The extracting method of polyphenol in a kind of Caulis Sacchari sinensis scum silica frost
Technical field
The invention belongs to plant component extraction technical field, be specifically related to the extracting method of polyphenol in a kind of Caulis Sacchari sinensis scum silica frost.
Background technology
The research and development of aldehydes matter are the focus propositions in the fields such as current light industry and food, pharmaceutical chemistry.In recent years, phenol
Many physiologically actives of class material are gradually recognized by scientific circles, such as: defying age, blood sugar lowering, blood fat reducing, disease-resistant change, regulation are exempted from
Epidemic disease power etc..Aldehydes matter is the main active of cane suger material.At present, the Caulis Sacchari sinensis aldehydes matter that oneself finds has 16 kinds.Caulis Sacchari sinensis
It is temperate zone and torrid zone crops, is the raw material producing sucrose.Sugar Industry is the industry of agricultural, is inexhaustible, nexhaustible
The reproducible means of livelihood.In current sugar refining technology, the material in addition to Sucrose need to be tried one's best high by series as non-sugar impurities
The operation clarifications such as temperature, chemical reagent destruction are removed, and produce and meet the industry need to high-quality white Saccharum Sinensis Roxb. such as downstream food and chemical industry
Want.
Sugar price was relatively low in recent years, and most of sugar enterprises are in serious lossing state, and sugaring industry is badly in need of introducing
Or reform processing technology, reduce production cost, improve enterprise profit, to realize the sustainable development of self.Extract Caulis Sacchari sinensis
The nutritional health ingredient such as middle phenols, for extending tradition sugaring industrial chain, to realize reducing enterprise cost benefit and the holding of increasing peasant income
Supervention exhibition is significant, is also the inexorable trend of social development.
Aldehydes matter in sugarcane material has been extracted and has made many-sided deep exploitation and research by Chinese scholars.Chinese invention is special
Profit ZL200610032882.5 discloses extracting method and the application thereof of leaf of Caulis Sacchari sinensis polyphenoils, Chinese invention patent
ZL201410507594.5 discloses a kind of method extracting polyphenol from Cortex Sacchari sinensis, Chinese invention patent ZL201110406170.6
Disclose a kind of method extracting aldehydes matter from sugarcane toppers.The shortcoming of these current correlation techniques is can not be with continuous print
Closed Circulation in Sugar Production technique is actual to combine, it is impossible to meet the Sugarcane juice decolorization problem that solves while functional mass in extracting Caulis Sacchari sinensis.
Summary of the invention
In place of solving the shortcoming and defect of above prior art, it is an object of the invention to provide a kind of Caulis Sacchari sinensis scum silica frost
The extracting method of middle polyphenol.
The object of the invention is achieved through the following technical solutions:
In a kind of Caulis Sacchari sinensis scum silica frost, the extracting method of polyphenol, comprises the steps:
(1) with the Cane Mixed Juice scum silica frost obtained during cane sugar manufacture or sugarcane syrup scum silica frost as raw material, by solid-liquid ratio
For 1:(2~10) ratio of (w/v), the ethanol solution that concentration is 40%~80% (v/v) the extraction Caulis Sacchari sinensis adding pH 2~6 floats
Polyphenol in slag raw material;Opening ultrasound wave simultaneously and carry out auxiliary extraction, ultrasound condition is: ultrasound intensity 10W/cm2~40W/cm2, super
Acoustic frequency 2 × 104Hz~2 × 109Hz;After extraction time 30min~120min, filter, obtain the filtrate of filtering residue and extraction;
(2) in dehydrated alcohol: in step (1), filtrate is than being (5~10): the ratio of 1 (v/v), and dehydrated alcohol is added step
Suddenly in (1) gained filtrate, stirring 2min~10min, then static 12h~48h under conditions of 2 DEG C~5 DEG C, centrifugal sedimentation divides
From, collect upper solution;
(3) upper solution collected in step (2) is concentrated at temperature 55 DEG C~75 DEG C, be concentrated into original volume 1/20
~when 1/10, stop, obtaining concentrated solution and reclaim the alcohol solvent distilled out;
(4) by the concentrated solution in step (3) through macroporous resin adsorption, macroporous resin and the effluent of adsorbing polyphenols are obtained,
Then the macroporous resin of adsorbing polyphenols is carried out eluting, obtain polyphenol eluent;
(5) the polyphenol eluent obtained in step (4) is concentrated at temperature 55 DEG C~75 DEG C, obtain Caulis Sacchari sinensis scum silica frost
In polyphenol product and reclaim the alcohol solvent that distills out;
(6) polyphenol product obtained in step (5) is dried, obtains end product.
