CN105445081B - The application of vitamin B6 in a kind of double-aqueous phase system and its separation watermelon flesh - Google Patents
The application of vitamin B6 in a kind of double-aqueous phase system and its separation watermelon flesh Download PDFInfo
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Abstract
The invention discloses a kind of applications of vitamin B6 in double-aqueous phase system and its separation watermelon flesh, including chlorination N butyl-pyridiniums ionic liquid, potassium dihydrogen phosphate and water, by mass percentage, chlorination N butyl-pyridiniums ionic liquid is 50%~70.1% in double-aqueous phase system, potassium dihydrogen phosphate is 15.3%~24.2%, remaining component is water, and the total mass fraction of three components is 100%.This method is to the extraction yield of vitamin B6 up to 98.9%.The features such as wide with the range of linearity, detection limit is low, and relative standard deviation is smaller, high to the measure rate of recovery of sample, and effect of extracting is good.It can be provided for multiple fields such as biological medicines largely, the vitamin B6 of high-purity.
Description
Technical field
The invention belongs to environmental projects and the environmental technology field of analytical chemistry, and in particular to a kind of double-aqueous phase system and its
Detach the application of vitamin B6 in watermelon flesh.
Background technology
Vitamin B6 (Vitamin B6) is also known as pyridoxine, is a kind of water soluble vitamin, meets light or alkali destructible, intolerant to
High temperature.It is the constituent of certain coenzyme in human body, participates in a variety of metabolic responses of human body, especially has with amino acid metabolism close
Cut relationship.Vitamin B6 can slow down insulin for treating diabetes vascular complication, be as caused by artery sclerosis.And tie up life
The activation pattern phosphoric acid ratio of plain B6 is trembled aldehyde (Pyridoxal phosphate, PDP), is had in protection vascular endothelial cell reduces
Chrotoplast is acted on by activated blood platelet damage, inhibits platelet aggregation and blood clotting.With the depth of clinical application research
Enter, it is found that vitamin B6 clinically also has extensive new application.Such as anaemia is treated, poisoning by isoniazid is rescued, treatment is white
Cytopenia, treatment intellectual development is sluggish, treatment parkinson's syndrome etc..It is clinically prevented at present using Vitamin B6 preparation
The vomiting of pregnancy and radiation sickness vomiting.
In view of major contribution of the vitamin B6 to physianthropy, the vitamin B6 of separating high-purity has very great meaning
Justice.Saccharomycete, liver, vegetables, grain, meat, fish, egg, beans contain a large amount of vitamin B6, especially content in the pulp of watermelon
It is larger.Vitamin B6 is measured and detaches frequently with high performance liquid chromatography etc. at present.But in analytical instrument, detection side
Also there are many problems for method, separation determination, data processing etc..Such as large-scale instrument is expensive, separation method efficiency is low,
Time-consuming and the low research for influencing its drug effect and clinical practice of the vitamin B6 purity of separation and Extraction.Therefore it needs more
Efficient extracting process extracts vitamin B6.
For ionic liquid aqueous two-phase as a kind of novel green separation system occurred in recent years, itself has toxicity
It is small, the properties such as non-combustible, non-volatile, not oxidizable.It has been investigated that ionic liquid is on the one hand to the molten of inorganic and organic materials
Solution has selectivity, and on the other hand immiscible with certain organic solvents, this feature may be used on liquid-liquid extraction, the micro- extraction of liquid phase
It takes, solid phase microextraction, ionic liquid/supercritical CO2Extraction etc..Again because it is with the split-phase time is short, extraction yield is high, extraction
Take process be not easy emulsification and ionic liquid the advantages that can recycling and receive more and more attention.In addition, ionic liquid
The main component of double-aqueous phase system two-phase is all water so that it is being extracted with the required benign environment of bioactive molecule
It has broad application prospects on separation biological substance.
