CN107556350A - Rubusoside crystal, its preparation method, food compositions and application with crystal formation A forms - Google Patents
Rubusoside crystal, its preparation method, food compositions and application with crystal formation A forms Download PDFInfo
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Abstract
The invention belongs to sweetener technical field, more particularly to a kind of Rubusoside crystal, its preparation method, food compositions and application with crystal formation A forms, the X ray powder diffraction analysis that the Rubusoside crystal with crystal formation A forms is measured using Cu K alpha rays, to spend the 2 θ angles represented at least 5.14,10.08, there is obvious characteristic diffraction peak at 10.48,12.60 and 15.18.The present invention characterizes with the Solid-state Chemistry such as XRD, DSC, TGA analysis means to the crystal, it is found that the crystal has the advantages that crystallinity height, good water solubility, stability are high, suitable for more widely using field.Preparation method of the present invention is simple, easily operated, more, the favorable reproducibility of selectivity, can stably obtain target crystal formation.
Description
Technical field
The invention belongs to sweetener technical field, more particularly to a kind of Rubusoside crystal with crystal formation A forms, its preparation
Method, food compositions and application.
Background technology
Steviol glycoside is the diterpene stevia rebaudianum alcohol glycoside mixture general name extracted from STEVIA REBAUDIANA, and its sugariness is about sucrose
200-350 times, but heat is only the 1/300 of sucrose, is a kind of natural non-thermal type food additives (sweetener).Stevioside
Glycosides or a kind of functional food additives, have the biology such as treatment diabetes, anti-caries, hypotensive, anti-inflammatory, antitumor living
Property.Recently as increase of the people to healthy natural sweetener demand, steviol glycoside turns into international the third-largest situation of selling well high power sweet tea
Taste agent and it is described as " the 3rd sugar source ".Steviol glycoside containing stevioside, stevioside A-F glycosides, steviolbioside, Du Ke glycosides A etc. into
Point, wherein a variety of crystal formations preparation of many compositions, particularly stevioside A glycosides (Reb A) has been reported and patented mandate；
As patent CN103739639A and patent CN103739640A report the crystal formation 7 and crystal formation 9 of stevioside A glycosides, two kinds of crystalline substances respectively
Type is respectively provided with the advantages of crystallinity is high, dissolubility is good, stability is high.
Rubusoside (Rubusoside, RU) is the stevioside glycosides compound that a kind of sugariness is about 200 times of sweetness of cane sugar,
It is one of main steviol glycoside in STEVIA REBAUDIANA, its structural formula is as follows：
The maximum source of natural Rubusoside is Sweet tea tree, next to that STEVIA REBAUDIANA.Patent CN106243164A reports one kind
The method that Rubusoside is extracted from sweet tea, patent CN102250990A are reported with beta galactosidase catalyzing hydrolysis stevioside
The method that glycosides prepares Rubusoside, but the crystal formation of Rubusoside is not studied.Rubusoside has obtained U.S. FDA certification and had
" tea, sugar, medicine " 3 kinds of effects, and be added to as sweetener in beverage, candy, medicine, plurality of advantages makes it have extensively
General application prospect.Rubusoside is water-soluble relatively low at room temperature, so as to limit its application.Crystal formation can influence the thing of material
Reason stability, solubility, outward appearance even can influence mouthfeel and sugariness.This area is high, water-soluble there is an urgent need to provide a kind of crystallinity
The crystal formation that property is good, stability is high.
The content of the invention
[technical problems to be solved]
It is an object of the invention to provide a kind of Rubusoside crystal with crystal formation A forms, specifically a kind of technique letter
The acquisition of Rubusoside crystal with crystal formation A forms single, easily operated, crystallinity is high, good water solubility, stability are high.
[technical scheme]
Rubusoside crystal with crystal formation A forms, the X-ray powder diffraction that the crystal formation A is measured using Cu-K alpha rays
Analysis, there is obvious characteristic diffraction peak at the 2 θ angles at least 5.14,10.08,10.48,12.60 and 15.18 represented to spend.
