CN103450139A - Extraction method for high-purity high-oxidative-activity aronia melanocarpa procyanidine - Google Patents
Extraction method for high-purity high-oxidative-activity aronia melanocarpa procyanidine Download PDFInfo
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Abstract
The invention provides an extraction method for high-purity high-oxidative-activity aronia melanocarpa procyanidine and belongs to the technical field of extraction and purification of procyanidine. The method comprises the following steps: as aronia melanocarpa is taken as a raw material, firstly, adopting a freeze drying technology to obtain aronia melanocarpa freeze-dried powder; then, extracting the aronia melanocarpa freeze-dried powder by adopting a supercritical CO2 extraction technology; finally, purifying the aronia melanocarpa procyanidine by adopting an AB-8 type macroporous adsorption resin purification technology. According to the extraction method, the freeze drying technology and the supercritical CO2 extraction technology are adopted so that the extraction efficiency is improved and the biological activity is kept; the macroporous resin purification technology is adopted so that the extraction purity of the aronia melanocarpa procyanidine is improved and the purity reaches to 90.1%-98.6%; the cleaning capability of the aronia melanocarpa procyanidine to DPPH (1,6-bis(diphenylphosphino)hexane) is within a range from 11.2 micrograms/milliliter to 15.6 micrograms/milliliter; the obtained procyanidine is high in purity and good in activity, can be directly applied to medicines and health-care foods.
Description
Technical field
The invention belongs to the extraction and purification technical field of pycnogenols, be specifically related to a kind ofly take that to deceive fruit gland rib Sorbus alnifloria be that raw material extracts and the method for purifying pycnogenols.
Background technology
At present, the extracting method of pycnogenols (being called for short OPC) mainly contains following several:
1, solvent method: the method is one of modal method during pycnogenols extracts, be also apply the earliest, one of method the most widely, solvent is commonly used water, methyl alcohol, ethanol, acetone, sherwood oil, though its technique is simple, but a large amount of uses of polarity noxious solvent, very easily produce the problem of the aspects such as environmental pollution, production safety and product safety, high energy consumption is one of outstanding problem in the method application always simultaneously.The people such as Chen Jian adopt the methanol extraction vaccinium oxycoccus pigment, methanol concentration 80%, yield 4.29%(is shown in Chen Jian, Sun Aidong, Gao Xuejuan; Tao Xiao Yun, Wang Shanshan. the extraction of vaccinium oxycoccus pigment and the research of oxidation-resistance [J]. Beijing Forestry University's journal, 2011,33(2): 126-129), its solvent strength is too high, poor stability, and yield is low.
2, assisted Extraction is followed the example of or comprehensive extraction method: the method is usually on the basis of solvent method, add Aided Physical, chemical-biological method, promote the stripping of pycnogenols, thereby reach the purpose that improves extraction yield, usually adopt the methods such as ultrasonic wave, ultra-high voltage, pulsed electric field, microwave, cellulase hydrolysis, because industrialization apparatus expensive, supporting application cost are high, its physical principle easily causes the pycnogenols modification simultaneously, reduce resistance of oxidation, restricting the commercial application of householder method.The people such as Xiao Lixia are on the basis of extraction using alcohol, adopt respectively microwave, cellulase and ultrasonic-assisted extraction Proanthocyanidins from Grape Seeds, result shows that the best approach is that microwave-assisted extracts, its optimum process condition: solid-liquid ratio 1:25 (g/mL), volume fraction of ethanol 80%, microwave time 40s, microwave power 115W, the extraction yield of pycnogenols is that 10.70%(is shown in Xiao Lixia, He Zhigui, Zhu Yong, Zeng Qingwen, Hu Boran. Proanthocyanidins from Grape Seeds extraction process [J]. Food science, 2011,32(20): 89-94).Microwave is as a kind of electric wave, and its electric field also has the wedge angle centrality, i.e. edge effect, and it is very fast that this effect heats up the corner of material, even can these parts are burned.Pycnogenols, as a kind of active substance, easily loses activity at microwave condition, reduces resistance of oxidation.