Invention content
For long there are extraction time in the extracting process of existing vitamin B6, equipment costliness, complicated for operation, extraction yield
Low shortcoming, the object of the present invention is to provide vitamins in a kind of ionic liquid double-aqueous phase system and its separation watermelon flesh
The application of B6.This method can obtain largely, and the vitamin B6 of high-purity shortens the disengaging time of vitamin B6, has simultaneously
Have it is easy to operate, without using large-scale instrument, the characteristics of reduction using traditional volatile organic solvent to avoid secondary pollution is brought.
In order to realize above-mentioned task, the present invention takes following technical solution：
A kind of double-aqueous phase system, including chlorination-N- butyl-pyridiniums ionic liquid, potassium dihydrogen phosphate and water.
Specifically, by mass percentage, in double-aqueous phase system chlorination-N- butyl-pyridiniums ionic liquid for 50%~
70.1%, potassium dihydrogen phosphate is 15.3%~24.2%, remaining is water, and three's mass fraction summation is 100%.
Preferably, by mass percentage, chlorination-N- butyl-pyridiniums ionic liquid is 55.1% in double-aqueous phase system, phosphorus
Acid dihydride potassium is 18.3%, remaining is water, and three's mass fraction summation is 100%.
The application of vitamin B6 in the double-aqueous phase system separation watermelon flesh.
Include the step of vitamin B6 in separation watermelon flesh：
Step 1：The watermelon flesh to be separated processing that squeeze the juice is obtained into watermelon flesh Normal juice；
Step 2：It is 1 in mass ratio by watermelon flesh Normal juice and the double-aqueous phase system:5 mixing are extracted, and are extracted
Temperature is 25 DEG C~35 DEG C, and extraction pH is 4.5~5.5.
Preferred condition, detach watermelon flesh in vitamin B6 the step of include：
Step 1：The watermelon flesh to be separated processing that squeeze the juice is obtained into watermelon flesh Normal juice；
Step 2：It is 1 in mass ratio by watermelon flesh Normal juice and the double-aqueous phase system:5 mixing are extracted, and are extracted
Temperature is 30 DEG C, and extraction pH is 5.
Advantages of the present invention is as follows：
(1) of the invention method set ionic liquid and the advantages of aqueous two-phase, overcomes traditional polymer aqueous two-phase
The easy emulsification of system, the shortcomings of split-phase time is long.
(2) due to containing glycine betaine in watermelon flesh, the chlorination-N- butyl-pyridiniums that can be selected with the present invention react generation ammonia
The pyridoxamine pairing of ylidene ligands, such ligand and vitamin B6, therefore largely increase the extraction yield of vitamin B6.This
Double-aqueous phase system described in patent can reach 98.9% to the extraction yield of the vitamin B6 in watermelon flesh.
(3) double-aqueous phase system of the invention is with extraction time is short, easy to operate, purity is high and reagent green is without secondary
The advantages that pollution, the vitamin B6 that the research for multiple fields such as clinical medicine obtains a large amount of high-purities provide new way.
Description of the drawings
Fig. 1 is KH2PO4The influence relational graph of concentration on extraction rate；
Fig. 2 is the influence relational graph of [BPy] Cl concentration on extraction rates；
Fig. 3 is influence of the double-aqueous phase system to the extraction yield of vitamin B6 under different temperatures；
Fig. 4 is different pH value to influence of the double-aqueous phase system to the extraction yield of vitamin B6；
The present invention is further explained below in conjunction with the drawings and specific embodiments.
Specific embodiment
Chlorination-N- butyl-pyridinium ionic liquids selected by the present invention are purchased from marine origin victory Chemical Co., Ltd., purity
It is 0.99.
Contain glycine betaine in watermelon flesh, the chlorination-N- butyl-pyridinium ionic liquids that can be selected with the present invention react generation
The pyridoxamine pairing of amino ligands, such ligand and vitamin B6, therefore the extraction yield of vitamin B6 is largely increased,
This is the characteristics of other ionic liquids do not have.But up to the present, about ionic liquid double-aqueous phase system as extractor body
The data information of system also extremely lacks, meanwhile, the research about pyridine ionic liquid two phase aqueous extraction system has not been reported,
Thus there is theoretical and realistic meaning to the research and inquirement of such system.