More specifically, the X-ray powder diffraction that the crystal formation A is measured using Cu-K alpha rays is analyzed, to spend 2 θ represented
Value, error range are ± 1 °, withThe relative intensity of the interplanar distance d of expression and the diffraction maximum being expressed as a percentage has as follows
Feature：
More specifically, the Rubusoside crystal with crystal formation A forms, it is characterised in that the Sweet tea with crystal formation A forms
Glycosides crystal has scans the main suction in thermal analysis curue and thermogravimetic analysis (TGA) figure with identical differential shown in Fig. 2 and Fig. 3 respectively
Receive peak or indicatrix.
More specifically, the crystal formation A has shape characteristic as shown in Figure 5.
More specifically, the preparation method of the Rubusoside crystal with crystal formation A forms, the preparation method includes following step
Suddenly：
(1) the separation drying of suspension：Rubusoside under stirring at low speed is mixed into 0.3-24h with solvent first, obtains sweet tea
The suspension of tea glycosides, temperature during mixing is in 0 DEG C to the scope being less than at 1-2 DEG C of solvent boiling point；Above-mentioned suspension is filtered
Or centrifugation, gained solid produce the white Rubusoside crystal with crystal formation A forms after drying；
(2) the separation drying of filtrate (or supernatant after centrifugation)：The clarification obtained after step (1) is filtered or centrifuged is molten
Liquid, is cooled to certain temperature, chilling temperature 0 DEG C-be less than 5-20 DEG C of solvent boiling point in the range of；The white solid of precipitation is done
It is dry, produce the Rubusoside crystal with crystal formation A forms；Or the settled solution after step (1) is filtered or centrifuged, it is placed in 10-
Volatilized in 60 DEG C under certain temperature, gained solid after filtering is dried, also obtains the Rubusoside crystal with crystal formation A forms.
More specifically, in step (1), the dry purity of the Rubusoside is 50%-100%, and the mixing speed is not
Higher than 30rpm.
More specifically, the solvent is water, methanol, ethanol, isopropanol, 3- methyl-1-butanols, acetonitrile, acetone, acetic acid first
It is more than one or both of ester, Ethyl formate or isopropyl acetate.
Described drying mode, which includes normal pressure, to be dried and is dried in vacuo.
The invention provides it is a kind of containing described Rubusoside crystal with crystal formation A forms and preparation method thereof food,
The application of beverage and medicine.
[beneficial effect]
The preparation method of Rubusoside crystal provided by the invention with crystal formation A forms, its technique is simple, it is easily operated,
The Rubusoside crystal with crystal formation A forms, and obtained product can be made by a variety of methods, crystallinity is high, stability is high, water
Dissolubility is good.
Brief description of the drawings
Fig. 1 is X-ray powder diffraction (XRD) figure of the Rubusoside crystal provided by the invention with crystal formation A forms；
Fig. 2 is differential scanning heat analysis (DSC) figure of the Rubusoside crystal provided by the invention with crystal formation A forms；
Fig. 3 is thermogravimetic analysis (TGA) (TG) figure of the Rubusoside crystal provided by the invention with crystal formation A forms；
Fig. 4 is infrared spectrum (IR) figure of the Rubusoside crystal provided by the invention with crystal formation A forms；
Fig. 5 is the Rubusoside crystal polarized light microscopy figure provided by the invention with crystal formation A forms；
Fig. 6 figures are the Rubusoside crystal provided by the invention with crystal formation A forms in 40 DEG C, the lower storage half of humidity 75%
Efficient liquid phase (HPLC) figure in year.
Embodiment
With reference to specific embodiment, the present invention is further illustrated, but the present invention is not subject in any way
Limitation, based on present invention teach that any conversion or replacement made, belong to protection scope of the present invention.