3, supercritical methanol technology: the method is to utilize the dissolving power of supercutical fluid and the relation of its density, utilizes pressure and temperature to carry out the impact of supercutical fluid dissolving power.Under supercritical state, supercutical fluid is contacted with material to be separated, it is extracted the composition of polarity size, boiling point height and molecular size range selectively successively.The people such as Ye Chunhao optimize integration supercritical liquid extraction technique and macroporous adsorption resin technology, extract raisin seed oil and pycnogenols from Semen Vitis viniferae, form the integrated metallization processes of high efficiency extraction, purifying pycnogenols.Separate the pycnogenols obtained by this method and analyze procyanidin content 97.82% through the UV method, total extraction yield is 4.88%.(see Ye Chunhao, Li Shufen, Tang Shaokun. supercritical CO 2-macroporous resin separation and purification Proanthocyanidins from Grape Seeds [J]. chemical industry and engineering, 2006,23(3): 220-223).The people such as Wu Chaoxia adopt supercritical CO
2abstraction technique extracts oligomeric procyanidolics in Semen Vitis viniferae (OPC ' s), and initial analysis the formation of product.Result shows: while not using entrainment agent, can not extract OPC ' s; Methyl alcohol or ethanol can increase the extraction yield of OPC ' s during as entrainment agent, and the methyl alcohol better effects if, but overall extraction yield is still lower.Further stratographic analysis shows, contains catechin, l-Epicatechol and two kinds of dimers in product and (sees Wu Chaoxia, Meng Xianjun, Zhang Hong, Wu Chaohui. the pre-test of oligomeric procyanidolics [J] in the SCF-CO 2 Semen Vitis viniferae. Agricultural University Of Shenyang's journal, 2007,38(2): 241-243).The method application is at the early-stage, and, due to the difference of raw material, its preparation technology also has larger otherness, must carry out applied research targetedly.
Comprehensive above summary, and find by document and patent retrieval, the extraction of pycnogenols has had suitable history, but its technique mainly concentrates on solvent method, solvent adopts methyl alcohol and the acetone that cost is minimum more, and its solvent has toxicity, residual, not only seriously restricting the industry development of pycnogenols, more environment has brought very big pollution, with advocating the friendly industry of green environment today, disagrees, therefore must improve on technique.
Analysis according to U.S. Ta Fuci (Tufts) university, in 40 kinds of vegetables and fruit with anti-oxidant effect, the procyanidin content of blueberry ranks the first, its content of cultivation blueberry raw anthocyanidin is at the 0.07-0.15g/100g fresh weight, and black fruit gland rib Sorbus alnifloria procyanidin content is the 1.3-2g/100g fresh weight after testing, be 9-29 times of blueberry raw anthocyanidin content.At present, Russia and Poland are the Main Cultivation states of black fruit gland rib Sorbus alnifloria, and Korea and China are Asia Main Cultivation states, and through the development of more than ten years, the cultivated area of China has reached more than 1000 hectares.And, at Applied research fields, only only have the research report of 1 piece of black fruit gland rib Sorbus alnifloria fruit wine, the research of its feature pycnogenols and application also occur there are no report; And, adopt the technique of the pycnogenols that black fruit gland rib Sorbus alnifloria is raw material extraction high purity high anti-oxidation activity also to have no report.
Summary of the invention
The purpose of this invention is to provide a kind of technique of can industrialization extracting high purity high anti-oxidation reactive black fruit gland rib Sorbus alnifloria pycnogenols, provide simultaneously and be applicable to best freeze drying process, the supercritical CO that black fruit gland rib Sorbus alnifloria pycnogenols extracts
2extraction process, macroporous resin purification technique, the technical problem such as solve that the pycnogenols extraction yield that prior art exists is not high, inactivation, purity are low.
The research and development thinking of the extracting method of high purity high anti-oxidation reactive black fruit gland rib Sorbus alnifloria pycnogenols of the present invention is: the preparation of at first take is of high nutritive value, the pycnogenols storage rate is good, the high-quality black fruit gland rib Sorbus alnifloria dry powder of the dry exquisiteness of outward appearance is target, the procyanidin content of take has been studied the technical indicators such as different drying supports, different dry drying method, concrete drying process as index, finally obtained the design parameter of freeze drying process; Secondly, studied supercritical CO
2the processing parameter of the black fruit of extraction gland rib Sorbus alnifloria dry powder, as research object, adopt experiment of single factor, optimization of orthogonal test parameter by the consumption of the pressure of extraction, extraction temperature, solid-liquid ratio, entrainment agent, finally obtained supercritical CO
2the technique ginseng of the black fruit of extraction gland rib Sorbus alnifloria dry powder; Finally, study the purifying absorbing process of macroporous resin, studied the purification effect of different macroporous resins to pycnogenols, finally chosen AB-8 type macroporous adsorbent resin, finally obtained the suitable adsorption conditions of AB-8 type resin to black fruit gland rib Sorbus alnifloria pycnogenols.