It is sweet that Cane Mixed Juice scum silica frost or sugarcane syrup scum silica frost described in step (1) refer to that employing air-float technology process obtains
Sugarcane mix indicator technique or sugarcane syrup scum silica frost.
Described in step (4), the model of macroporous resin is D-101, DA-201, HPD-100 or DM-301.
Eluting described in step (4) refers to the ethanol solution desorbing macroporous resin that concentration is 30%~80% (v/v)
The polyphenol adsorbed.
Described in step (5), in polyphenol product, the mass fraction of moisture content is 10%~40%.
Being dried as spray drying, intake air temperature 150~220 DEG C, air outlet temperature 70~120 described in step (6)
℃。
Preparation method and the obtained product of the present invention have the advantage that and beneficial effect:
(1) present invention can extract phenol acid substance in sugarcane juice and organically combine with sugaring cleaning technique, is extracting phenolic acids thing
Sugarcane juice decolorization and the problem of process continuity is solved, for extending tradition sugaring industrial chain, to realize reducing enterprise cost while matter
The sustainable development of benefit and increasing peasant income is significant;
(2) polyphenol during the present invention uses the technique separation of sugarcane scum silica frost of safety non-toxic, environmental protection, organic solvent can be whole
Reclaim and recycle, do not produce spent process water, economic benefit and social benefit highly significant;
(3) present invention uses low temperature and high concentration precipitate with ethanol technology to remove substantial amounts of polymer substance in the filtrate of extraction, improves
The macroporous resin adsorption separation efficiency to polyphenol, can significantly reduce production cost.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described in further detail, but embodiments of the present invention are not limited to this.
Comparative example
This comparative example does not use low temperature and high concentration precipitate with ethanol technology to extract polyphenol
(1) take air-float technology during cane sugar manufacture to process the Cane Mixed Juice scum silica frost 100g obtained and put in container, so
Polyphenol in the ethanol solution 200mL that concentration is 40% (v/v) the extraction Caulis Sacchari sinensis float material of rear addition pH=2;Open super simultaneously
Sound wave carries out auxiliary extraction, and ultrasound condition is: ultrasound intensity 10W/cm2, supersonic frequency 2 × 104Hz;After extraction time 30min,
Filter, obtain the filtrate of filtering residue and extraction;
(2) filtrate of the 100mL collected in step (1) extraction is concentrated at temperature 55 DEG C, be concentrated into 27.5 ± 0.5mL
Time, stop, obtaining 27.5mL concentrated solution and reclaim the alcohol solvent distilled out;
(3) by the concentrated solution in step (2) through D-101 type macroporous resin adsorption, obtain adsorbing polyphenols macroporous resin and
Effluent, has then adsorbed many with the ethanol solution desorbing macroporous resin that the concentration of 3 times of macroporous resin volumes is 30% (v/v)
Phenol, obtains polyphenol eluent;
(4) being concentrated at temperature 55 DEG C by the polyphenol eluent obtained in step (3), the quality obtaining moisture content is divided
The alcohol solvent that several 10 ± 1% polyphenol product and recovery distill out;
(5) polyphenol product that will obtain in step (4), spray-dried, spray drying condition be intake air temperature 150 ±
2 DEG C, air outlet temperature 70 ± 2 DEG C.Detecting through liquid chromatography, product polyphenol content is 69.8%;The DPPH method detection of employing is produced
The radical scavenging activity of product is 75.2%.
