CN103087546A - Method for extracting pigments in eleocharis tuberose peel - Google Patents
Method for extracting pigments in eleocharis tuberose peel Download PDFInfo
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- CN103087546A CN103087546A CN2013100199576A CN201310019957A CN103087546A CN 103087546 A CN103087546 A CN 103087546A CN 2013100199576 A CN2013100199576 A CN 2013100199576A CN 201310019957 A CN201310019957 A CN 201310019957A CN 103087546 A CN103087546 A CN 103087546A
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- 238000000034 method Methods 0.000 title claims abstract description 37
- 239000000049 pigment Substances 0.000 title claims abstract description 29
- 241000202829 Eleocharis Species 0.000 title abstract description 10
- 235000016067 Polianthes tuberosa Nutrition 0.000 title abstract 9
- 244000014047 Polianthes tuberosa Species 0.000 title abstract 9
- 239000000706 filtrate Substances 0.000 claims abstract description 37
- 238000000605 extraction Methods 0.000 claims abstract description 29
- 239000001058 brown pigment Substances 0.000 claims abstract description 25
- 239000000047 product Substances 0.000 claims abstract description 21
- 239000000843 powder Substances 0.000 claims abstract description 16
- 108010059820 Polygalacturonase Proteins 0.000 claims abstract description 14
- 108010059892 Cellulase Proteins 0.000 claims abstract description 13
- 229940106157 cellulase Drugs 0.000 claims abstract description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000001291 vacuum drying Methods 0.000 claims abstract description 10
- 238000001035 drying Methods 0.000 claims abstract description 3
- 235000003283 Pachira macrocarpa Nutrition 0.000 claims description 54
- 235000014364 Trapa natans Nutrition 0.000 claims description 54
- 235000009165 saligot Nutrition 0.000 claims description 54
- 241001083492 Trapa Species 0.000 claims description 52
- 239000000284 extract Substances 0.000 claims description 34
- 238000000926 separation method Methods 0.000 claims description 29
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 26
- 238000010828 elution Methods 0.000 claims description 18
- 239000011347 resin Substances 0.000 claims description 16
- 229920005989 resin Polymers 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 238000006243 chemical reaction Methods 0.000 claims description 10
- 230000035484 reaction time Effects 0.000 claims description 10
- 244000285774 Cyperus esculentus Species 0.000 claims description 8
- 235000005853 Cyperus esculentus Nutrition 0.000 claims description 8
- 239000007864 aqueous solution Substances 0.000 claims description 8
- 239000010903 husk Substances 0.000 claims description 8
- 239000008213 purified water Substances 0.000 claims description 7
- 239000002253 acid Substances 0.000 claims description 6
- 239000003463 adsorbent Substances 0.000 claims description 6
- 238000007605 air drying Methods 0.000 claims description 6
- 230000020477 pH reduction Effects 0.000 claims description 6
- 238000000746 purification Methods 0.000 claims description 6
- 238000012546 transfer Methods 0.000 claims description 5
- 239000011259 mixed solution Substances 0.000 claims description 4
- 238000010521 absorption reaction Methods 0.000 claims description 2
- 238000007654 immersion Methods 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 238000011175 product filtration Methods 0.000 claims description 2
- 239000012264 purified product Substances 0.000 claims description 2
- 238000001179 sorption measurement Methods 0.000 claims description 2
- 238000004090 dissolution Methods 0.000 abstract description 3
- 238000001914 filtration Methods 0.000 abstract description 3
- 239000001913 cellulose Substances 0.000 abstract description 2
- 229920002678 cellulose Polymers 0.000 abstract description 2
- 108010093305 exopolygalacturonase Proteins 0.000 abstract 2
- 238000002386 leaching Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 9
- 230000000274 adsorptive effect Effects 0.000 description 8
- 238000002474 experimental method Methods 0.000 description 5
- 238000004140 cleaning Methods 0.000 description 4
- 238000007598 dipping method Methods 0.000 description 4
- 239000003480 eluent Substances 0.000 description 4
- 238000001704 evaporation Methods 0.000 description 4
- 230000008020 evaporation Effects 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 238000010298 pulverizing process Methods 0.000 description 4
- -1 and Substances 0.000 description 3
- 239000000084 colloidal system Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 241000196324 Embryophyta Species 0.000 description 2
- 240000001085 Trapa natans Species 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 235000013311 vegetables Nutrition 0.000 description 2
- 229920002488 Hemicellulose Polymers 0.000 description 1
- 241000287420 Pyrus x nivalis Species 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000001814 pectin Substances 0.000 description 1