The technical scheme that technical solution problem of the present invention is taked is as follows:
The extracting method of high purity high anti-oxidation reactive black fruit gland rib Sorbus alnifloria pycnogenols, comprise the steps:
The first step, deceiving fruit gland rib Sorbus alnifloria with tissue mashing machine, to grind to form homogeneous fine and closely woven puree standby;
Second step, the puree that the first step grinding is obtained evenly tile to refrigerator tray, and the thickness of puree was 3-4mm ,-40 ℃ of lower quick-frozens 4 hours, condenser temperature is-50 ℃, then dry 18h on freeze drier, smashed 100 mesh sieves after drying, obtains black fruit gland rib Sorbus alnifloria lyophilized powder;
The 3rd step, the black fruit gland rib Sorbus alnifloria lyophilized powder that second step is obtained carry out supercritical CO
2extraction, take quantitative black fruit gland rib Sorbus alnifloria lyophilized powder and put into extractor, and pass into CO in tank
2, setting extracting pressure by control panel is that 30-40MPa, extraction temperature are 40-50 ℃, extraction time 90min, solid-liquid ratio 1:1.08, with the entrainment agent pump, adds concentration 40-70% ethanol as entrainment agent, receives the extract obtained in separating still;
The 4th step, the AB-8 type purification with macroreticular resin for extract that the 3rd step is obtained, the adsorption column diameter is 24mm, and adsorption column aspect ratio value is 10, and the loading flow velocity is 200-240BVh
-1, applied sample amount is 4 times of resin volume, and the pH value is 3, and adsorption temp is 25 ℃, and desorption liquid is the ethanol that concentration is 40-60%, inhales de-flow velocity 110-130BVh
-1, desorption temperature is 50 ℃, obtains the black fruit gland rib Sorbus alnifloria pycnogenols of high purity high anti-oxidation activity.
The invention has the beneficial effects as follows: the present invention adopts Freeze Drying Technique and supercritical CO
2the extraction process that abstraction technique combines, evaded organic solvent environmental problem and safety problem, greatly reduces the resistance of oxidation loss in leaching process; Secondly, adopt the macroporous resin purification technology, guaranteed maximum extracted rate and the purity of pycnogenols, Technology is suitable for the black fruit of modern industry production high purity gland rib Sorbus alnifloria pycnogenols.Owing to having adopted Freeze Drying Technique and supercritical CO
2abstraction technique, improve extraction efficiency and kept biological activity, adopt the macroporous resin purification technology to improve the DNA purity of black fruit gland rib Sorbus alnifloria pycnogenols, its purity reaches 90.1-98.6%, black fruit gland rib Sorbus alnifloria pycnogenols is 11.2-15.6 μ g/mL to the IC50 of the removing ability of DPPH, the gained pycnogenols, because its purity is high, the activity is good, can directly apply in medicine, protective foods.
Embodiment
Below in conjunction with embodiment, the present invention is described in further details.
Embodiment mono-
Select the black fruit gland rib Sorbus alnifloria starting material of ripe anosis insect pest, with tissue mashing machine's making beating, broken slurry and be placed in-40 ℃ of quick-frozens 4 hours, the dry pan that freezes, material thickness 3-4mm, condenser temperature-50 ℃, then be placed in lyophilize 18h on freeze drier.After drying is complete, lyophilized powder is pulverized with pulverizer, then crosses 100 mesh sieve, obtains black fruit gland rib Sorbus alnifloria lyophilized powder.
Get lyophilized powder 500g, carry out supercritical CO
2pressure 35MPa, the extraction time 90min of extraction, extraction, 45 ℃ of extraction temperature, solid-liquid ratio 1:1.08,60% ethanol is as entrainment agent, with this understanding extracting procyanidins.