The present invention is used and is formed with chlorination-N- butyl-pyridiniums ionic liquid and potassium dihydrogen phosphate by a series of experiment
Double-aqueous phase system as extractant, extract the vitamin B6 in watermelon flesh.Specifically comprise the following steps：By 5.00~
Chlorination-N- butyl-pyridiniums ([BPy] Cl) ionic liquid and 1.53~2.42g potassium dihydrogen phosphates of 7.01g is uniformly mixed with water,
Obtain 10g two phase aqueous extraction systems；Add in the two phase aqueous extraction system into 2g watermelon flesh Normal juice to be measured, then 25~
35 DEG C of temperature and pH value are constant temperature oscillation 30min under conditions of 4.5~5.5, and extraction is stood for 24 hours after split-phase.
The glycine betaine that the present invention is demonstrated by contrast test in watermelon, which has the extraction process of vitamin B6, to be promoted
Effect.Specific experiment operating procedure is as follows：
1st, watermelon is detected by liquid chromatography before testing, finds to contain a large amount of glycine betaine in watermelon.
2nd, 5.51g chlorination-N- butyl-pyridinium ionic liquids are taken in test tube, thereto add in 2g glycine betaines standard solution and
2.96g water, abundant mixing simultaneously stand 3~5 minutes, are detected by liquid chromatography.Testing result shows in mixed solution
There is the presence of amino.1.53g potassium dihydrogen phosphates and 2g vitamin B6 standard solution are added in into the solution after reaction, in 30 DEG C
With constant temperature oscillation 30min under pH5.0, extraction is stood for 24 hours after split-phase.After split-phase is clear.Measure remaining vitamin B6 in water phase
Concentration, by the extraction yield of the content calculation vitamin B6 of vitamin B6 in water phase before and after extraction.
3rd, control experiment is carried out.5.51g chlorination-N- butyl-pyridinium ionic liquids is taken to add in 1.53g thereto in test tube
Potassium dihydrogen phosphate and 4.96g water, abundant mixing, then 2g vitamin B6 standard solution is added in thereto, under 30 DEG C and pH5.0
Constant temperature oscillation 30min stands extraction for 24 hours after split-phase.After split-phase is clear.The concentration of remaining vitamin B6 in water phase is measured, by
Before and after extraction in water phase the content calculation vitamin B6 of vitamin B6 extraction yield.
4th, it is calculated at after adding in glycine betaine, the extraction yield of vitamin B6 is 94.5%, and does not add in the system of glycine betaine
Extraction yield to vitamin B6 is 84.6%.Through test of many times, experimental result shows the extraction of vitamin B6 after addition glycine betaine
Take rate higher.Match it can thus be appreciated that the chlorination-N- butyl-pyridinium ionic liquids that glycine betaine can be selected with the present invention react generation amino
The pyridoxamine pairing of body, such ligand and vitamin B6, therefore largely increase the extraction yield of vitamin B6.
In order to realize high extraction yield, a series of experiments has also been devised to obtain preferably technological parameter in the present invention：
1st, 5.51g chlorination-N- butyl-pyridiniums ionic liquid, 1- butyl -3- picoline tetrafluoro boric acid salt ions are taken respectively
Liquid, 1-butyl-3-methylimidazolium bromide ionic liquid, polyvinylpyrrolidone k30, polyethylene glycol 400 add in five centrifugations
Guan Zhong adds in 1.83g KH2PO4And appropriate distilled water makes gross mass in centrifuge tube be 10g.2g watermelon flesh Normal juice is added to fill
Divide mixing.Extraction is stood after 30 DEG C and constant temperature oscillation 30min under pH5.0, split-phase for 24 hours.After split-phase is clear.It measures in water phase
The concentration of remaining vitamin B6, by the extraction yield of the content calculation vitamin B6 of vitamin B6 in water phase before and after extraction.As a result such as
Shown in table one.