- 229920001277 pectin Polymers 0.000 description 1
- 235000010987 pectin Nutrition 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000002137 ultrasound extraction Methods 0.000 description 1
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- Coloring Foods And Improving Nutritive Qualities (AREA)
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Abstract
The invention discloses a method for extracting pigments in eleocharis tuberose peel and belongs to the field of extraction of natural pigments. The method for extracting the pigments in the eleocharis tuberose peel comprises the following steps of: firstly drying and smashing the eleocharis tuberose peel to obtain eleocharis tuberose peel powder, and dissolving the eleocharis tuberose peel into an ethanol solution; secondly, adding cellulose and pectinase to carry out enzymolysis, and filtering the obtained products after the enzymolysis, so that primarily extracted filter residue is obtained; and thirdly, carrying out vacuum drying on primarily separated filtrate, so that powdery brown pigment is obtained. According to the method for extracting the pigments in the eleocharis tuberose peel, double enzymolysis is carried out on the eleocharis tuberose peel by adopting the cellulase and pectinase, and dissolution rate and leaching rate of the pigments in the eleocharis tuberose peel are increased.
Description
Technical field
The present invention relates to the extraction field of natural pigment, particularly a kind of method of pigment in extraction of chufa husk.
Background technology
water chestnut (Eleochairis tuberosa), popular name water chestnut (Water chestnut), it is the Cyperaceae Eleocharis underground bulb of aquatic herbaceous plant for many years, a kind of common natural cash crop, the good reputation that underground snow pear is arranged from ancient times, at present, the output of China water chestnut accounts for more than 95% of the world, on the south China Yangtze valley, all there is distribution the each province, a large amount of water chestnuts are used as food and carry out deep processing, produced a large amount of discarded water chestnut skins in the course of processing, the quality of discarded water chestnut skin accounts for the 20%-25% of water chestnut total mass, a large amount of water chestnut skins are thrown away, both wasted resource, produce again environmental pollution.
in prior art in order to address this problem, discarded water chestnut skin is recycled, extract natural pigment from the water chestnut skin, extracting method to natural pigment in plant in existing document is a lot, extracting method commonly used is the natural brown pigment in ultrasonic-assisted extraction water chestnut skin, concrete microwave extract method is for take 50% edible ethanol as solvent, solid-liquid ratio is 1:10, ultrasonic frequency is 20kHz, ultrasonic power is 80w, ultrasonic time is 40min, extraction temperature is 70 ℃, with this understanding, get the thick solid of brown, the extraction rate of brown pigment of water chestnut peel is 22.79%.
In realizing process of the present invention, the contriver finds that there is following problem at least in prior art:
By the pigment in the prior art extraction of chufa husk, the toughness brown pigments colloid of gained, colloid wherein wraps the brown pigments in the water chestnut skin, cause the brown pigments in the water chestnut skin not discharge, and, these colloids also are unfavorable for separation and the filtration of subsequent technique, for the later experiment that utilizes brown pigments to carry out is made troubles.
Summary of the invention
For the problem that the brown pigments that solves extraction of chufa husk in prior art can not discharge, the embodiment of the present invention provides the method for pigment in a kind of extraction of chufa husk.Described technical scheme is as follows:
The invention provides the method for pigment in a kind of extraction of chufa husk, comprise the following steps:
1. after water chestnut skin drying being pulverized, obtain water chestnut skin powder, described water chestnut skin powder is dissolved in ethanolic soln, the quality of described water chestnut skin and the volume ratio of described ethanolic soln are 1:10 ~ 1:30, make mixed solution;
2. the pH value with described mixed solution transfers to 2 ~ 4, add cellulase and polygalacturonase, the consumption of described cellulase is 0.008 ~ 0.03% of described water chestnut skin opaque amount, the consumption of described polygalacturonase is 0.008 ~ 0.03% of described water chestnut skin opaque amount, mix, carry out enzymolysis, with the product filtration of gained after enzymolysis, obtain filtrate and the filter residue of primary separation;
3. with the filtrate vacuum-drying of described primary separation, get Powdered brown pigments.
