CN102671017A - Method for simultaneously preparing indocalamus leaf volatile oil, total flavone and total polysaccharide - Google Patents
Method for simultaneously preparing indocalamus leaf volatile oil, total flavone and total polysaccharide Download PDFInfo
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- CN102671017A CN102671017A CN201210128161XA CN201210128161A CN102671017A CN 102671017 A CN102671017 A CN 102671017A CN 201210128161X A CN201210128161X A CN 201210128161XA CN 201210128161 A CN201210128161 A CN 201210128161A CN 102671017 A CN102671017 A CN 102671017A
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Abstract
The invention discloses a method for simultaneously preparing indocalamus leaf volatile oil, total flavone and total polysaccharide, which comprises the following steps: taking indocalamus leaf powder and adding water of 5-12 times in weight; dipping for 0-4h; extracting for 2-12h through a steam distillation method; extracting through organic solvent to obtain the volatile oil; keeping the extracted medicine liquid for later use; adding 20-50% of ethanol of 6-12 times in raw dose mass by weight into the medicine dreg; carrying out backflow extraction for 2-3 times of 0.5-1.5h each time; filtering; combining each extracted liquid and extracting the medicine liquid after extracting the volatile oil; depressurizing and concentrating so as to obtain the extractive; adding water for dissolution; making the concentration of the loading solution be 0.4-1.0 g/ml by raw dose mass; passing through macroporous resin, wherein the absorbing flow speed is 1-3 BV/h, and the resin column height ratio is 1:5-8; firstly eluting using water for 2-4 BV; depositing the eluting liquid using the ethanol; drying to obtain the polysaccharide; subsequently eluting using 40-90% of ethanol for 3-6 BV, wherein the elution flow speed is 0.8-2 BV/h; and concentrating the eluting liquid and drying to obtain the total flavone.
Description
Technical field
The present invention relates to the deep process technology field of agricultural product, particularly a kind of method of from Folium indocalami tessellati, extracting bioactive ingredients such as volatile oil, flavone and polysaccharide simultaneously.This method relates to integrated vapor distillation, macroporous resin technology, and vacuum concentration technology etc. is extracted the method for Folium indocalami tessellati bioactive ingredients.
Background technology
Folium indocalami tessellati is the leaf that grass family (Graminales) Bambusoideae (BambusoideaeNees) Indocalanmus tessellatus belongs to (Indocal.mus) plant.Mainly be distributed in each provinces and regions on the south the Changjiang river.Can wrap up Oryza glutinosa with Folium indocalami tessellati and boil into food, this food is one of traditional cuisines of the Chinese nation, and southern area has a long history in China, has special faint scent, and instant, and storage tolerance are liked by the people deeply.Modern medicine shows that Folium indocalami tessellati has effects such as clearing away heat to stop bleeding, removing toxic substances and promoting subsidence of swelling, diuresis be anticancer.Modern scientific research proves, contains functional components such as volatile oil, flavone and polysaccharide in the Folium indocalami tessellati.The natural flavor that the distinctive brown fragrance of Folium indocalami tessellati is a kind of pleasant, the volatile oil that therefrom the extracts products such as natural essence, food additive of to redevelop; Pharmacological testing proves that the indicalamus leaf extracting solution has effects such as good antitumor, anti-inflammatory, antiulcer.At present; About the patent application of Folium indocalami tessellati volatile oil, total flavones and total polysaccharides method for preparing application number being arranged is application such as 03142883.5,01111117.8, but these methods all are single extractions, and resource utilization is lower; Extraction cost is higher, unsuitable industrialized great production.
Summary of the invention
The object of the present invention is to provide a kind of method for preparing volatile oil, total flavones and total polysaccharides of from Folium indocalami tessellati, extracting simultaneously; Thereby the wasting of resources that can avoid single extraction to bring; Improve the resource utilization of Folium indocalami tessellati, reduced cost, and the big production of this method for preparing suitability for industrialized.