Embodiment one：
The Rubusoside that 25g purity is 80% is mixed with 100mL water, 24h is stirred under 30rpm at 10 DEG C, obtains Sweet tea
The suspension of glycosides；Above-mentioned suspension is filtered, gained solid is dried in vacuo at 40 DEG C, produces the white with crystal formation A forms
Rubusoside crystal.
The filtrate obtained after above-mentioned suspension is filtered is cooled to 40 DEG C, separates out white solid, by this solid in 100 DEG C of bakings
The Rubusoside crystal with crystal formation A forms is produced after dry.
Embodiment two：
The Rubusoside that 15g purity is 99.5% is mixed with 100mL 95% methanol aqueous solution, at 20 DEG C under 10rpm
1h is stirred, obtains the suspension of Rubusoside；Above-mentioned suspension is centrifuged, gained solid produces after being dried in vacuo at 25 DEG C to be had
The white Rubusoside crystal of crystal formation A forms.
Obtained filtrate is cooled to 0 DEG C after above-mentioned suspension is centrifuged, and separates out white solid, by this solid at 25 DEG C it is true
Sky produces the Rubusoside crystal with crystal formation A forms after drying.
Embodiment three：
The Rubusoside that 35g purity is 55% is mixed with 100mL 97% isopropanol, stirred at 40 DEG C under 20rpm
0.5h, obtain the suspension of Rubusoside；Above-mentioned suspension is centrifuged, gained solid is produced after being dried in vacuo at 45 DEG C with crystalline substance
The white Rubusoside crystal of type A forms.
The settled solution that centrifuged suspension is obtained again is cooled to 10 DEG C, separates out white solid, by gained solid after filtering
It is dried in vacuo at 45 DEG C, produces the Rubusoside crystal with crystal formation A forms.
Example IV：
The Rubusoside that 20g purity is 65% is mixed with 100mL 90% ethanol, 5h is stirred under 5rpm at 15 DEG C, obtains
To the suspension of Rubusoside；Above-mentioned suspension is filtered, gained solid is produced after being dried in vacuo at 40 DEG C with crystal formation A forms
White Rubusoside crystal；The settled solution obtained after filtering is placed in evaporation of solvent at 40 DEG C again, by gained solid in 40
It is dried in vacuo at DEG C, that is, obtains the Rubusoside crystal with crystal formation A forms.
Embodiment five：
The Rubusoside that 5g purity is 90% is mixed with 100mL acetone, 4h is stirred under 5rpm at 0 DEG C, obtains Rubusoside
Suspension；Above-mentioned suspension is filtered, gained solid volatilizees at 20 DEG C and is dried in vacuo at 20 DEG C, produces with crystal formation
The white Rubusoside crystal of A forms.The settled solution obtained after filtering is placed in evaporation of solvent at 20 DEG C again, by gained solid
It is dried in vacuo at 20 DEG C, that is, obtains the Rubusoside crystal with crystal formation A forms.
Embodiment six：
The Rubusoside that 15g purity is 91.5% is mixed with 100mL 65% acetonitrile solution, at 20 DEG C under 10rpm
10h is stirred, obtains the suspension of Rubusoside；Above-mentioned suspension is centrifuged, gained solid produces tool after being dried in vacuo at 35 DEG C
There is the white Rubusoside crystal of crystal formation A forms.
Embodiment seven：
The Rubusoside that 8g purity the is 75% isopropanol-isopropyl acetate solution isometric with 100mL is mixed, at 60 DEG C
0.5h is stirred under 30rpm, obtains the suspension of Rubusoside；Above-mentioned suspension is filtered, then obtained settled solution is cooled down
To 40 DEG C, white solid is separated out, obtained solid is produced into the Rubusoside crystal with crystal formation A forms after 100 DEG C of drying.