By supercritical CO
2aB-8 type purification with macroreticular resin for extract, adsorption column diameter 24mm, adsorption column aspect ratio value is 10, original liquid concentration 0.285mg/ml, the loading flow velocity is 220BVh
-1, pH value 3, applied sample amount is 4 times of resin volume, adsorption temp is 25 ℃, 50% ethanol-water solution desorption for eluent, eluent flow rate 120BVh
-1, 50 ℃ of desorption temperatures, after desorb, eluting rate 96.37%, and procyanidin content reaches 98.6%, extraction process extraction yield 89%.Comparison and detection shows, blueberry raw anthocyanidin is about 17.5 μ g/ml to the IC50 of the removing ability of DPPH, and black fruit gland rib Sorbus alnifloria pycnogenols is about 11.2 μ g/mL to the IC50 of the removing ability of DPPH.
Embodiment bis-
Select the black fruit gland rib Sorbus alnifloria starting material of ripe anosis insect pest, with tissue mashing machine's making beating, broken slurry and be placed in-40 ℃ of quick-frozens 4 hours, the dry pan that freezes, material thickness 3-4mm, condenser temperature-50 ℃, then be placed in lyophilize 18h on freeze drier.After drying is complete, lyophilized powder is pulverized with pulverizer, then crosses 100 mesh sieve, obtains black fruit gland rib Sorbus alnifloria lyophilized powder.
Get lyophilized powder 500g, carry out supercritical CO
245 ℃ of pressure 30MPa, extraction temperature, the extraction time 90min of extraction, extraction, solid-liquid ratio 1:1.08,60% ethanol is as entrainment agent, with this understanding extracting procyanidins.
By supercritical CO
2aB-8 type purification with macroreticular resin for extract, adsorption column diameter 24mm, adsorption column aspect ratio value is 10, original liquid concentration 0.285mg/ml, the loading flow velocity is 220BVh
-1, pH value 3, applied sample amount is 4 times of resin volume, adsorption temp is 25 ℃, 50% ethanol-water solution desorption for eluent, eluent flow rate 120BVh
-1, 50 ℃ of desorption temperatures, after desorb, eluting rate 96.11%, and procyanidin content reaches 95.8%, extraction process extraction yield 81%, this black fruit gland rib Sorbus alnifloria pycnogenols is about 12.2 μ g/mL to the IC50 of the removing ability of DPPH.
Embodiment tri-
Select the black fruit gland rib Sorbus alnifloria starting material of ripe anosis insect pest, with tissue mashing machine's making beating, broken slurry and be placed in-40 ℃ of quick-frozens 4 hours, the dry pan that freezes, material thickness 3-4mm, condenser temperature-50 ℃, then be placed in lyophilize 18h on freeze drier.After drying is complete, lyophilized powder is pulverized with pulverizer, then crosses 100 mesh sieve, obtains black fruit gland rib Sorbus alnifloria lyophilized powder.
Get lyophilized powder 500g, carry out supercritical CO
2pressure 40MPa, the extraction time 90min of extraction, extraction, 45 ℃ of extraction temperature, solid-liquid ratio 1:1.08,60% ethanol is as entrainment agent, with this understanding extracting procyanidins.
By supercritical CO
2aB-8 type purification with macroreticular resin for extract, adsorption column diameter 24mm, adsorption column aspect ratio value is 10, original liquid concentration 0.285mg/ml, the loading flow velocity is 220BVh
-1, pH value 3, applied sample amount is 4 times of resin volume, adsorption temp is 25 ℃, 50% ethanol-water solution desorption for eluent, eluent flow rate 120BVh
-1, 50 ℃ of desorption temperatures, after desorb, eluting rate 96.20%, and procyanidin content reaches 94.1%, extraction process extraction yield 78%, this black fruit gland rib Sorbus alnifloria pycnogenols is about 12.3 μ g/mL to the IC50 of the removing ability of DPPH.
Embodiment tetra-
Select the black fruit gland rib Sorbus alnifloria starting material of ripe anosis insect pest, with tissue mashing machine's making beating, broken slurry and be placed in-40 ℃ of quick-frozens 4 hours, the dry pan that freezes, material thickness 3-4mm, condenser temperature-50 ℃, then be placed in lyophilize 18h on freeze drier.After drying is complete, lyophilized powder is pulverized with pulverizer, then crosses 100 mesh sieve, obtains black fruit gland rib Sorbus alnifloria lyophilized powder.