The object of the invention is realized through following technical scheme:
A kind of method for preparing Folium indocalami tessellati volatile oil, total flavones and total polysaccharides simultaneously, its processing step is: get the water that the Folium indocalami tessellati powder adds 5-12 times of weight (L/kg), soak 0-4h, steam distillation extracts 2-12h, gets volatile oil; Medicinal liquid is continued to employ after extracting volatile oil, and medicinal residues add in the 20-50% alcohol reflux of 6-12 times of weight of crude drug amount (L/kg) 2-3 time, each 0.5-1.5h, filtration; Behind the decompression recycling ethanol, medicinal liquid after merging each extracting solution and extracting volatile oil, concentrating under reduced pressure gets extract; Add the aqueous dispersion dissolving, making sample solution concentration in the crude drug amount is 0.4-1.0g/ml, through macroporous resin; Absorption flow velocity 1-3BV/h, the resin column blade diameter length ratio is 1: 5-8, use earlier water elution 2-3BV; The eluent ethanol precipitation, drying gets the Folium indocalami tessellati total polysaccharide extractive; Use 40-90% ethanol elution 3-5BV then, elution flow rate is 0.8-2BV/h, and this eluent concentrates, and drying gets the Folium indocalami tessellati extractive of general flavone.
Raw material Folium indocalami tessellati according to the invention derives from grass family (Graminales) Bambusoideae (BambusoideaeNees) Indocalanmus tessellatus and belongs to (Indocal.mus) wherein leaf of any one plant.
The raw material of said extraction Folium indocalami tessellati volatile oil, total flavones and total polysaccharides; Folium indocalami tessellati is wild indicalamus leaf, comprising in pubescence Indocalanmus tessellatus, Hunan Indocalanmus tessellatus, broadleaf indocalamus, Folium indocalami tessellati bamboo, Southern Mountain Indocalanmus tessellatus, Yiyang Indocalanmus tessellatus, square arteries and veins Indocalanmus tessellatus, Indocalanmus tessellatus and the west place in Hubei Indocalanmus tessellatus etc. any one arranged.
The used organic solvent of said extraction is any one or more than one combination in low polarity such as petroleum ether, ether, ethyl acetate or the medium polar solvent.
Said when utilizing Amberlyst process to prepare, the big pore resin can be any one types such as nonpolar, low pole and middle polarity,
Said macroporous resin model is any one among HP20, HPD100A, D101, D201, the AB-8 etc.
Said technology can be by following conditional operation: get Folium indocalami tessellati powder 2-5kg, add the water of 5-12 times of weight, soak 0-4h, steam distillation extracts 4-12h, volatile oil; Medicinal liquid is continued to employ after extracting volatile oil, and medicinal residues add in the 20-50% alcohol reflux of crude drug 6-12 times weight 2-3 time, at every turn 0.5-1.5h; Filter, merge extractive liquid, and volatile oil extract back medicinal liquid, concentrating under reduced pressure; Get extract, add the aqueous dispersion dissolving, making sample solution concentration in the crude drug amount is 0.4-1.0g/ml; Through macroporous adsorbent resin, absorption flow velocity 1-3BV/h, the resin column blade diameter length ratio is 1: 5-8; With pure water eluting 2-4BV, the polysaccharide elution flow rate is 3-5BV/h earlier, gets the Folium indocalami tessellati total polysaccharide extractive; Use 70% ethanol elution 3-6BV then, elution flow rate is 0.8-2.0BV/h, and 70% ethanol elution concentrates, and drying gets the Folium indocalami tessellati extractive of general flavone.
The implication of BV and BV/h is among the present invention: usually resin is loaded in the resin column of cylinder property, solution passes through continuously.The volume that loads resin in the resin column is called bed volume (BV), and the various inventories during work are unit with BV all.For example, solution is 2-4BV/h through the flow speed of resin, that is, per hour the volume through solution is the volumetrical 2-4 of resin bed times.
Method of quality control of the present invention can comprise following one or more content assaying methods:
1, volatile oil:
Volatile oil adopts direct weight method to calculate:
2, total flavones
It is an amount of that precision takes by weighing the Hesperidin reference substance, adds dissolve with methanol and process the solution that every 1ml contains Hesperidin 0.22mg.The accurate respectively Hesperidin reference substance solution 1,2,3,4 of drawing, 5ml in the 5ml measuring bottle, adds methanol constant volume, shakes up.The above-mentioned reference substance solution 0.5ml of accurate respectively absorption puts in the 25ml measuring bottle, accurately adds 10%AlCl3 solution 1.0ml, and the reuse distilled water is settled to scale; Shake up, room temperature is placed 15min, measures absorbance in the 310nm place; With Hesperidin concentration is abscissa, and absorbance is a vertical coordinate, curve plotting.
