CN103417588A - Preparation method of effective part of Hippophae rhamnoides - Google Patents
Preparation method of effective part of Hippophae rhamnoides Download PDFInfo
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Abstract
The invention relates to a preparation method of the effective part of Hippophae rhamnoides. The method includes: crushing and screening aired Hippophae fruits or post-pressing Hippophae fruit residue, heating ethanol for reflux extraction, collecting extract, performing reduced-pressure recovery on the ethanol, condensing, enriching the condensate with macroporous resin, and vacuum-drying to obtain the total effective part of Hippophae rhamnoides. Hippophae rhamnoides contains 75-85% of the total effective part. The total effective part contains 35-50% of triterpene and 32-45% of total phenols. The results of in-vitro anti-oxidization and anti-bacteria experiments and bioactivity experiments show that the effective part of Hippophae rhamnoides is high in capacity of clearing free radicals in 2, 2-azino-bis(3-ethyl- benzothiazole-6-sulfonate) diammonium salt, high in inhibition on Staphylococcus aureus, and high in oxidation resistance and gram-positive bacterium inhibition. The product obtained by the preparation method is applicable to health foods, drugs, cosmetics or solid drink materials having the functions of protecting liver, lowering blood lipid, age defying, protecting gastric mucosa, antisepsis and anti-inflammation.
Description
Technical field
The present invention relates to a kind of preparation method of central asian sea buckthorn effective site.
Background technology
Fructus Hippophae is the huge industrial crops of a kind of potentiality to be exploited, has very superior ecological benefits and social benefit.Not only there is the Ecology Action of checking winds and fixing drifting sand and conserving water and soil, and be rich in the bioactive ingredients such as multivitamin, flavone, organic acid, terpenoid, sterol, carotenoid, unsaturated fatty acid because of it, there is fine exploitation at cosmetics, health food and field of medicaments and be worth.There is long Fructus Hippophae medicinal history in China, in eightth century of Christian era Tibetan medicine's books " month king a medicine examine ", just the drug effect of Fructus Hippophae has been done to detailed record, is the medical record of relevant Fructus Hippophae the earliest in the world.All use the diseases such as single Fructus Hippophae or compound treatment bronchitis, stomachache, dyspepsia, traumatic injury, amenorrhea in China dimension doctor, Tibetan medicine and Mongolian medicine's traditional medicine, good effect, cheap.Within 1977, Ministry of Public Health is formally listed Fructus Hippophae in " Chinese pharmacopoeia.
Central asian sea buckthorn (Hippophae rhamnoides L.subsp.Turkestanica) machaka or dungarunga, 6 meters of Gao Keda are rare to 15 meters, twig is close by the silvery white scale, gives birth to the branch scale more than 1 year and comes off, and epidermis is white in color, light, the breakaway of old branch bark part; Sting more and shorter, branch sometimes; Internode is slightly long; Bud is little.Single leaf alternate, linear, long 15-45 millimeter, wide 2-4 millimeter, top obtuse or subcircular, the base portion wedge shape, the two sides silvery white, close by scale (green above rare), without the rust scale; Petiole is short, is about 1 millimeter.Fruit oblong or obovate be to subcircular, long 5-7 (9) millimeter, and diameter 3-4 millimeter (length of cultivation can reach the 6-9 millimeter, diameter 6-8 millimeter), when dry, sarcocarp is more crisp; The long 3-4 millimeter of carpopodium; Shape of the seed differs, often slightly flat, long 2.8-4.2 millimeter.May at florescence, the fruit phase 8-9 month.Originate in Xinjiang of China.Be born in height above sea level 800-3000 rice step ground, river valley, open spacious hillside, be common in alluvial flat.What have makes hedgerow.Soviet Union Tadzhikistan, Kirghiz Republic, Uzbekistan, Kazak and Afghanistan are western, west Mongolia has distribution.Central asian sea buckthorn has a wide range of applications in Uygur nationality's traditional medicine, and it is by name that it ties up medicine: " Ji Han ", have and give birth to dry living trembling with fear, clearing and antitussive, clearing stomach increases food, sending down the abnormal ascending QI emesis removing dampness and eliminating phlegm, diuresis eliminating dampness by diuresis, soft liver detumescent, removing heat from blood blood pressure lowering, the effect of the centering of relievining asthma.