Embodiment 1
(1) take air-float technology during cane sugar manufacture to process the Cane Mixed Juice scum silica frost 100g obtained and put in container, so
Polyphenol in the ethanol solution 200mL that concentration is 40% (v/v) the extraction Caulis Sacchari sinensis float material of rear addition pH=2;Open super simultaneously
Sound wave carries out auxiliary extraction, and ultrasound condition is: ultrasound intensity 10W/cm2, supersonic frequency 2 × 104Hz;After extraction time 30min,
Filter, obtain the filtrate of filtering residue and extraction;
(2) take the filtrate 100mL of the extraction that step (1) prepares, be subsequently adding dehydrated alcohol 500mL, stir 2min,
Then static 12h under conditions of 2 DEG C, centrifugal sedimentation separates, collects 550mL upper solution;
(3) the 550mL upper solution collected in step (2) is concentrated at temperature 55 DEG C, be concentrated into 27.5 ± 0.5mL
Time, stop, obtaining 27.5mL concentrated solution and reclaim the alcohol solvent distilled out;
(4) by the concentrated solution in step (3) through D-101 type macroporous resin adsorption, obtain adsorbing polyphenols macroporous resin and
Effluent, has then adsorbed many with the ethanol solution desorbing macroporous resin that the concentration of 3 times of macroporous resin volumes is 30% (v/v)
Phenol, obtains polyphenol eluent;
(5) being concentrated at temperature 55 DEG C by the polyphenol eluent obtained in step (4), the quality obtaining moisture content is divided
The alcohol solvent that several 10 ± 1% polyphenol product and recovery distill out;
(6) polyphenol product that will obtain in step (5), spray-dried, spray drying condition be intake air temperature 150 ±
2 DEG C, air outlet temperature 70 ± 2 DEG C.Detecting through liquid chromatography, product polyphenol content is 85.5%;The DPPH method detection of employing is produced
The radical scavenging activity of product is 75.3%.
The result of contrast above example shows, uses low temperature and high concentration precipitate with ethanol technology to be remarkably improved macroporous resin to many
The adsorption separation efficiency of phenol, provides robust techniques for reducing production cost.
Embodiment 2
(1) take air-float technology during cane sugar manufacture to process the Cane Mixed Juice scum silica frost 100g obtained and put in container, so
Polyphenol in the ethanol solution 1000mL that concentration is 80% (v/v) the extraction Caulis Sacchari sinensis float material of rear addition pH=6;Open super simultaneously
Sound wave carries out auxiliary extraction, and ultrasound condition is: ultrasound intensity 40W/cm2, supersonic frequency 2 × 109Hz;After extraction time 120min,
Filter, obtain the filtrate of filtering residue and extraction;
(2) take the filtrate 100mL of the extraction that step (1) prepares, be subsequently adding dehydrated alcohol 1000mL, stirring
10min, then static 48h under conditions of 5 DEG C, centrifugal sedimentation separates, and collects 1000mL upper solution;
(3) the 1000mL upper solution collected in step (2) is concentrated at temperature 75 DEG C, when being concentrated into 100mL, stop
Only, obtain 100mL concentrated solution and reclaim the alcohol solvent distilled out;
(4) by the concentrated solution in step (3) through DA-201 type macroporous resin adsorption, obtain adsorbing polyphenols macroporous resin and
Effluent, has then adsorbed many with the ethanol solution desorbing macroporous resin that the concentration of 3 times of macroporous resin volumes is 80% (v/v)
Phenol, obtains polyphenol eluent;
(5) being concentrated at temperature 75 DEG C by the polyphenol eluent obtained in step (4), the quality obtaining moisture content is divided
The alcohol solvent that several 40 ± 1% polyphenol product and recovery distill out;
(6) polyphenol product that will obtain in step (5), spray-dried, spray drying condition be intake air temperature 220 ±
2 DEG C, air outlet temperature 120 ± 2 DEG C.Detecting through liquid chromatography, product polyphenol content is 80.2%;The DPPH method detection of employing is produced
The radical scavenging activity of product is 78.6%.