Particularly, before described product filtered, described method also comprised:
Described product is carried out microwave assisting method extract, the reaction power of described microwave assisting method is 200W ~ 400W, and the reaction times is 2min ~ 6min.
Particularly, the concentration of described ethanolic soln is 40% ~ 70%.
Particularly, the temperature of described enzymolysis is 35 ~ 55 ℃, and the time of described enzymolysis is 1h ~ 3h.
Particularly, described acid purification of aqueous solutions is that concentration is 1% ~ 3% hydrochloric acid purification of aqueous solutions.
Particularly, described vacuum drying vacuum tightness is 650 ~ 750mmHg post.
Particularly, step 2. after, step 3. before, described method also comprises:
Described filter residue is dissolved with acid purification of aqueous solutions, and 2. the aqueous solution of gained extract according to step again, obtains filtrate and the filter residue of secondary separation, and the filtrate of described primary separation is carried out vacuum-drying with described secondary filtrate of separating.
Further, after the filtrate that obtains described secondary separation and filter residue, step 3. before, described method also comprises:
1. with the filtrate of described primary separation with described secondary filtrate of separating after adsorption resin column absorption, use the ethanolic soln wash-out, described elution flow rate is 0.5 ~ 2.5 times of column volume per hour, elution volume is 1.5 ~ 3.5 times of column volumes, use again hydrochloric acid purified water wash-out, elution flow rate is 1 ~ 3 times of column volume per hour, collects elutriant;
2. with described elutriant concentrated evaporate to dryness at the temperature of 30 ℃ ~ 50 ℃, obtain purified product.
Particularly, described polymeric adsorbent is macroporous adsorbent resin, and model is HPD-600, is that 1.0 ~ 3.0 hydrochloric acid soln carries out acidification with the pH value before using, then is alcohol immersion 20 ~ 24h of 80% with concentration, natural air drying.
Particularly, the filtrate of described primary separation and the described secondary filtrate flow that separates are 1 ~ 3 times of column volume per hour through the speed of polymeric adsorbent.
Particularly, the pH value of described ethanolic soln is 1.0 ~ 3.0, and concentration is 75% ~ 95%.
Particularly, the pH value of described hydrochloric acid purified water is 1.0 ~ 3.0.
Particularly, step 1. in, be that 40 ~ 100 described water chestnut skin of purpose powder are dissolved in described ethanolic soln with fineness.
The beneficial effect that the technical scheme that the embodiment of the present invention provides is brought is: the method for pigment in a kind of extraction of chufa husk provided by the invention, because the water chestnut intracutaneous exists more Mierocrystalline cellulose, hemicellulose and pectin substance, not only affect the release of brown pigments, and bring difficulty for again separation and the filtration of subsequent technique, the present invention adopts cellulase and polygalacturonase to carry out double enzymolysis to the water chestnut skin, double enzymolysis is beneficial to the broken wall of vegetable cell, improves dissolution rate and the solubility rate of pigment in the water chestnut skin.
Embodiment
For making the purpose, technical solutions and advantages of the present invention clearer, below embodiment of the present invention is described further in detail.