Total phenols and total triterpene are two active components main in the central asian sea buckthorn fruit.Total phenols in the central asian sea buckthorn fruit be take flavone, catechuic acid, tocopherol, anthocyanidin, coumarin and a small amount of tannin composition as main.Clinical research show Fructus Hippophae flavone have antiinflammatory, antibacterial, protect the liver, the effect such as relieving cough and asthma, treatment cardiovascular and cerebrovascular disease; Catechuic acid all has bacteriostasis in various degree to bacillus pyocyaneus, escherichia coli, Bacillus typhi, dysentery bacterium, Bacillus alcaligenes and bacillus subtilis and staphylococcus aureus, also eliminate the phlegm, antiasthmatic effect, the clinical chronic tracheitis that is used for the treatment of, and there is the effect that suppresses dental caries; Tocopherol has another name called vitamin E gastric ulcer is had to certain therapeutical effect; on the one hand by the effect of regulating fat oxidation, removing oxyradical; the infringement that the protection gastric mucosa is not oxidated dose; simultaneously; a large amount of vitamin Es can improve again the peripheral blood circulation; increase the supply of tissue oxygen, thereby good nutritional condition is created in healing to ulcer surface, tocopherol also has the effect that promotes sex hormones secretion in addition.In addition also contain other phenols components such as a certain amount of anthocyanidin, coumarin and tannin constituents in Fructus Hippophae, there is equally the effects such as antioxidation, antibacterial and antiinflammatory.
Triterpenes composition in the central asian sea buckthorn fruit exists and mainly take oleanolic acid and ursolic acid as main mainly with the form of triterpenic acid.Oleanolic acid is the hepatopathy adjuvant, and the clinical infectiousness acute icterohepatitis that is used for the treatment of, also can be used for psoriasis, rheumatic arthritis, oedema due to nephritis, cirrhotic ascites, acute, chronic hepatitis, stomachache stranguria with turbid discharge, metrorrhagia, traumatic injury, carbuncle, soreness of the waist and knees, the diseases such as frequent fetal movement; Ursolic acid is that the isomers of oleanolic acid has very strong hepatoprotective effect equally, there is the various biological effects such as calmness, antiinflammatory, antibiotic, antiulcer, reduction blood glucose simultaneously, ursolic acid also has obvious anti-oxidation function, is widely used as medicine and cosmetic material.
China is sea buckthorn resources maximum country that distributes in the world, and 95% Fructus Hippophae all is distributed in China.Fructus Hippophae product on market mainly be take Oleum Hippophae and Fructus Hippophae flavone as main, and in the Fructus Hippophae total phenols except flavones ingredient, other phenols component rich contents such as catechuic acid, tocopherol, anthocyanidin, coumarin and have good biological activity, therefore be optimized and have certain exploitation and be worth the process of enriching of total phenols in Fructus Hippophae.And, the triterpenes components content in sea buckthorn fruit more (2%-3%), and have with total phenols similarly protect the liver, antiinflammatory, antioxidation, antibiotic, treatment ulcer isoreactivity, the rare research of preparation specific examples of such components from Fructus Hippophae both at home and abroad.Therefore synchronously total triterpene and total phenols two constituents are carried out to enrichment, be conducive to make different active components to act on a plurality of target spots, by synergism better bring into play the Fructus Hippophae antiinflammatory, protect the liver, the pharmacological action such as antioxidation, antibiotic, antiulcer, for the further exploitation of Related product provides material base.The present invention is extracted total triterpene and total phenols by the method for solvent refluxing, by macroporous resin, it is carried out to purification, and utilization rate of raw materials is high, and method is simple, is convenient to industry and amplifies.
Summary of the invention
The object of the invention is, a kind of preparation method and purposes of central asian sea buckthorn effective site is provided, and the method is that the marc after central asian sea buckthorn fruit or oil expression is dried in the shade, pulverize, sieve, the water-ethanol system is extracted, and filters, concentrated filtrate decompression recycling ethanol, again concentrated solution is carried out to purification with macroporous resin, vacuum drying, can obtain central asian sea buckthorn total effective parts content 75-85%, wherein in effective site, contain total triterpene contents 35-50%, total phenol content 32-45%.This effective site have protect the liver, health food, medicine, cosmetics or the solid beverage raw material of the function such as blood fat reducing, defying age, protection gastric mucosa, anti-inflammation.