Embodiment 3
(1) take air-float technology during cane sugar manufacture to process the Cane Mixed Juice scum silica frost 100g obtained and put in container, so
Polyphenol in the ethanol solution 400mL that concentration is 50% (v/v) the extraction Caulis Sacchari sinensis float material of rear addition pH=4;Open super simultaneously
Sound wave carries out auxiliary extraction, and ultrasound condition is: ultrasound intensity 20W/cm2, supersonic frequency 2 × 106Hz;After extraction time 60min,
Filter, obtain the filtrate of filtering residue and extraction;
(2) take the filtrate 100mL of the extraction that step (1) prepares, be subsequently adding dehydrated alcohol 700mL, stir 5min,
Then static 24h under conditions of 3 DEG C, centrifugal sedimentation separates, and collects 750mL upper solution;
(3) the 750mL upper solution collected in step (2) is concentrated under temperature 60 C, when being concentrated into 50mL, stops,
Obtain 50mL concentrated solution and reclaim the alcohol solvent distilled out;
(4) by the concentrated solution in step (3) through HPD-100 type macroporous resin adsorption, the macroporous resin of adsorbing polyphenols is obtained
And effluent, then adsorb with the ethanol solution desorbing macroporous resin that the concentration of 3 times of macroporous resin volumes is 60% (v/v)
Polyphenol, obtains polyphenol eluent;
(5) being concentrated under temperature 60 C by the polyphenol eluent obtained in step (4), the quality obtaining moisture content is divided
The alcohol solvent that several 30 ± 1% polyphenol product and recovery distill out;
(6) polyphenol product that will obtain in step (5), spray-dried, spray drying condition be intake air temperature 180 ±
2 DEG C, air outlet temperature 90 ± 2 DEG C.Detecting through liquid chromatography, product polyphenol content is 86.6%;The DPPH method detection of employing is produced
The radical scavenging activity of product is 79.2%.
Embodiment 4
(1) take air-float technology during cane sugar manufacture to process the sugarcane syrup scum silica frost 100g obtained and put in container, then
Add polyphenol in the ethanol solution 700mL that concentration is 60% (v/v) the extraction Caulis Sacchari sinensis float material of pH=5;Open ultrasonic simultaneously
Ripple carries out auxiliary extraction, and ultrasound condition is: ultrasound intensity 30W/cm2, supersonic frequency 2 × 107Hz;After extraction time 90min, mistake
Filter, obtains the filtrate of filtering residue and extraction;
(2) take the filtrate 100mL of the extraction that step (1) prepares, be subsequently adding dehydrated alcohol 800mL, stir 8min,
Then static 36h under conditions of 4 DEG C, centrifugal sedimentation separates, and collects 850mL upper solution;
(3) the 850mL upper solution collected in step (2) is concentrated under temperature 70 C, when being concentrated into 50mL, stops,
Obtain 50mL concentrated solution and reclaim the alcohol solvent distilled out;
(4) by the concentrated solution in step (3) through DM-301 type macroporous resin adsorption, obtain adsorbing polyphenols macroporous resin and
Effluent, has then adsorbed many with the ethanol solution desorbing macroporous resin that the concentration of 3 times of macroporous resin volumes is 50% (v/v)
Phenol, obtains polyphenol eluent;
(5) being concentrated under temperature 70 C by the polyphenol eluent obtained in step (4), the quality obtaining moisture content is divided
The alcohol solvent that several 20 ± 1% polyphenol product and recovery distill out.
(6) polyphenol product that will obtain in step (5), spray-dried, spray drying condition be intake air temperature 200 ±
2 DEG C, air outlet temperature 102 ± 2 DEG C.Detecting through liquid chromatography, product polyphenol content is 83.7%;The DPPH method detection of employing is produced
The radical scavenging activity of product is 76.9%.
Above-described embodiment is the present invention preferably embodiment, but embodiments of the present invention are not by above-described embodiment
Limit, the change made under other any spirit without departing from the present invention and principle, modify, substitute, combine, simplify,
All should be the substitute mode of equivalence, within being included in protection scope of the present invention.