Reference examples
with after cleaning water chestnut skin that nature dries and pulverizing, obtain water chestnut skin powder, cross 40 mesh sieves, the water chestnut skin powder of getting after 20g sieves is placed in extraction flask, adding concentration is 50% ethanolic soln 200mL, carry out microwave-assisted and extract pigment, wherein, reaction power is 200W, reaction times is 6min, filter and extract product, obtain filtrate and the filter residue of primary separation, be that 1% hydrochloric acid-pure water solution 300mL repeats to extract once with this filter residue concentration, the reaction power that microwave-assisted extracts is 200W, reaction times is 6min, filter and extract product, obtain filtrate and the filter residue of secondary separation, being concentrated into the filtrate of primary separation and the secondary filtrate of separating mixing approximately, 250mL carries out the purifying experiment, adopting model is the macroporous adsorptive resins of HPD-600, this macroporous adsorptive resins is that 1.0 hydrochloric acid carries out acidification with the pH value before use, be 80% alcohol solution dipping 20h again with concentration, natural air drying, to extract the product upper prop and carry out purifying, be 1 times of column volume per hour through the flow velocity of resin, pH value as the ethanolic soln of eluent is 1.0, concentration is 75%, elution flow rate is 1 times of column volume per hour, elution volume is 1.5 times of column volumes, wash-out again, the pH value of its hydrochloric acid purified water is 1.0, and elution flow rate is 3 times of column volumes per hour, elutriant with Rotary Evaporators 30 ℃ of lower evaporation concentration to doing, with extract 40 ℃ of lower vacuum-dryings, its vacuum tightness is the 750mmHg post, obtains the brown pigments extract and is used for contrast, and its pigment extraction yield is about 22%.
Embodiment one
The embodiment of the present invention is compared with reference examples increases the double enzymolysis step, specific as follows:
with after cleaning water chestnut skin that nature dries and pulverizing, obtain water chestnut skin powder, cross 40 mesh sieves, the water chestnut skin powder of getting after 20g sieves is placed in extraction flask, adding concentration is 50% ethanolic soln 200mL, then add cellulase and polygalacturonase, wherein, the consumption of cellulase is 0.008% of water chestnut skin grain weight amount, the consumption of polygalacturonase is water chestnut skin grain weight amount 0.03%, stir, transfer pH to 2, be under 35 ℃ in temperature, enzymolysis 1h, proceed again microwave-assisted and extract pigment, wherein, reaction power is 200W, reaction times is 6min, filter and extract product, obtain filtrate and the filter residue of primary separation, be that 1% hydrochloric acid-pure water solution 300mL repeats to extract once with this filter residue concentration, the reaction power that microwave-assisted extracts is 200W, reaction times is 6min, filter and extract product, obtain filtrate and the filter residue of secondary separation, being concentrated into the filtrate of primary separation and the secondary filtrate of separating mixing approximately, 250mL carries out the purifying experiment, adopting model is the macroporous adsorptive resins of HPD-600, this macroporous adsorptive resins is that 1.0 hydrochloric acid carries out acidification with the pH value before use, be 80% alcohol solution dipping 20h again with concentration, natural air drying, to extract the product upper prop and carry out purifying, be 1 times of column volume per hour through the flow velocity of resin, pH value as the ethanolic soln of eluent is 1.0, concentration is 75%, elution flow rate is 1 times of column volume per hour, elution volume is 1.5 times of column volumes, wash-out again, the pH value of its hydrochloric acid purified water is 1.0, elution flow rate is 3 times of column volumes per hour, elutriant is extremely done 30 ℃ of lower evaporation concentration with Rotary Evaporators, with extract 40 ℃ of lower vacuum-dryings, its vacuum tightness is the 750mmHg post, obtain Powdered brown pigments 5.04g, the pigment extraction yield is 25.2%, improved 12.23% with the pigment extraction yield that reference examples gained brown pigments extract is compared the embodiment of the present invention and provided, improved 35.89% with the look valency extraction yield of reference examples gained brown pigments extract, the extraction product that the embodiment of the present invention provides is without gluey material, and, brown pigments in the water chestnut skin is effectively discharged.