Get lyophilized powder 500g, carry out supercritical CO
240 ℃ of pressure 35MPa, extraction temperature, the extraction time 90min of extraction, extraction, solid-liquid ratio 1:1.08,60% ethanol is as entrainment agent, with this understanding extracting procyanidins.
By supercritical CO
2aB-8 type purification with macroreticular resin for extract, adsorption column diameter 24mm, adsorption column aspect ratio value is 10, original liquid concentration 0.285mg/ml, the loading flow velocity is 220BVh
-1, pH value 3, applied sample amount is 4 times of resin volume, adsorption temp is 25 ℃, 50% ethanol-water solution desorption for eluent, eluent flow rate 120BVh
-1, 50 ℃ of desorption temperatures, after desorb, eluting rate 95,89%, and procyanidin content reaches 95.6%, extraction process extraction yield 79%, this black fruit gland rib Sorbus alnifloria pycnogenols is about 12.8 μ g/mL to the IC50 of the removing ability of DPPH.
Embodiment five
Select the black fruit gland rib Sorbus alnifloria starting material of ripe anosis insect pest, with tissue mashing machine's making beating, broken slurry and be placed in-40 ℃ of quick-frozens 4 hours, the dry pan that freezes, material thickness 3-4mm, condenser temperature-50 ℃, then be placed in lyophilize 18h on freeze drier.After drying is complete, lyophilized powder is pulverized with pulverizer, then crosses 100 mesh sieve, obtains black fruit gland rib Sorbus alnifloria lyophilized powder.
Get lyophilized powder 500g, carry out supercritical CO
250 ℃ of pressure 35MPa, extraction temperature, the extraction time 90min of extraction, extraction, solid-liquid ratio 1:1.08,60% ethanol is as entrainment agent, with this understanding extracting procyanidins.
By supercritical CO
2aB-8 type purification with macroreticular resin for extract, adsorption column diameter 24mm, adsorption column aspect ratio value is 10, original liquid concentration 0.285mg/ml, the loading flow velocity is 220BVh
-1, pH value 3, applied sample amount is 4 times of resin volume, adsorption temp is 25 ℃, 50% ethanol-water solution desorption for eluent, eluent flow rate 120BVh
-1, 50 ℃ of desorption temperatures, after desorb, eluting rate 95,66%, and procyanidin content reaches 96.1%, extraction process extraction yield 83%, this black fruit gland rib Sorbus alnifloria pycnogenols is about 13.7 μ g/mL to the IC50 of the removing ability of DPPH.
Embodiment six
Select the black fruit gland rib Sorbus alnifloria starting material of ripe anosis insect pest, with tissue mashing machine's making beating, broken slurry and be placed in-40 ℃ of quick-frozens 4 hours, the dry pan that freezes, material thickness 3-4mm, condenser temperature-50 ℃, then be placed in lyophilize 18h on freeze drier.After drying is complete, lyophilized powder is pulverized with pulverizer, then crosses 100 mesh sieve, obtains black fruit gland rib Sorbus alnifloria lyophilized powder.
Get lyophilized powder 500g, carry out supercritical CO
245 ℃ of pressure 35MPa, extraction temperature, the extraction time 90min of extraction, extraction, solid-liquid ratio 1:1.08,50% ethanol is as entrainment agent, with this understanding extracting procyanidins.
By supercritical CO
2aB-8 type purification with macroreticular resin for extract, adsorption column diameter 24mm, adsorption column aspect ratio value is 10, original liquid concentration 0.285mg/ml, the loading flow velocity is 220BVh
-1, pH value 3, applied sample amount is 4 times of resin volume, adsorption temp is 25 ℃, 50% ethanol-water solution desorption for eluent, eluent flow rate 120BVh
-1, 50 ℃ of desorption temperatures, after desorb, eluting rate 95,78%, and procyanidin content reaches 96.4%, extraction process extraction yield 76%, this black fruit gland rib Sorbus alnifloria pycnogenols is about 15.2 μ g/mL to the IC50 of the removing ability of DPPH.