Table one is that variety classes ionic liquid or polymer form double-aqueous phase system to vitamin B6 with potassium dihydrogen phosphate
Extraction yield, significantly can be relatively low to the extraction yield of vitamin B6 with other several ionic liquids by data in table, and difference lies in only
Chlorination-N- butyl-pyridiniums ionic liquid can be reacted with the glycine betaine in watermelon flesh Normal juice generation amino ligands, such ligand with
The pyridoxamine pairing of vitamin B6, therefore largely increase the extraction yield of vitamin B6.And other double-aqueous phase systems are then
Do not have this property, therefore extraction yield is relatively low.
Table one
2nd, the chlorination-N- butyl-pyridinium ionic liquids of 5.51g are taken, are placed in centrifuge tube, then add the phosphoric acid of 1.83g respectively
Potassium dihydrogen, sodium sulfite, disodium-hydrogen, ammonium citrate, ammonium sulfate and appropriate distilled water make gross mass in centrifuge tube be 10g,
Add the abundant mixing of 2g watermelon flesh Normal juice.Extraction is stood after 30 DEG C and constant temperature oscillation 30min under pH5.0, split-phase for 24 hours.
After split-phase is clear, the concentration of remaining vitamin B6 in water phase is measured, by the content calculation of vitamin B6 in water phase before and after extraction
The extraction yield of vitamin B6.As a result as shown in Table 2.
Table is second is that different types of salt forms extraction yield of the double-aqueous phase system to vitamin B6 with [BPy] Cl, by number in table
According to understanding [BPy] Cl/KH2PO4Double-aqueous phase system is maximum to the extraction yield of vitamin B6, is 98.9%.Because KH2PO4With
[BPy] Cl split-phase degree is best, most thorough, therefore maximum to the extraction yield of vitamin B6.And there are split-phases for other several salt
Phenomena such as being not thorough, therefore extraction yield is low.
Table two
| Salt type | Potassium dihydrogen phosphate | Sodium sulfite | Disodium-hydrogen | Ammonium citrate | Ammonium sulfate |
| Extraction yield (%) | 98.9 | 82.6 | 90.2 | 84.1 | 88.8 |
3rd, the chlorination-N- butyl-pyridinium ionic liquids of 5.51g are taken, is placed in centrifuge tube, adds in the biphosphate of 1.83g
Potassium and appropriate distilled water make in centrifuge tube gross mass be 10g, then be separately added into 2g watermelon flesh Normal juice, kiwi-fruit juice, tomato juice,
Walnut oil and the abundant mixing of peanut oil.Extraction is stood after 30 DEG C and constant temperature oscillation 30min under pH5.0, split-phase for 24 hours.It treats point
After phase is clear.The concentration of remaining vitamin B6 in water phase is measured, life is tieed up by the content calculation of vitamin B6 in water phase before and after extraction
The extraction yield of plain B6.As a result as shown in Table 3
Table three is [BPy] Cl/KH2PO4Double-aqueous phase system is to the extraction yield of separate sources vitamin B6.It can by data in table
To find out, [BPy] Cl/KH2PO4Double-aqueous phase system is to the extraction yield highest of the vitamin B6 in watermelon flesh Normal juice.This is because
Glycine betaine in watermelon flesh Normal juice can be reacted with [BPy] Cl, increase extraction yield, and other raw materials do not have this property then,
Therefore the double-aqueous phase system is poor compared with watermelon flesh Normal juice to the effect of extracting of the vitamin B6 in other sources and extraction yield compares phase
Closely.