Embodiment eight：
Rubusoside methyl acetate-the ethanol solution isometric with 100mL that 10g purity is 65% is mixed, at 5 DEG C
18h is stirred under 5rpm, obtains the suspension of Rubusoside；Above-mentioned suspension is filtered, then the settled solution obtained after filtering is put
Volatilization is concentrated into the 10% of original volume at 60 DEG C, and the solid obtained after filtering is dried in vacuo at 35 DEG C, that is, had
The Rubusoside crystal of crystal formation A forms.
Embodiment nine：
The Rubusoside that 3g purity is 90% is mixed with 100mL 3- methyl-1-butanols, stirred at 0 DEG C under 10rpm
20h, obtain the suspension of Rubusoside；Above-mentioned suspension is centrifuged, gained solid volatilized at 70 DEG C after at 45 DEG C vacuum
Dry, produce the white Rubusoside crystal with crystal formation A forms.
Embodiment ten：
The Rubusoside that 2g purity is 90% is mixed with 100mL methyl acetates, 20h is stirred under 5rpm at 0 DEG C, obtains sweet tea
The suspension of tea glycosides；Above-mentioned suspension is filtered, gained solid is dried in vacuo at 30 DEG C, is produced with the white of crystal formation A forms
Color Rubusoside crystal.
Embodiment 11：
The Rubusoside that 25g purity is 91.5% is mixed with 100mL 65% acetonitrile solution, at 20 DEG C under 20rpm
10h is stirred, obtains the suspension of Rubusoside；Above-mentioned suspension is centrifuged, gained solid produces tool after being dried in vacuo at 40 DEG C
There is the white Rubusoside crystal of crystal formation A forms.
Embodiment 12：
The Rubusoside that 10g purity the is 75% isopropanol-isopropyl acetate solution isometric with 100mL is mixed, 60 DEG C
Under stir 0.5h under 10rpm, obtain the suspension of Rubusoside；Above-mentioned suspension is centrifuged, then obtained settled solution is cold
But to 40 DEG C, white solid is separated out, this solid is produced into the Rubusoside crystal with crystal formation A forms after 100 DEG C of drying.
Embodiment 13：
Rubusoside methyl acetate-the ethanol solution isometric with 100mL that 12g purity is 85% is mixed, at 5 DEG C
18h is stirred under 5rpm, obtains the suspension of Rubusoside；Above-mentioned suspension is filtered, then the settled solution obtained after filtering is put
Volatilization is concentrated into the 10% of original volume at 60 DEG C, and gained solid after filtering is dried in vacuo at 35 DEG C, that is, obtains having crystalline substance
The Rubusoside crystal of type A forms.
Embodiment 14：
By the Rubusoside and 100mL methyl acetates-ethanol solution (1 that 10g purity is 55%：8, v/v) mix, at 35 DEG C
7h is stirred under 10rpm, obtains the suspension of Rubusoside, gained solid after filtering is dried in vacuo at 35 DEG C, that is, had
The Rubusoside crystal of crystal formation A forms.
To having the Rubusoside crystal of crystal formation A forms to carry out X-ray powder diffraction analysis made from above-described embodiment
(XRD), differential scanning calorimetric analysis (DSC), thermogravimetic analysis (TGA) (TG) etc..
XRD analysis its use the diffractometers of German Brooker AXS Co., Ltds BrukerD8Advance types to be carried out in room temperature
Detection, uses Cu-K alpha rays, from 3 degree to 50 degree, sweep speed is 4 degree mins for 2 θ angle sweeps.It analyzes knot
Fruit sees Fig. 1, and XRD spectra shows that the Rubusoside crystal with crystal formation A forms is with good crystallinity made from above-described embodiment.
In sample powder X-ray powder diffraction pattern, the diffraction spectrogram obtained by specific crystal formation is often characteristic.