Embodiment two
The embodiment of the present invention is compared with reference examples increases the double enzymolysis step, specific as follows:
with after cleaning water chestnut skin that nature dries and pulverizing, obtain water chestnut skin powder, cross 60 mesh sieves, the water chestnut skin powder of getting after 15g sieves is placed in extraction flask, adding concentration is 70% ethanolic soln 270mL, then add cellulase and polygalacturonase, wherein, the consumption of cellulase is 0.01% of water chestnut skin grain weight amount, the consumption of polygalacturonase is water chestnut skin grain weight amount 0.01%, stir, transfer pH to 3, be under 45 ℃ in temperature, enzymolysis 2h, proceed again microwave-assisted and extract pigment, wherein, reaction power is 280W, reaction times is 4min, filter and extract product, obtain filtrate and the filter residue of primary separation, be that 2% hydrochloric acid-pure water solution 270mL repeats to extract once with this filter residue concentration, the reaction power that microwave-assisted extracts is 280W, reaction times is 4min, filter and extract product, obtain filtrate and the filter residue of secondary separation, being concentrated into the filtrate of primary separation and the secondary filtrate of separating mixing approximately, 250mL carries out the purifying experiment, adopting model is the macroporous adsorptive resins of HPD-600, this macroporous adsorptive resins is that 2.0 hydrochloric acid carries out acidification with the pH value before use, be 80% alcohol solution dipping 22h again with concentration, natural air drying, to extract the product upper prop and carry out purifying, be 2 times of column volumes per hour through the flow velocity of resin, pH value as the ethanolic soln of eluent is 2.0, concentration is 80%, elution flow rate is 1.5 times of column volumes per hour, elution volume is 2.5 times of column volumes, wash-out again, the pH value of its acid purified water is 2.0, elution flow rate is 2 times of column volumes per hour, elutriant is extremely done 40 ℃ of lower evaporation concentration with Rotary Evaporators, with extract 35 ℃ of lower vacuum-dryings, its vacuum tightness is the 700mmHg post, obtain Powdered brown pigments 3.825g, the pigment extraction yield is 25.5%, improved 12.57% with the pigment extraction yield that reference examples gained brown pigments extract is compared the embodiment of the present invention and provided, improved 36.25% with the look valency extraction yield of reference examples gained brown pigments extract, the extraction product that the embodiment of the present invention provides is without gluey material, and, brown pigments in the water chestnut skin is effectively discharged.
Embodiment three
The embodiment of the present invention is compared with reference examples increases the double enzymolysis step, specific as follows:
with after cleaning water chestnut skin that nature dries and pulverizing, obtain water chestnut skin powder, cross 100 mesh sieves, the water chestnut skin powder of getting after 25g sieves is placed in extraction flask, adding concentration is 40% ethanolic soln 750mL, then add cellulase and polygalacturonase, wherein, the consumption of cellulase is 0.03% of water chestnut skin grain weight amount, the consumption of polygalacturonase is water chestnut skin grain weight amount 0.008%, stir, transfer pH to 4, be under 50 ℃ in temperature, enzymolysis 3h, proceed again microwave-assisted and extract pigment, wherein, reaction power is 400W, reaction times is 2min, filter and extract product, obtain filtrate and the filter residue of primary separation, be that 3% hydrochloric acid-pure water solution 500mL repeats to extract once with this filter residue concentration, the reaction power that microwave-assisted extracts is 400W, reaction times is 2min, filter and extract product, obtain filtrate and the filter residue of secondary separation, being concentrated into the filtrate of primary separation and the secondary filtrate of separating mixing approximately, 250mL carries out the purifying experiment, adopting model is the macroporous adsorptive resins of HPD-600, this macroporous adsorptive resins is that 3.0 hydrochloric acid carries out acidification with the pH value before use, be 80% alcohol solution dipping 24h again with concentration, natural air drying, to extract the product upper prop and carry out purifying, be 3 times of column volumes per hour through the flow velocity of resin, pH value as the ethanolic soln of eluent is 3.0, concentration is 95%, elution flow rate is 2.5 times of column volumes per hour, elution volume is 3.5 times of column volumes, wash-out again, the pH value of its acid purified water is 3.0, elution flow rate is 3 times of column volumes per hour, elutriant is extremely done 50 ℃ of lower evaporation concentration with Rotary Evaporators, with extract 30 ℃ of lower vacuum-dryings, its vacuum tightness is the 650mmHg post, obtain Powdered brown pigments 6.25g, the pigment extraction yield is 25.0%, improved 11.98% with the pigment extraction yield that reference examples gained brown pigments extract is compared the embodiment of the present invention and provided, improved 35.45% with the look valency extraction yield of reference examples gained brown pigments extract, the extraction product that the embodiment of the present invention provides is without gluey material, and, brown pigments in the water chestnut skin is effectively discharged.