Table three
| Vitamin B6 source | Watermelon flesh Normal juice | Kiwi-fruit juice | Tomato juice | Walnut oil | Peanut oil |
| Extraction yield (%) | 98.9 | 82.6 | 84.4 | 79.6 | 80.2 |
4th, the chlorination-N- butyl-pyridinium ionic liquids of 5.51g are taken, are placed in centrifuge tube, be separately added into 0.33g, 0.67g,
The potassium dihydrogen phosphate of 0.97g, 1.21g, 1.53g, 1.83g, 2.11g, 2.42g, 2.76g, 3.05g and appropriate distilled water make centrifugation
Gross mass is 10g in pipe, then is separately added into the abundant mixing of 2g watermelon flesh Normal juice.The constant temperature oscillation under 30 DEG C and pH5.0
30min stands extraction for 24 hours after split-phase.After split-phase is clear, the concentration of remaining vitamin B6 in water phase is measured, before and after extraction
The extraction yield of the content calculation vitamin B6 of vitamin B6 in water phase.The results are shown in Figure 1.
Fig. 1 is KH2PO4The influence relational graph of concentration on extraction rate.Wherein, abscissa represents KH2PO4It is to be measured molten adding in
Concentration in extraction system before liquid, ordinate represent extraction yield.With KH in system2PO4The increase of concentration, vitamin B6
Extraction yield is in the trend of first increases and then decreases.Chlorination-N- butyl-pyridiniums/the potassium dihydrogen phosphate formed before solution to be measured is added in
In double-aqueous phase system, KH2PO4Concentration at 3.3%~18.3%, the extraction yield of vitamin B6 is with KH2PO4The increase of concentration
And increase, up to 98.9% is reached at a concentration of 18.3%.Work as KH2PO4Concentration be more than 18.3% when, vitamin B6
Extraction yield is declined slightly.It can be seen from the figure that KH2PO4Addition extraction yield in the range of 1.53~24.2g is not less than
97%, therefore the optimal concentration of the potassium dihydrogen phosphate in the extraction system before adding in solution to be measured is 15.3~24.2%.
5th, 3.00g, 3.51g, 4.01g, 4.52g, 5.00g, 5.51g, 6.00g, 6.51g, 7.01g, 7.51g are taken respectively
Chlorination-N- butyl-pyridinium ionic liquids be placed in centrifuge tube, the potassium dihydrogen phosphate and appropriate distilled water for adding in 1.83g make centrifugation
Gross mass is 10g in pipe, then is separately added into the abundant mixing of 2g watermelon flesh Normal juice.The constant temperature oscillation under 30 DEG C and pH5.0
30min stands extraction for 24 hours after split-phase.After split-phase is clear, the concentration of remaining vitamin B6 in water phase is measured, before and after extraction
The extraction yield of the content calculation vitamin B6 of vitamin B6 in water phase.The results are shown in Figure 2.
Fig. 2 is the influence relational graph of [BPy] Cl concentration on extraction rates.Wherein, abscissa represents chlorination-N- butyl-pyridiniums
Concentration of the ionic liquid in the extraction system before adding in solution to be measured, ordinate represent extraction yield.The extraction of vitamin B6
Rate increases first with the increase of the concentration of ionic liquid, and up to 98.9% is reached when salinity reaches 55.1%.When
When chlorination-N- butyl-pyridiniums ionic liquid concentration is more than 55.1%, the extraction yield of vitamin B6 has a declining tendency and declines slow
Slowly.It can be seen from the figure that extraction yield is not less than 97% when ionic liquid addition is 5.00~7.01g, therefore, chlorination-
Optimal concentration of the N- butyl-pyridiniums in the extraction system before adding in solution to be measured is 50~70.1%.
6th, 5.51g chlorination-N- butyl-pyridinium ionic liquids are taken in centrifuge tube, add in the potassium dihydrogen phosphate of 1.83g and are fitted
Amount distilled water makes gross mass in centrifuge tube be 10g, then be separately added into the abundant mixing of 2g watermelon flesh Normal juice.Respectively at 20 DEG C, 25
DEG C, 30 DEG C, 35 DEG C, 40 DEG C, 45 DEG C, 50 DEG C, 55 DEG C, 60 DEG C, constant temperature oscillation 30min under 65 DEG C and pH5.0, stand after split-phase
Extraction is for 24 hours.After split-phase is clear, the concentration of remaining vitamin B6 in water phase is measured, by vitamin B6 in water phase before and after extraction
The extraction yield of content calculation vitamin B6.Shown in result figure 3.
