4:Step(a-c)With embodiment 1;Then, by 50 mg glucose and 20 mg CCC-SO3H is added to
In 0.5 g [BMIM] Cl, it is placed on after sealing in oil bath pan and 15 min is heated under 160 °C;React after terminating in frozen water
Room temperature is rapidly decreased in bath, 2 mL deionized waters are added, is well mixed;10000 rpm are centrifuged 5 min, and upper strata is glucose
Dehydration liquid;Above-mentioned gluconate dehydratase reaction solution is diluted 2000 times, its absorbance is determined with ultraviolet specrophotometer, according to
Standard curve in embodiment 1 calculates HMF contents for 16.46 mg.
Embodiment 5:Step(a-c)With embodiment 1;Then, by 150 mg glucose and 90 mg H β-zeolite (Si/
Al=25) it is added in 1.5 g [BMIM] Cl, is placed on after sealing in oil bath pan and 50 min are heated under 150 °C;Reaction
Room temperature is rapidly decreased to after end in ice-water bath, 6 mL deionized waters are added, is well mixed;5000 rpm are centrifuged 10 min, on
Layer is gluconate dehydratase reaction solution;Above-mentioned gluconate dehydratase reaction solution is diluted 2000 times, it is determined with ultraviolet specrophotometer
Absorbance, the standard curve in embodiment 1 calculates HMF contents for 53.32 mg.
Embodiment 6:Step(a-c)With embodiment 1;Then, by 100 mg glucose and 50 mg SO4 2-/TiO2-ZrO2
It is added in 2 g [BMIM] Cl, is placed on after sealing in oil bath pan and 60 min are heated under 140 °C;Reaction terminate after
Room temperature is rapidly decreased in ice-water bath, 8 mL deionized waters are added, is well mixed;10000 rpm are centrifuged 5 min, and upper strata is grape
Sugared dehydration liquid;Above-mentioned gluconate dehydratase reaction solution is diluted 2000 times, its absorbance, root are determined with ultraviolet specrophotometer
HMF contents are calculated for 33.95 mg according to the standard curve in embodiment 1.
Above-described embodiment is not limitation of the present invention, and the present invention is also not limited to above-described embodiment.This technology is led
Change, remodeling, addition or replacement that the technical staff in domain makes in essential scope of the invention, fall within guarantor of the invention
Shield scope.
Claims (4)
1. in gluconate dehydratase reaction solution 5 hydroxymethyl furfural content rapid assay methods, the assay method include following step
Suddenly:(1)The preparation of 5 hydroxymethyl furfural, glucose and ionic liquid standard liquid;(2)5 hydroxymethyl furfural maximum absorption wavelength
Determination;(3)The foundation of 5 hydroxymethyl furfural standard curve;(4)The preparation of gluconate dehydratase reaction solution;(5)In absorption maximum
Absorbance detection is carried out to the 5 hydroxymethyl furfural in gluconate dehydratase reaction solution at wavelength and its content is calculated;Its feature exists
In:Step(1)In, the concentration of described 5 hydroxymethyl furfural standard liquid is 0.001 ~ 1 mg/mL;Glucose standards solution
Concentration is 0.005 ~ 0.1 mg/mL;Ionic liquid is 1- butyl -3- methylimidazole villaumites([BMIM]Cl), its standard liquid
Concentration is 0.05 ~ 0.2 mg/mL;Step(2)In, a length of 260 ~ 300 nm of maximum absorption wave of described 5 hydroxymethyl furfural;
Step(4)In, the preparation process of described gluconate dehydratase reaction solution is:A certain amount of glucose and catalyst are added to
In [BMIM] Cl, heating response certain hour in oil bath pan is placed on after sealing;Reaction is dropped rapidly after terminating in ice-water bath
To room temperature, a certain amount of deionized water is added, be centrifuged after being well mixed, upper strata is gluconate dehydratase reaction solution, dilution is certain
Can be measured after multiple.
2. in gluconate dehydratase reaction solution according to claim 15 hydroxymethyl furfural content rapid assay methods, its
It is characterised by:Step(1)In, the concentration of glucose standards solution is 0.01 mg/mL, and the concentration of [BMIM] Cl standard liquids is
0.1 mg/mL。
3. in gluconate dehydratase reaction solution according to claim 15 hydroxymethyl furfural content rapid assay methods, its
It is characterised by:Step(2)In, a length of 284 nm of maximum absorption wave of described 5 hydroxymethyl furfural.
4. in gluconate dehydratase reaction solution according to claim 15 hydroxymethyl furfural content rapid assay methods, its
It is characterised by:In the preparation process of gluconate dehydratase reaction solution, the consumption of described [BMIM] Cl is 0.5 ~ 2 g;Described Portugal
The consumption of grape sugar is 50 ~ 150 mg;Described catalyst is AlCl3·6H2O、CrCl2、CrCl3·6H2O、CCC-SO3H、Si/
H β-the zeolite or SO of Al=254 2-/TiO2-ZrO2In one kind, its consumption be 13.4 ~ 90 mg;Described reaction temperature is
110 ~ 160 °C, the described reaction time is 15 ~ 60 min;Described deionized water consumption is 2 ~ 8 mL, and centrifugal rotational speed is
5000 ~ 10000 rpm, centrifugation time is 5 ~ 10 min;Described extension rate is 5 ~ 2000 times.
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CN105954215A (en) * | 2016-05-03 | 2016-09-21 | 河南师范大学 | Method for measuring content of furfural by utilizing aniline hydrochloride salt solution |
CN110618098A (en) * | 2019-09-06 | 2019-12-27 | 东莞理工学院 | Method for measuring AGEs content in soybean milk |
CN110658146A (en) * | 2019-11-12 | 2020-01-07 | 浙江华康药业股份有限公司 | Method for rapidly determining content of hydroxymethylfurfural in high fructose corn syrup |
Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102711994A (en) * | 2009-09-25 | 2012-10-03 | 国立大学法人北海道大学 | Catalyst for hydrolysis of cellulose or hemicellulose, and process for production of sugar-containing solution using the catalyst |
-
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Patent Citations (1)
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---|---|---|---|---|
CN102711994A (en) * | 2009-09-25 | 2012-10-03 | 国立大学法人北海道大学 | Catalyst for hydrolysis of cellulose or hemicellulose, and process for production of sugar-containing solution using the catalyst |
Non-Patent Citations (3)
Title |
---|
固体催化剂催化葡萄糖制备5-羟甲基糠醛;杨柳;《CNKI中国优秀硕士学位论文全文数据库》;20130115;第16-19页 * |
离子液体中金属氯化物催化糖脱水制备5-羟甲基糠醛;代学民;《CNKI中国优秀硕士学位论文全文数据库》;20090915;第23-24页 * |
紫外分光光度法测定复方电解质葡萄糖注射液)中的5-羟甲基糠醛;李华龙等;《天津药学》;20090131;第21卷(第1期);全文 * |
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