The present invention adopts cellulase and polygalacturonase to carry out double enzymolysis and microwave assisting method to the broken wall of vegetable cell to the water chestnut skin, the coupling of two kinds of methods more is conducive to the raising of dissolution rate and the solubility rate of pigment in the water chestnut skin, and will extract product and carry out purifying, finally obtain the powder of brown pigments, look valency and the purity of this powder all increase significantly, can be directly as foodstuff additive.
The above is only preferred embodiment of the present invention, and is in order to limit the present invention, within the spirit and principles in the present invention not all, any modification of doing, is equal to replacement, improvement etc., within all should being included in protection scope of the present invention.
Claims (10)
1. the method for pigment in an extraction of chufa husk, is characterized in that, comprises the following steps:
1. water chestnut skin drying is pulverized, obtained water chestnut skin powder, described water chestnut skin powder is dissolved in ethanolic soln, the quality of described water chestnut skin and the volume ratio of described ethanolic soln are 1:10 ~ 1:30, make mixed solution;
2. the pH value with described mixed solution transfers to 2 ~ 4, add cellulase and polygalacturonase, the consumption of described cellulase is 0.008 ~ 0.03% of described water chestnut skin opaque amount, the consumption of described polygalacturonase is 0.008 ~ 0.03% of described water chestnut skin opaque amount, mix, carry out enzymolysis, with the product filtration of gained after enzymolysis, obtain filtrate and the filter residue of primary separation;
3. with the filtrate vacuum-drying of described primary separation, get Powdered brown pigments.
2. extracting method according to claim 1, is characterized in that, before described product filtered, described method also comprised:
Described product is carried out microwave assisting method extract, the reaction power of described microwave assisting method is 200W ~ 400W, and the reaction times is 2min ~ 6min.
3. extracting method according to claim 1, is characterized in that, the concentration of described ethanolic soln is 40% ~ 70%.
4. extracting method according to claim 1, is characterized in that, the temperature of described enzymolysis is 35 ~ 55 ℃, and the time of described enzymolysis is 1h ~ 3h.
5. extracting method according to claim 1, is characterized in that, described acid purification of aqueous solutions is that concentration is 1% ~ 3% hydrochloric acid purification of aqueous solutions.
6. extracting method according to claim 1, is characterized in that, step 2. after, step 3. before, described method also comprises:
The filter residue of described primary separation is dissolved with acid purification of aqueous solutions, and 2. the aqueous solution of gained extract according to step again, obtains filtrate and the filter residue of secondary separation, and the filtrate of described primary separation is carried out vacuum-drying with described secondary filtrate of separating.
7. extracting method according to claim 6, is characterized in that, after the filtrate that obtains described secondary separation and filter residue, step 3. before, described method also comprises:
1. with the filtrate of described primary separation with described secondary filtrate of separating after adsorption resin column absorption, use the ethanolic soln wash-out, described elution flow rate is 0.5 ~ 2.5 times of column volume per hour, elution volume is 1.5 ~ 3.5 times of column volumes, use again hydrochloric acid purified water wash-out, elution flow rate is 1 ~ 3 times of column volume per hour, collects elutriant;
2. with described elutriant concentrated evaporate to dryness at the temperature of 30 ℃ ~ 50 ℃, obtain purified product.
8. extracting method according to claim 7, is characterized in that, described polymeric adsorbent is macroporous adsorbent resin, is that 1.0 ~ 3.0 hydrochloric acid soln carries out acidification with the pH value before using, then is alcohol immersion 20 ~ 24h of 80% with concentration, natural air drying.
9. extracting method according to claim 8, is characterized in that, the filtrate of described primary separation and the described secondary filtrate flow that separates are 1 ~ 3 times of column volume per hour through the speed of polymeric adsorbent.
10. extracting method according to claim 8, is characterized in that, the pH value of described ethanolic soln is 1.0 ~ 3.0, and concentration is 75% ~ 95%.
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