Fig. 3 is influence of the double-aqueous phase system to the extraction yield of vitamin B6 at different temperatures.The result shows that temperature is 20
DEG C~30 DEG C between, extraction yield is increased rapidly with the raising of temperature, and extraction yield reaches highest at 30 DEG C, be 98.9%.
After more than 30 DEG C, the extraction yield of vitamin B6 reduces temperature with the raising of temperature, it can be seen from the figure that described double
Aqueous phase system is when temperature is 25~35 DEG C to the extraction yield of vitamin B6 not less than 95%, therefore 25~35 DEG C are aqueous two-phases
System extracts the optimum temperature range of vitamin B6, wherein extraction yield highest at 30 DEG C.
7th, 5.51g chlorination-N- butyl-pyridinium ionic liquids are taken in centrifuge tube, add in the potassium dihydrogen phosphate of 1.83g and are fitted
Amount distilled water makes gross mass in centrifuge tube be 10g, then be separately added into the abundant mixing of 2g watermelon flesh Normal juice.Respectively at pH 2,3,
4th, constant temperature oscillation 30min at 4.5,5,5.5,6,7,8,9 and 30 DEG C stands extraction for 24 hours after split-phase.After split-phase is clear, measure
The concentration of remaining vitamin B6 in water phase, by the extraction yield of the content calculation vitamin B6 of vitamin B6 in water phase before and after extraction.
Shown in result figure 4.
Fig. 4 is different pH value to influence of the double-aqueous phase system to the extraction yield of vitamin B6.The result shows that pH is 2~5
Between, extraction yield is increased rapidly with the increase of pH, and when pH is 5.0, the extraction yield of vitamin B6 reaches highest.PH is 5~9
Between, the extraction yield of vitamin B6 declines rapidly with the increase of pH values.It can be seen from the figure that the double-aqueous phase system exists
PH is not less than 93%, therefore pH is this aqueous two-phase body for 4.5~5.5 under the conditions of being 4.5~5.5 to the extraction yield of vitamin B6
The optimal pH range of system's extraction vitamin B6, wherein, pH5.0 extraction yield highests are 98.9%.
To sum up experimental result understands chlorination-N- butyl-pyridiniums ([BPy] Cl) ion that mass fraction is 50%~70.1%
Liquid and mass fraction are that the double-aqueous phase system of 15.3%~24.2% potassium dihydrogen phosphate composition in pH is 4.5~5.5, extraction temperature
Spend be 25~35 DEG C under conditions of effect of extracting it is best.
It is the specific embodiment that inventor provides below.
Embodiment 1：
5.51g chlorination-N- butyl-pyridinium ionic liquids are taken, is placed in centrifuge tube, adds in the KH of 1.83g2PO4And appropriate steaming
Distilled water makes gross mass in centrifuge tube be 10g, adds 2g watermelon flesh Normal juice, abundant mixing.Constant temperature shakes under 30 DEG C and pH5.0
30min is swung, extraction is stood for 24 hours after split-phase.
After split-phase is clear, the concentration of remaining vitamin B6 in water phase is measured, by vitamin B6 in water phase before and after extraction
The extraction yield that content meter calculates vitamin B6 is 98.9%.Show that the invention has very well the vitamin B6 in watermelon flesh Normal juice
Extraction.
Embodiment 2：
Preparation method in the present embodiment is same as Example 1, and the condition differed only in preparation process is different, this reality
It applies chlorination-N- butyl-pyridinium ionic liquid structural reform polyvinylpyrrolidone k30 in example, remaining condition is constant.
After split-phase is clear, the concentration of remaining vitamin B6 in water phase is measured, by vitamin B6 in water phase before and after extraction
The extraction yield that content meter calculates vitamin B6 is 73.6%.Show that the invention imitates the extraction of vitamin B6 in watermelon flesh Normal juice
Fruit effect is general.