Because the difference of the relative amount of crystallization condition, particle diameter, mixture and other test conditions, diffraction spectrogram may produce preferentially
Orientation effect, so as to cause some bands of a spectrum in spectrogram, especially changed in the relative intensity of low angle.Therefore, diffraction maximum
Relative intensity to targeted crystal be not be characteristic, when judging whether identical with known crystal formation, it should be further noted that
Be peak position rather than their relative intensity.In addition, judge crystal formation whether when should be noted that holding organic conception, because
To be not that a diffracted ray represents a thing phase, but a set of specific " dI/I1 " data just represent a certain thing phase.It should also refer to
Go out, in the identification of mixture, the missing of part diffracted ray can be caused because content such as declines at the factor, now, without according to
Rely the whole bands of a spectrum observed in high-purity sample, or even a bands of a spectrum may also be characteristic to given crystal.
Dsc analysis：It uses the DSC Q2000 type differential scanning calorimeters of TA instrument companies of the U.S. to be detected, atmosphere
For nitrogen, firing rate is 10 degrees celsius/minutes.Its analysis result is shown in Fig. 2.
TG is analyzed：It uses the TGA-1100SF types thermogravimetric analyzer of Switzerland's plum Teller-support benefit International Trade Corporation to examine
Survey, 50-500 DEG C of temperature range, sweep speed：10K/min, purge gass：25L/min.Its analysis result is shown in Fig. 3.
Petrographic microscope photo：It uses the petrographic microscope of karr Zeiss company to be tested, and tests multiplication factor
Times.Its analysis result is shown in Fig. 4.Polarisation photo shows that the obtained Rubusoside crystal with crystal formation A forms of above-described embodiment is post
Shape crystal, there is good shape characteristic.
HPLC is analyzed：To having the Rubusoside crystal of crystal formation A forms, 40 DEG C, relative humidity made from above-described embodiment
HPLC analyses are carried out after 75% storage half a year, analyze its waters2695 liquid chromatograph for using waters Co., Ltds of the U.S.
Measure.Sample solution compound method：Accurate weighing 25-50 milligrams have the Rubusoside crystal prototype of crystal formation A forms, are put into 25 millis
In the volumetric flask risen, water-acetonitrile (7 is then added:3, v/v), solution, dissolved and be settled to scale.Sodium phosphate buffer
(specification:10mmol/L, pH value 2.6) collocation method：3.12 grams of sodium dihydrogen phosphates are dissolved into 2 liters of water, add phosphoric acid, will
PH value is adjusted to 2.6.Chromatographic column：The C18 type chromatographic columns of Kromasil companies.The μ L of sample size 10.Flow velocity 1.0mL/min.Column temperature 40
℃.Detector：210nm ultraviolet detections.Mobile phase：Acetonitrile and sodium phosphate buffer (specification：10mmol/L, pH2.6) ratio
For 32：68.Its analysis result is shown in Fig. 6, and the obtained Rubusoside crystal with crystal formation A forms of above-described embodiment is analyzed aobvious through HPLC
Show after storing half a year under the conditions of 40 DEG C, RH75%, purity is still up to 98.5%.The change of its purity is less than 1.5%.
The obtained Rubusoside crystal with crystal formation A forms of above-described embodiment, has good reappearance, and water-soluble
It is stable.Purity be 98.5%, have crystal formation A forms Rubusoside crystal in 250C, solubility is 114mg/mL in water.
Rubusoside raw material used is provided by East Platform Na Shengte bio tech ltd in above-described embodiment, from stevia rebaudianum
The enzymatic hydrolysis product of Si Tifu glycosides in extract and steviol glycoside.
Rubusoside crystal provided by the invention with crystal formation A forms can be applied to food, beverage and medicine as sweetener
In product.
Rubusoside crystal preparation method provided by the invention with crystal formation A forms can be applied to food, beverage and medicine
Preparation technology in.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
All any modification, equivalent and improvement made within refreshing and principle etc., should be included in the scope of the protection.
Claims (8)
1. the Rubusoside crystal with crystal formation A forms, it is characterised in that the X-ray that the crystal formation A is measured using Cu-K alpha rays
Powder diffraction analysis, at least there is obvious feature at 5.14,10.08,10.48,12.60 and 15.18 to spend the 2 θ angles represented
Diffraction maximum.