Embodiment seven
Select the black fruit gland rib Sorbus alnifloria starting material of ripe anosis insect pest, with tissue mashing machine's making beating, broken slurry and be placed in-40 ℃ of quick-frozens 4 hours, the dry pan that freezes, material thickness 3-4mm, condenser temperature-50 ℃, then be placed in lyophilize 18h on freeze drier.After drying is complete, lyophilized powder is pulverized with pulverizer, then crosses 100 mesh sieve, obtains black fruit gland rib Sorbus alnifloria lyophilized powder.
Get lyophilized powder 500g, carry out supercritical CO
245 ℃ of pressure 35MPa, extraction temperature, the extraction time 90min of extraction, extraction, solid-liquid ratio 1:1.08,70% ethanol is as entrainment agent, with this understanding extracting procyanidins.
By supercritical CO
2aB-8 type purification with macroreticular resin for extract, adsorption column diameter 24mm, adsorption column aspect ratio value is 10, original liquid concentration 0.285mg/ml, the loading flow velocity is 220BVh
-1, pH value 3, applied sample amount is 4 times of resin volume, adsorption temp is 25 ℃, 50% ethanol-water solution desorption for eluent, eluent flow rate 120BVh
-1, 50 ℃ of desorption temperatures, after desorb, eluting rate 95,63%, and procyanidin content reaches 95.3%, extraction process extraction yield 79%, this black fruit gland rib Sorbus alnifloria pycnogenols is about 14.2 μ g/mL to the IC50 of the removing ability of DPPH.
Embodiment eight
Select the black fruit gland rib Sorbus alnifloria starting material of ripe anosis insect pest, with tissue mashing machine's making beating, broken slurry and be placed in-40 ℃ of quick-frozens 4 hours, the dry pan that freezes, material thickness 3-4mm, condenser temperature-50 ℃, then be placed in lyophilize 18h on freeze drier.After drying is complete, lyophilized powder is pulverized with pulverizer, then crosses 100 mesh sieve, obtains black fruit gland rib Sorbus alnifloria lyophilized powder.
Get lyophilized powder 500g, carry out supercritical CO
245 ℃ of pressure 35MPa, extraction temperature, the extraction time 90min of extraction, extraction, solid-liquid ratio 1:1.08,60% ethanol is as entrainment agent, with this understanding extracting procyanidins.
By supercritical CO
2aB-8 type purification with macroreticular resin for extract, adsorption column diameter 24mm, adsorption column aspect ratio value is 10, original liquid concentration 0.285mg/ml, the loading flow velocity is 220BVh
-1, pH value 3, applied sample amount is 4 times of resin volume, adsorption temp is 25 ℃, 40% ethanol-water solution desorption for eluent, eluent flow rate 120BVh
-1, 50 ℃ of desorption temperatures, after desorb, eluting rate 96.13%, and procyanidin content reaches 94.9%, extraction process extraction yield 88%, this black fruit gland rib Sorbus alnifloria pycnogenols is about 14.4 μ g/mL to the IC50 of the removing ability of DPPH.
Embodiment nine
Select the black fruit gland rib Sorbus alnifloria starting material of ripe anosis insect pest, with tissue mashing machine's making beating, broken slurry and be placed in-40 ℃ of quick-frozens 4 hours, the dry pan that freezes, material thickness 3-4mm, condenser temperature-50 ℃, then be placed in lyophilize 18h on freeze drier.After drying is complete, lyophilized powder is pulverized with pulverizer, then crosses 100 mesh sieve, obtains black fruit gland rib Sorbus alnifloria lyophilized powder.
Get lyophilized powder 500g, carry out supercritical CO
250 ℃ of pressure 35MPa, extraction temperature, the extraction time 90min of extraction, extraction, solid-liquid ratio 1:1.08,60% ethanol is as entrainment agent, with this understanding extracting procyanidins.
By supercritical CO
2aB-8 type purification with macroreticular resin for extract, adsorption column diameter 24mm, adsorption column aspect ratio value is 10, original liquid concentration 0.285mg/ml, the loading flow velocity is 220BVh
-1, pH value 3, applied sample amount is 4 times of resin volume, adsorption temp is 25 ℃, 60% ethanol-water solution desorption for eluent, eluent flow rate 120BVh
-1, 50 ℃ of desorption temperatures, after desorb, eluting rate 95.81%, and procyanidin content reaches 93.1%, extraction process extraction yield 89%, this black fruit gland rib Sorbus alnifloria pycnogenols is about 13.9 μ g/mL to the IC50 of the removing ability of DPPH.