Embodiment 3：
Preparation method in the present embodiment is same as Example 1, and the condition differed only in preparation process is different, this reality
The sodium sulfite that potassium dihydrogen phosphate is changed to equivalent in example is applied, remaining condition is constant.
After split-phase is clear, the concentration of remaining vitamin B6 in water phase is measured, by vitamin B6 in water phase before and after extraction
The extraction yield that content meter calculates vitamin B6 is 82.6%.Show that the invention imitates the extraction of vitamin B6 in watermelon flesh Normal juice
Fruit effect is general.
Embodiment 4：
Preparation method in the present embodiment is same as Example 1, differs only in extraction object source difference, this implementation
Extraction object is changed to walnut oil in example, remaining condition is constant.
After split-phase is clear, the concentration of remaining vitamin B6 in water phase is measured, by vitamin B6 in water phase before and after extraction
The extraction yield that content meter calculates vitamin B6 is 79.6%.Show that the invention imitates the extraction of vitamin B6 in watermelon flesh Normal juice
Fruit effect is general.
Embodiment 5：
Preparation method in the present embodiment is same as Example 1, and the condition differed only in preparation process is different, this reality
It applies in example and the dosage of potassium dihydrogen phosphate is changed to 3.05g, remaining condition is constant.
After split-phase is clear, the concentration of remaining vitamin B6 in water phase is measured, by vitamin B6 in water phase before and after extraction
The extraction yield that content meter calculates vitamin B6 is 94.8%.Show that the invention extracts effect to the vitamin B6 in watermelon flesh Normal juice
Fruit is general.
Embodiment 6：
Preparation method in the present embodiment is same as Example 1, and the condition differed only in preparation process is different, this reality
It applies in example and the dosage of potassium dihydrogen phosphate is changed to 0.33g, remaining condition is constant.
After split-phase is clear, the concentration of remaining vitamin B6 in water phase is measured, by vitamin B6 in water phase before and after extraction
The extraction yield that content meter calculates vitamin B6 is 88.2%.Show that the invention extracts effect to the vitamin B6 in watermelon flesh Normal juice
Fruit is general.
Embodiment 7：
Preparation method in the present embodiment is same as Example 1, and the condition differed only in preparation process is different, this reality
The amount by chlorination-N- butyl-pyridinium ionic liquids applied in example is changed to 3.00g, remaining condition is constant.
After split-phase is clear, the concentration of remaining vitamin B6 in water phase is measured, by vitamin B6 in water phase before and after extraction
The extraction yield that content meter calculates vitamin B6 is 90.0%.Show that the invention extracts effect to the vitamin B6 in watermelon flesh Normal juice
Fruit is general.
Embodiment 8：
Preparation method in the present embodiment is same as Example 1, and the condition differed only in preparation process is different, this reality
The amount by chlorination-N- butyl-pyridinium ionic liquids applied in example is changed to 7.51g, remaining condition is constant.
After split-phase is clear, the concentration of remaining vitamin B6 in water phase is measured, by vitamin B6 in water phase before and after extraction
The extraction yield that content meter calculates vitamin B6 is 96.8%.Show that the invention extracts effect to the vitamin B6 in watermelon flesh Normal juice
Fruit is preferable.
Embodiment 9：
Preparation method in the present embodiment is same as Example 1, and the condition differed only in preparation process is different, this reality
It applies in example and the temperature for extracting environment is down to 20 DEG C, remaining condition is constant.
After split-phase is clear, the concentration of remaining vitamin B6 in water phase is measured, by vitamin B6 in water phase before and after extraction
The extraction yield that content meter calculates vitamin B6 is 86.4%.Show that the invention extracts effect to the vitamin B6 in watermelon flesh Normal juice
Fruit is bad.
Embodiment 10：
Preparation method in the present embodiment is same as Example 1, and the condition differed only in preparation process is different, this reality
It applies in example and the temperature for extracting environment is risen to 65 DEG C, remaining condition is constant.