Precision takes by weighing each 3 parts in Folium indocalami tessellati flavone extract sample, and every part of 5mg adds dissolve with methanol and standardize solution in the 25ml volumetric flask, shakes up.The above-mentioned reference substance solution 0.5ml of accurate respectively absorption puts in the 25ml measuring bottle, accurately adds 10%AlCl3 solution 1.0ml, and the reuse distilled water is settled to scale, shakes up, and room temperature is placed 15min, measures absorbance in the 310nm place, calculates content.
3, total polysaccharides
Accurately take by weighing the glucose 20mg of 105 ℃ of dry constant weights, put in the 500ml volumetric flask, standardize solution shakes up (containing glucose 40mg/L).Draw glucose standard solution 0.4,0.6,0.8,1.0 respectively; 1.2,1.4,1.6,1.8mL; Be supplemented to 2.0mL with distilled water, add 5% phenol solution lmL, shake up, draw the 5m1 concentrated sulphuric acid and pour in the Boiling tube energetically; Static l0min shakes up, and room temperature held 20min measures absorbance in the 490hm place.(with the 2.0mL distilled water as blank).
Precision takes by weighing each 3 parts in Folium indocalami tessellati polyoses extract sample, every part of 5mg, and being dissolved in water also, standardize solution shakes up in the 25ml volumetric flask.Accurately get polysaccharide diluent 1.0mL to be measured, add phenol test solution 1.0mL, shake up, behind the placement 10min; Add the 5.0mL concentrated sulphuric acid fast, shake up, place 20min; Measure light absorption value in 490nm,, calculate polyoses content according to polysaccharide concentration in each liquid to be measured of regression equation calculation.
Beneficial effect of the present invention:
The present invention is the method for preparing of volatile oil, total flavones and total polysaccharides in a kind of while extraction separation Folium indocalami tessellati; Adopt this method can three effective constituents in the Folium indocalami tessellati be extracted simultaneously; Avoided the wasting of resources that single extraction brought effectively; Improve the resource utilization of Folium indocalami tessellati, reduced cost, and the big production of this method for preparing suitability for industrialized.
The specific embodiment
Below in conjunction with embodiment the present invention is further described, but embodiment does not have any restriction to the present invention.
Embodiment 1:
Get Folium indocalami tessellati powder 2kg, add 8 times of water gagings, soak 2h, steam distillation extracts 7h, gets volatile oil; Medicinal liquid is continued to employ after extracting volatile oil, and medicinal residues add in 9 times of amount meters of crude drug amount, 30% alcohol reflux 3 times, each 1.0h; Filter, behind the extracting solution decompression recycling ethanol, medicinal liquid after merging each extracting solution and extracting volatile oil, concentrating under reduced pressure; Get extract, add the aqueous dispersion dissolving, making sample solution concentration in the crude drug amount is 0.7g/ml, through the AB-8 macroporous resin; Absorption flow velocity 2BV/h, the resin column blade diameter length ratio is 1: 6, using water elution 3BV, elution flow rate earlier is 3BV/h; Eluent concentrates, ethanol precipitation, and drying gets the Folium indocalami tessellati total polysaccharide extractive; Use 70% ethanol elution 3BV then, elution flow rate is 1.5BV/h, and this eluent concentrates, and drying gets the Folium indocalami tessellati extractive of general flavone.
Embodiment 2:
Get Folium indocalami tessellati powder 5kg, add 5 times of water gagings, soak 4h, steam distillation extracts 12h, gets volatile oil; Medicinal liquid is continued to employ after extracting volatile oil, and medicinal residues add in 12 times of amount meters of crude drug amount, 40% alcohol reflux 3 times, each 1.5h; Filter, behind the extracting solution decompression recycling ethanol, medicinal liquid after merging each extracting solution and extracting volatile oil, concentrating under reduced pressure; Get extract, add the aqueous dispersion dissolving, making sample solution concentration in the crude drug amount is 1.0g/ml, through the HP-20 macroporous resin; Absorption flow velocity 3BV/h, the resin column blade diameter length ratio is 1: 8, using water elution 4BV, elution flow rate earlier is 4BV/h; Eluent concentrates, ethanol precipitation, and drying gets the Folium indocalami tessellati total polysaccharide extractive; Use 70% ethanol elution 4BV then, elution flow rate is 2BV/h, and this eluent concentrates, and drying gets the Folium indocalami tessellati extractive of general flavone.