The preparation method of a kind of central asian sea buckthorn effective site of the present invention, the method central asian sea buckthorn raw material is the marc after sea buckthorn fruit or oil expression, concrete operations follow these steps to carry out:
A. the marc after central asian sea buckthorn fruit or oil expression is dried in the shade, pulverize, cross the 40-50 mesh sieve, get the fruit powder of pulverizing, the concentration of doubly measuring with mass volume ratio 5-15 is that 30-90% ethanol heating in water bath refluxes, and bath temperature is 60-95 ℃, extract 1-4 time, time 1-3h, collect extracting solution, decompression recycling ethanol;
B. step a extracting solution is concentrated into to mass concentration 0.067g crude drug/mL, uses saturated NaHCO
3Or Na
2CO
3Solution is regulated pH to 3-7, again concentrated solution is carried out to purification with macroporous resin, then the ethanol that water and volumetric concentration are 30%-80% carries out eluting successively, collect ethanol elution, wherein the water elution volume is 1-3BV, the washing flow velocity is 1-4BV/h, and the ethanol elution volume is 1-4BV, and ethanol elution speed is 1-4BV/h;
C. by the ethanol elution of step b, vacuum drying, can obtain central asian sea buckthorn total effective parts content 75-85%, total triterpene contents 35-50% in total effective parts wherein, total phenol content 32-45%.
Step b is concentrated into mass concentration 0.067g crude drug/mL at temperature 45 C by step a extracting solution with vacuum rotary evaporator.
Macroporous resin in step b is HPD-100, HPD-300, HPD-450, HPD-600, HPD-700, AB-8 or NKA-9 type.
The preparation method of a kind of central asian sea buckthorn effective site of the present invention and purposes, through the impact on purified total phenols and total triterpene contents on the different model macroporous resin; The impact of the different loading concentration of macroporous resin on total phenols and total triterpene adsorption rate; The impact of the different loading pH of macroporous resin on total phenols and total triterpene adsorption rate; The impact of the different adsorption rate of macroporous resin on purified total phenols and total triterpene contents; The impact of macroporous resin strippant on purified total phenols and total triterpene contents; The dynamic desorption of 70% ethanol; Macroporous resin desorbing test is as follows:
Nine kinds of macroporous resins static adsorption and desorption experiment to Fructus Hippophae total phenols and total triterpene:
Get the macroporous resin that is equivalent to 1g dried resin weight of different model, concentration is that 95% soak with ethanol is spent the night, and pure water is cleaned, and is respectively charged in the extracting solution of 50mL certain mass concentration, room temperature concussion (250r/min) 12h, the balance total phenols of survey supernatant and total triterpene mass concentration ρ
e(mg/mL), after the elimination extracting solution, resin cleans through the 50mL pure water, then to put into 50mL concentration be 60% ethanol, desorbing under the same terms, filter, then be that 95% ethanol carries out desorbing by 50mL concentration, merge filtrate twice, measure the total triterpene of stripping liquid and total phenols mass concentration ρ
d(mg/mL), be calculated as follows respectively adsorbance, desorption quantity, desorption efficiency, therefrom filter out the best resin of performance and carry out subsequent experimental, the results are shown in Figure 1;
Adsorbance (mg/g dried resin)=(ρ
0-ρ
e) * V
0/ m
Desorption quantity (mg/g dried resin)=ρ
d* V
d/ m
Desorption efficiency=desorption quantity * 100/ adsorbance
Wherein: ρ
0Total triterpene and total phenols mass concentration (mg/mL) in-extracting solution, V
0-extracting liquid volume (mL), V
d-stripping liquid volume (mL), m-resin quality (g);
Result shows (Fig. 1), in 8 kinds of macroporous resins, all higher to Fructus Hippophae total phenols and total triterpene adsorbance and desorption quantity is AB-8, HPD-100 and HPD-300, AB-8 resin best results wherein, consider that the AB-8 macroporous resin has better mechanical strength and reasonable prices, so finally select the AB-8 macroporous resin.