Embodiment ten
Select the black fruit gland rib Sorbus alnifloria starting material of ripe anosis insect pest, with tissue mashing machine's making beating, broken slurry and be placed in-40 ℃ of quick-frozens 4 hours, the dry pan that freezes, material thickness 3-4mm, condenser temperature-50 ℃, then be placed in lyophilize 18h on freeze drier.After drying is complete, lyophilized powder is pulverized with pulverizer, then crosses 100 mesh sieve, obtains black fruit gland rib Sorbus alnifloria lyophilized powder.
Get lyophilized powder 500g, carry out supercritical CO
245 ℃ of pressure 35MPa, extraction temperature, the extraction time 90min of extraction, extraction, solid-liquid ratio 1:1.08,60% ethanol is as entrainment agent, with this understanding extracting procyanidins.
By supercritical CO
2aB-8 type purification with macroreticular resin for extract, adsorption column diameter 24mm, adsorption column aspect ratio value is 10, original liquid concentration 0.285mg/ml, the loading flow velocity is 200BVh
-1-, pH value 3, applied sample amount is 4 times of resin volume, adsorption temp is 25 ℃, 60% ethanol-water solution desorption for eluent, eluent flow rate 120BVh
-1, 50 ℃ of desorption temperatures, after desorb, eluting rate 95.47%, and procyanidin content reaches 92.1%, extraction process extraction yield 87%, this black fruit gland rib Sorbus alnifloria pycnogenols is about 14.5 μ g/mL to the IC50 of the removing ability of DPPH.
Embodiment 11
Select the black fruit gland rib Sorbus alnifloria starting material of ripe anosis insect pest, with tissue mashing machine's making beating, broken slurry and be placed in-40 ℃ of quick-frozens 4 hours, the dry pan that freezes, material thickness 3-4mm, condenser temperature-50 ℃, then be placed in lyophilize 18h on freeze drier.After drying is complete, lyophilized powder is pulverized with pulverizer, then crosses 100 mesh sieve, obtains black fruit gland rib Sorbus alnifloria lyophilized powder.
Get lyophilized powder 500g, carry out supercritical CO
245 ℃ of pressure 35MPa, extraction temperature, the extraction time 90min of extraction, extraction, solid-liquid ratio 1:1.08,60% ethanol is as entrainment agent, with this understanding extracting procyanidins.
By supercritical CO
2aB-8 type purification with macroreticular resin for extract, adsorption column diameter 24mm, adsorption column aspect ratio value is 10, original liquid concentration 0.285mg/ml, the loading flow velocity is 240BVh
-1-, pH value 3, applied sample amount is 4 times of resin volume, adsorption temp is 25 ℃, 60% ethanol-water solution desorption for eluent, eluent flow rate 120BVh
-1, 50 ℃ of desorption temperatures, after desorb, eluting rate 95.55%, and procyanidin content reaches 91.1%, extraction process extraction yield 88%, this black fruit gland rib Sorbus alnifloria pycnogenols is about 15.6 μ g/mL to the IC50 of the removing ability of DPPH.
Embodiment 12
Select the black fruit gland rib Sorbus alnifloria starting material of ripe anosis insect pest, with tissue mashing machine's making beating, broken slurry and be placed in-40 ℃ of quick-frozens 4 hours, the dry pan that freezes, material thickness 3-4mm, condenser temperature-50 ℃, then be placed in lyophilize 18h on freeze drier.After drying is complete, lyophilized powder is pulverized with pulverizer, then crosses 100 mesh sieve, obtains black fruit gland rib Sorbus alnifloria lyophilized powder.
Get lyophilized powder 500g, carry out supercritical CO
250 ℃ of pressure 35MPa, extraction temperature, the extraction time 90min of extraction, extraction, solid-liquid ratio 1:1.08,60% ethanol is as entrainment agent, with this understanding extracting procyanidins.
By supercritical CO
2aB-8 type purification with macroreticular resin for extract, adsorption column diameter 24mm, adsorption column aspect ratio value is 10, original liquid concentration 0.285mg/ml, the loading flow velocity is 220BVh
-1, pH value 3, applied sample amount is 4 times of resin volume, adsorption temp is 25 ℃, 60% ethanol-water solution desorption for eluent, eluent flow rate 110BVh
-1, 50 ℃ of desorption temperatures, after desorb, eluting rate 93.15%, and procyanidin content reaches 94.1%, extraction process extraction yield 89%, this black fruit gland rib Sorbus alnifloria pycnogenols is about 13.2 μ g/mL to the IC50 of the removing ability of DPPH.