Embodiment 3:
Get Folium indocalami tessellati powder 2kg, add 12 times of water gagings, soak 0h, steam distillation extracts 4h, gets volatile oil; Medicinal liquid is continued to employ after extracting volatile oil, and medicinal residues add in 6 times of amount meters of crude drug amount, 40% alcohol reflux 3 times, each 1.0h; Filter, behind the extracting solution decompression recycling ethanol, medicinal liquid after merging each extracting solution and extracting volatile oil, concentrating under reduced pressure; Get extract, add the aqueous dispersion dissolving, making sample solution concentration in the crude drug amount is 0.8g/ml, through the D-101 macroporous resin; Absorption flow velocity 2BV/h, the resin column blade diameter length ratio is 1: 7, using water elution 2BV, elution flow rate earlier is 2BV/h; Eluent concentrates, ethanol precipitation, and drying gets the Folium indocalami tessellati total polysaccharide extractive; Use 70% ethanol elution 3BV then, elution flow rate is 1BV/h, and this eluent concentrates, and drying gets the Folium indocalami tessellati extractive of general flavone.
Embodiment 4:
Get Folium indocalami tessellati powder 3kg, add 5 times of water gagings, soak 3h, steam distillation extracts 6h, gets volatile oil; Medicinal liquid is continued to employ after extracting volatile oil, and medicinal residues add in 8 times of amount meters of crude drug amount, 40% alcohol reflux 3 times, each 1.5h; Filter, behind the extracting solution decompression recycling ethanol, medicinal liquid after merging each extracting solution and extracting volatile oil, concentrating under reduced pressure; Get extract, add the aqueous dispersion dissolving, making sample solution concentration in the crude drug amount is 1.6g/ml, through the HPD-100A macroporous resin; Absorption flow velocity 3BV/h, the resin column blade diameter length ratio is 1: 8, using water elution 3BV, elution flow rate earlier is 2BV/h; Eluent concentrates, ethanol precipitation, and drying gets the Folium indocalami tessellati total polysaccharide extractive; Use 90% ethanol elution 4BV then, elution flow rate is 2BV/h, and this eluent concentrates, and drying gets the Folium indocalami tessellati extractive of general flavone.
Embodiment 5:
Get Folium indocalami tessellati powder 2kg, add 4 times of water gagings, soak 2h, steam distillation extracts 6h, gets volatile oil; Medicinal liquid is continued to employ after extracting volatile oil, and medicinal residues add in 7 times of amount meters of crude drug amount, 50% alcohol reflux 3 times, each 1.0h; Filter, behind the extracting solution decompression recycling ethanol, medicinal liquid after merging each extracting solution and extracting volatile oil, concentrating under reduced pressure; Get extract, add the aqueous dispersion dissolving, making sample solution concentration in the crude drug amount is 0.8g/ml, through the D-201 macroporous resin; Absorption flow velocity 2BV/h, the resin column blade diameter length ratio is 1: 6, using water elution 3BV, elution flow rate earlier is 2BV/h; Eluent concentrates, ethanol precipitation, and drying gets the Folium indocalami tessellati total polysaccharide extractive; Use 80% ethanol elution 3BV then, elution flow rate is 1BV/h, and this eluent concentrates, and drying gets the Folium indocalami tessellati extractive of general flavone.
It is following that above embodiment utilizes above-mentioned quality determining method to record volatile oil, total flavones and total polysaccharides content:
Obviously, those skilled in the art can carry out various changes and modification to the present invention and not break away from the spirit and scope of the present invention.If of the present invention these are revised and modification belongs to the scope of basic design of the present invention or equivalent technologies, then the present invention also should comprise these changes and modification.
If the content of not making detailed description is arranged, then belong to this area professional and technical personnel's technique known in this description, repeat no more here.