2. there is the Rubusoside crystal of crystal formation A forms as claimed in claim 1, it is characterised in that the crystal formation A uses Cu-K
The X-ray powder diffraction analysis that alpha ray measurement obtains, the 2 θ values (error range is ± 1 °) represented using angle, withRepresent
The relative intensity of interplanar distance d and the diffraction maximum being expressed as a percentage has following feature：
3. there is the Rubusoside crystal of crystal formation A forms as claimed in claim 1, it is characterised in that described that there is crystal formation A forms
Rubusoside crystal have and scanned respectively with identical differential shown in Fig. 2 and Fig. 3 in thermal analysis curue and thermogravimetic analysis (TGA) figure
Major absorbance peak or indicatrix.
4. the preparation method of the Rubusoside crystal with crystal formation A forms, it is characterised in that the preparation method includes following step
Suddenly：
(1) the separation drying of suspension：Rubusoside under stirring at low speed is mixed into 0.3-24h with solvent first, obtains Rubusoside
Suspension, temperature during mixing is in 0 DEG C to the scope being less than at 1-2 DEG C of solvent boiling point；By above-mentioned suspension filter or from
The heart, gained solid produce the white Rubusoside crystal with crystal formation A forms after drying；
(2) the separation drying of filtrate (or supernatant after centrifugation)：The settled solution obtained after step (1) is filtered or centrifuged,
Be cooled to certain temperature, chilling temperature 0 DEG C-be less than 5-20 DEG C of solvent boiling point in the range of；The white solid of precipitation is dried,
Produce the Rubusoside crystal with crystal formation A forms；Or the settled solution after step (1) is filtered or centrifuged, it is placed in 10-60 DEG C
Volatilized under interior certain temperature, gained solid after filtering is dried, obtains the Rubusoside crystal with crystal formation A forms.
5. the preparation method of the Rubusoside crystal with crystal formation A forms as claimed in claim 4, it is characterised in that step (1)
Described in solvent be water, methanol, ethanol, isopropanol, 3- methyl-1-butanols, acetonitrile, acetone, methyl acetate, Ethyl formate or
It is more than one or both of isopropyl acetate.
6. the preparation method of the Rubusoside crystal with crystal formation A forms as claimed in claim 4, it is characterised in that step (1)
Described in mixing speed under stirring at low speed be not higher than 30rpm.
7. a kind of food compositions, it is characterised in that the food compositions contain the tool described in claim 1-3 any one
There is the Rubusoside crystal of crystal formation A forms.
8. as described in claim any one of 1-3 with crystal formation A forms Rubusoside crystal and preparation method thereof food, drink
Application in material and medicine.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102838644A (en) * | 2012-08-23 | 2012-12-26 | 长沙绿蔓生物科技有限公司 | Production method for extracting sweet tea glucoside from sweet tea leaves |
| CN105061526A (en) * | 2015-07-23 | 2015-11-18 | 湖南华诚生物资源有限公司 | Extraction method for high purity rubusoside |
| CN105166198A (en) * | 2015-09-29 | 2015-12-23 | 重庆骄王天然产物股份有限公司 | Preparation method of high-purity rubusoside |
-
2017
- 2017-10-12 CN CN201710947380.3A patent/CN107556350A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102838644A (en) * | 2012-08-23 | 2012-12-26 | 长沙绿蔓生物科技有限公司 | Production method for extracting sweet tea glucoside from sweet tea leaves |
| CN105061526A (en) * | 2015-07-23 | 2015-11-18 | 湖南华诚生物资源有限公司 | Extraction method for high purity rubusoside |
| CN105166198A (en) * | 2015-09-29 | 2015-12-23 | 重庆骄王天然产物股份有限公司 | Preparation method of high-purity rubusoside |
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