After split-phase is clear, the concentration of remaining vitamin B6 in water phase is measured, by vitamin B6 in water phase before and after extraction
The extraction yield that content meter calculates vitamin B6 is 77.0%.Show that the invention extracts effect to the vitamin B6 in watermelon flesh Normal juice
Fruit is bad.
Embodiment 11：
Preparation method in the present embodiment is same as Example 1, and the condition differed only in preparation process is different, this reality
It applies in example and the pH for extracting environment is adjusted to 2.0, remaining condition is constant.
After split-phase is clear, the concentration of remaining vitamin B6 in water phase is measured, by vitamin B6 in water phase before and after extraction
The extraction yield that content meter calculates vitamin B6 is 55.4%.Show that the invention extracts effect to the vitamin B6 in watermelon flesh Normal juice
Fruit is bad.
Embodiment 12：
Preparation method in the present embodiment is same as Example 1, and the condition differed only in preparation process is different, this reality
It applies in example and the pH for extracting environment is adjusted to 9.0, remaining condition is constant.
After split-phase is clear, the concentration of remaining vitamin B6 in water phase is measured, by vitamin B6 in water phase before and after extraction
The extraction yield that content meter calculates vitamin B6 is 45.2%.Show that the invention extracts effect to the vitamin B6 in watermelon flesh Normal juice
Fruit is bad.
Claims (3)
- A kind of 1. application of vitamin B6 in double-aqueous phase system separation watermelon flesh, which is characterized in that the double-aqueous phase system It is made of chlorination-N- butyl-pyridiniums ionic liquid, potassium dihydrogen phosphate and water；By mass percentage, chlorination-N- butyl-pyridiniums ionic liquid is 50%~70.1% in double-aqueous phase system, biphosphate Potassium is 15.3%~24.2%, remaining is water, and three's mass fraction summation is 100%；Include the step of vitamin B6 in separation watermelon flesh：Step 1：The watermelon flesh to be separated processing that squeeze the juice is obtained into watermelon flesh Normal juice；Step 2：It is 1 in mass ratio by watermelon flesh Normal juice and the double-aqueous phase system:5 mixing are extracted, extraction temperature It it is 25 DEG C~35 DEG C, extraction pH is 4.5~5.5.
- 2. application as described in claim 1, which is characterized in that by mass percentage, chlorination-N- butyl in double-aqueous phase system Pyridine ion liquid is 55.1%, potassium dihydrogen phosphate 18.3%, remaining is water, and three's mass fraction summation is 100%.
- 3. application as described in claim 1, which is characterized in that include the step of vitamin B6 in separation watermelon flesh：Step 1：The watermelon flesh to be separated processing that squeeze the juice is obtained into watermelon flesh Normal juice；Step 2：It is 1 in mass ratio by watermelon flesh Normal juice and the double-aqueous phase system:5 mixing are extracted, extraction temperature It it is 30 DEG C, extraction pH is 5.
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| US6852229B2 (en) * | 2002-10-22 | 2005-02-08 | Exxonmobil Research And Engineering Company | Method for preparing high-purity ionic liquids |
| CN1944357A (en) * | 2005-10-09 | 2007-04-11 | 中国科学院过程工程研究所 | Recovery method for ionic liquid |
| CN104849389A (en) * | 2015-05-28 | 2015-08-19 | 华南农业大学 | Method for detecting spices in rice by ionic liquid two-aqueous-phase extraction/high performance liquid chromatography (HPLC) |
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| US6852229B2 (en) * | 2002-10-22 | 2005-02-08 | Exxonmobil Research And Engineering Company | Method for preparing high-purity ionic liquids |
| CN1944357A (en) * | 2005-10-09 | 2007-04-11 | 中国科学院过程工程研究所 | Recovery method for ionic liquid |
| CN104849389A (en) * | 2015-05-28 | 2015-08-19 | 华南农业大学 | Method for detecting spices in rice by ionic liquid two-aqueous-phase extraction/high performance liquid chromatography (HPLC) |
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