Claims (6)
1. method for preparing Folium indocalami tessellati volatile oil, total flavones and total polysaccharides simultaneously; It is characterized in that technology carries out according to the following steps: get the water that the Folium indocalami tessellati powder adds 5-12 times of weight; Soak 0-4h, steam distillation extracts 2-12h, obtains Folium indocalami tessellati volatile oil with organic solvent extracting; Medicinal liquid is continued to employ after extracting volatile oil, and medicinal residues add in the 20-50% alcohol reflux of 6-12 times of weight of crude drug amount 2-3 time, each 0.5-1.5h, filtration; Medicinal liquid after merging each extracting solution and extracting volatile oil, concentrating under reduced pressure gets extract, adds the aqueous dispersion dissolving; Making sample solution concentration in the crude drug amount is 0.4-1.0g/ml, through macroporous resin, and absorption flow velocity 1-3BV/h, the resin column blade diameter length ratio is 1: 5-8; Earlier use water elution 2-4BV, the eluent ethanol precipitation, drying gets the Folium indocalami tessellati total polysaccharide extractive; Use 40-90% ethanol elution 3-6BV then, elution flow rate is 0.8-2BV/h, and this eluent concentrates, and drying gets the Folium indocalami tessellati extractive of general flavone.
2. the method for preparing Folium indocalami tessellati volatile oil, total flavones and total polysaccharides simultaneously as claimed in claim 1; It is characterized in that: said raw material Folium indocalami tessellati is wild indicalamus leaf, includes in pubescence Indocalanmus tessellatus, Hunan Indocalanmus tessellatus, broadleaf indocalamus, Folium indocalami tessellati bamboo, Southern Mountain Indocalanmus tessellatus, Yiyang Indocalanmus tessellatus, square arteries and veins Indocalanmus tessellatus, Indocalanmus tessellatus and the west place in Hubei Indocalanmus tessellatus any one.
3. the method for preparing Folium indocalami tessellati volatile oil, total flavones and total polysaccharides simultaneously as claimed in claim 1 is characterized in that: the organic solvent of said extraction usefulness is any one or more than one combination in low polarity of petroleum ether, ether, ethyl acetate or the medium polar solvent.
4. the method for preparing Folium indocalami tessellati volatile oil, total flavones and total polysaccharides simultaneously as claimed in claim 1 is characterized in that: described macroporous resin be nonpolar, low pole and middle polarity any one.
5. like claim 1 or the 4 described methods that prepare Folium indocalami tessellati volatile oil, total flavones and total polysaccharides simultaneously, it is characterized in that: the model of said macroporous resin is any one among HP20, HPD100A, D101, D201, the AB-8.
6. the method for preparing Folium indocalami tessellati volatile oil, total flavones and total polysaccharides simultaneously as claimed in claim 1; It is characterized in that: said technology is by following conditional operation: get Folium indocalami tessellati powder 2-5kg, add the water of 5-12 times of weight, soak 0-4h; Steam distillation extracts 4-12h, gets volatile oil; Medicinal liquid is continued to employ after extracting volatile oil, and medicinal residues add in the 20-50% alcohol reflux of crude drug 6-12 times weight 2-3 time, at every turn 0.5-1.5h; Filter, merge extractive liquid, and volatile oil extract back medicinal liquid, concentrating under reduced pressure; Get extract, add the aqueous dispersion dissolving, making sample solution concentration in the crude drug amount is 0.4-1.0g/ml; Through macroporous adsorbent resin, absorption flow velocity 1-3BV/h, the resin column blade diameter length ratio is 1: 5-8; With pure water eluting 2-4BV, the polysaccharide elution flow rate is 3-5BV/h earlier, gets the Folium indocalami tessellati total polysaccharide extractive; Use 70% ethanol elution 3-6BV then, elution flow rate is 0.8-2.0BV/h, and 70% ethanol elution concentrates, and drying gets the Folium indocalami tessellati extractive of general flavone.
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| CN103074159A (en) * | 2013-01-25 | 2013-05-01 | 安徽中烟工业有限责任公司 | Preparation method of indocalamus leaf volatile oil and application of volatile oil in cigarette |
| CN103451022A (en) * | 2013-09-02 | 2013-12-18 | 南昌大学 | Method for integrally extracting volatile oil, polysaccharide and flavone from elsholtzia haichowensis sun |
| CN103585187A (en) * | 2013-10-31 | 2014-02-19 | 济南星懿医药技术有限公司 | Preparation method of Theloschestes flavicans extract |
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