The concentration screening test of loading solution:
Get 8.5g (being equivalent to the 3g dried resin) AB-8 macroporous resin, wet method dress post, the extract solution 100mL that is 0.1g crude drug/mL by mass concentration, thin up is to 100mL, 150mL respectively, 200mL, 300mL, 500mL cross respectively post with the flow velocity of 2BV/h, wash resin with pure water colourless to effluent, collect eluent, measure respectively total phenols and total triterpene contents in eluent, calculate the adsorbance to two constituents of AB-8 resin under different loading concentration;
As result shows (Fig. 2), variable concentrations, in the identical situation of applied sample amount, sample solution is diluted to 150mL(0.067) concentration continues to reduce its adsorbance and substantially no longer raises after g crude drug/mL, so selection concentration 0.067g crude drug/mL is best loading concentration.
The screening of the rate of adsorption:
Get 8.5g (being equivalent to the 3g dried resin) AB-8 macroporous resin, wet method dress post, get the extracting solution of 100mL0.1g crude drug/mL, flow velocity upper prop with 1.0BV/h, 2.0BV/h, 3.0BV/h and 4BV/h, wash resin with pure water colourless to effluent, collect eluent, measure respectively total phenols and total triterpene contents in eluent, calculate the adsorbance to two constituents of AB-8 resin under different loading concentration;
Result shows (Fig. 3), when the rate of adsorption is 1BV/h, and triterpene and total phenols adsorbance maximum, the total triterpene of 1BV/h and 2BV/h and total phenols adsorbance difference are less, but after 2BV/h, total triterpene and total phenols adsorbance obviously descend, and consider work efficiency, therefore, selecting the absorption flow velocity is 2BV/h.
The screening of sample solution pH:
Get 8.5g (being equivalent to the 3g dried resin) AB-8 macroporous resin, wet method fills post, gets the extracting solution of 100mL0.1g crude drug/mL, and stock solution pH is 3.1, uses respectively saturated Na
2CO
3Solution is regulated pH to 4,5,6,7, sample liquid after stock solution and adjusting pH, respectively with the 2BV/h upper prop, is washed to resin with pure water colourless to effluent, collect eluent, measure respectively total phenols and total triterpene contents in eluent, calculate the adsorbance to two constituents of AB-8 resin under different loading pH;
Result shows (Fig. 4), and sample solution pH is 6 o'clock, and it is maximum that triterpene and total phenols adsorbance all reach, so select sample solution pH, is 6.
The extracting solution applied sample amount is investigated test:
Get 8.5g (being equivalent to the 3g dried resin) AB-8 macroporous resin, wet method dress post, get Fructus Hippophae extracting solution (0.067g crude drug/mL), regulate pH to 6, upper AB-8 macroporous resin column, after being adsorbed with the 2BV/h flow velocity, collect eluent, in mensuration, total triterpene and total phenol content, the results are shown in Figure 5;
Reveal curve from Fig. 5, applied sample amount is from 10BV, and total triterpene amount of leakage increases severely, and the total phenols leakage rate is fast rising also, determines when applied sample amount is 9-10BV, and it is saturated that resin column reaches absorption.
The screening test of strippant:
Get 8.5g (being equivalent to the 3g dried resin) AB-8 macroporous resin, wet method dress post, get Fructus Hippophae extracting solution (0.067g crude drug/mL), regulate pH to 6, upper AB-8 macroporous resin column, with the 2BV/h flow velocity, adsorbed, wash resin with pure water colourless to eluent liquid, then wash post with the alcoholic solution of volume fraction 10%, 30%, 50%, 70% and 90% with 2BV/h successively, collect stripping liquid, measure respectively its total phenols and total triterpene contents, result is as Fig. 6;
From Fig. 6 result, can find out, when concentration is 70% ethanol elution, the total triterpene contents desorption efficiency is up to 98.7%, when concentration is 50% ethanol elution, total phenol content is up to 90.9%, but when concentration is 70% ethanol elution, the total phenols desorption efficiency is also up to 88%, consider, when concentration is 70% ethanol elution, total phenols and total triterpene have good desorption efficiency, so select concentration, are that 70% ethanol is strippant.