Embodiment 13
Select the black fruit gland rib Sorbus alnifloria starting material of ripe anosis insect pest, with tissue mashing machine's making beating, broken slurry and be placed in-40 ℃ of quick-frozens 4 hours, the dry pan that freezes, material thickness 3-4mm, condenser temperature-50 ℃, then be placed in lyophilize 18h on freeze drier.After drying is complete, lyophilized powder is pulverized with pulverizer, then crosses 100 mesh sieve, obtains black fruit gland rib Sorbus alnifloria lyophilized powder.
Get lyophilized powder 500g, carry out supercritical CO
240 ℃ of pressure 35MPa, extraction temperature, the extraction time 90min of extraction, extraction, solid-liquid ratio 1:1.08,50% ethanol is as entrainment agent, with this understanding extracting procyanidins.
By supercritical CO
2aB-8 type purification with macroreticular resin for extract, adsorption column diameter 24mm, adsorption column aspect ratio value is 10, original liquid concentration 0.285mg/ml, the loading flow velocity is 220BVh
-1, pH value 3, applied sample amount is 4 times of resin volume, adsorption temp is 25 ℃, 60% ethanol-water solution desorption for eluent, eluent flow rate 130BVh
-1, 50 ℃ of desorption temperatures, after desorb, eluting rate 96.15%, and procyanidin content reaches 90.1%, extraction process extraction yield 89%, this black fruit gland rib Sorbus alnifloria pycnogenols is about 11.9 μ g/mL to the IC50 of the removing ability of DPPH.
Claims (3)
1. the extracting method of high purity high anti-oxidation reactive black fruit gland rib Sorbus alnifloria pycnogenols, is characterized in that, the method comprises the steps:
The first step, deceiving fruit gland rib Sorbus alnifloria with tissue mashing machine, to grind to form homogeneous fine and closely woven puree standby;
Second step, the puree that the first step grinding is obtained evenly tile to refrigerator tray, and the thickness of puree was 3-4mm ,-40 ℃ of lower quick-frozens 4 hours, condenser temperature is-50 ℃, then dry 18h on freeze drier, smashed 100 mesh sieves after drying, obtains black fruit gland rib Sorbus alnifloria lyophilized powder;
The 3rd step, the black fruit gland rib Sorbus alnifloria lyophilized powder that second step is obtained carry out supercritical CO
2extraction, take quantitative black fruit gland rib Sorbus alnifloria lyophilized powder and put into extractor, and pass into CO in tank
2, setting extracting pressure by control panel is that 30-40MPa, extraction temperature are 40-50 ℃, extraction time 90min, solid-liquid ratio 1:1.08, with the entrainment agent pump, adds 40-70% ethanol as entrainment agent, receives the extract obtained in separating still;
The 4th step, the AB-8 type purification with macroreticular resin for extract that the 3rd step is obtained, the adsorption column diameter is 24mm, and adsorption column aspect ratio value is 10, and the loading flow velocity is 200-240BVh
-1, applied sample amount is 4 times of resin volume, and the pH value is 3, and adsorption temp is 25 ℃, and desorption liquid is the ethanol that concentration is 40-60%, inhales de-flow velocity 110-130BVh
-1, desorption temperature is 50 ℃, obtains the black fruit gland rib Sorbus alnifloria pycnogenols of high purity high anti-oxidation activity.
2. the extracting method of high purity high anti-oxidation reactive black fruit gland rib Sorbus alnifloria pycnogenols as claimed in claim 1, is characterized in that, the described extracting pressure of the 3rd step is 35MPa, and extraction temperature is 45 ℃, the ethanol that entrainment agent is concentration 60%.
3. the extracting method of high purity high anti-oxidation reactive black fruit gland rib Sorbus alnifloria pycnogenols as claimed in claim 1, is characterized in that, the described loading flow velocity of the 4th step is 220BVh
-1, desorption liquid is that concentration is 50% ethanol, inhaling de-flow velocity is 120BVh
-1.
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