The screening test of strippant consumption volume:
Get 8.5g (being equivalent to the 3g dried resin) AB-8 macroporous resin, wet method dress post, get Fructus Hippophae extracting solution (0.066g crude drug/mL), regulate pH to 6, upper AB-8 macroporous resin column, with the 2BV/h flow velocity, adsorbed, wash resin with pure water colourless to eluent liquid, with the alcoholic solution eluting of volume fraction 70%, every 0.5BV stripping liquid is collected once, 2.5 doubly after volume, every 1BV collects once, its dynamic desorption curve is shown in Fig. 7;
The result demonstration, the total phenols be desorbed and total triterpene mainly concentrate in 1.5BV, when the strippant consumption is 3.5BV, substantially without triterpene and phenols component, flow out, so, the strippant of selection 3.5BV.
The preparation method of a kind of central asian sea buckthorn effective site of the present invention has the following advantages:
Edible ethanol take in described method as solvent and eluant, inexpensive, nontoxic; The macroporous resin price adopted is lower, and safety is higher, can reuse, and is current domestic medicine trade macroporous resin commonly used.The vanillin for Fructus Hippophae effective site obtained by the method for the invention-perchloric acid colorimetric method for determining total triterpene contents is 35-50%, with Folin-Ciocalteu colorimetric method for determining total phenol content 32-45%, the total effective parts mass content can reach the 75-85%(total triterpene contents and total phenol content can't reach the highest or minimum simultaneously, so the highest and minimum content of total effective parts, be not the highest and minimum content of two kinds of compositions add and).There is after tested good antioxidation and antibacterial activity, not the adding preservative agent long preservation.
The central asian sea buckthorn effective site obtained by the method for the invention can be used for preparation have protect the liver, health food, medicine, cosmetics or the solid beverage raw material of the functions such as blood fat reducing, defying age, protection gastric mucosa, anti-inflammation.
The accompanying drawing explanation
Fig. 1 be different model macroporous resin of the present invention to the total triterpene of Fructus Hippophae and total phenols adsorbance and desorption quantity, wherein 1 is total triterpene adsorbance, 2 is total triterpene desorption quantity, 3 is the total phenols adsorbance, 4 is the total phenols desorption quantity;
Fig. 2 is that the different loading concentration of the present invention affects figure to the total triterpene of AB-8 macroporous resin adsorption Fructus Hippophae and total phenols amount, wherein
For total triterpene,
For total phenols;
Fig. 3 is that the different loading flow velocitys of the present invention affect figure to the total triterpene of AB-8 macroporous resin adsorption Fructus Hippophae and total phenols amount, wherein
For total triterpene,
For total phenols;
Fig. 4 is that the different loading pH of the present invention affect figure to the total triterpene of AB-8 macroporous resin adsorption Fructus Hippophae and total phenols amount, wherein
For total triterpene,
For total phenols;
Fig. 5 is that the leakage curve chart is adsorbed in the present invention, wherein
For total triterpene,
For total phenols;
Fig. 6 be different concentration ethanol of the present invention on the total triterpene of Fructus Hippophae and total phenols on the AB-8 macroporous resin desorption efficiency affect figure, wherein 1 is total triterpene, 2 is total phenols;
The dynamic desorption curve chart that Fig. 7 is the present invention's 70% ethanol, wherein
For total triterpene,
For total phenols.
The specific embodiment:
The present invention is described further in connection with specific embodiment, but is not limited to the present embodiment scope;
A. sea buckthorn fruit being dried in the shade, pulverize, cross 40 mesh sieves, get the fruit powder 100g of pulverizing, is that 50% ethanol adopts heating in water bath to reflux by the concentration of 5 times of amounts of mass volume ratio, and bath temperature is 95 ℃, extracts 3 times, and time 3h, collect extracting solution, decompression recycling ethanol;
B. step a extracting solution is concentrated into to mass concentration 0.067g crude drug/mL with vacuum rotary evaporator when the temperature 45 C, uses saturated NaHCO
3Solution is regulated pH to 6, again concentrated solution is carried out to purification with macroporous resin AB-8, then the ethanol that water and volumetric concentration are 70% carries out eluting successively, collect ethanol elution, wherein the water elution volume is 3BV, the washing flow velocity is 1.5BV/h, and the ethanol elution volume is 3BV, and ethanol elution speed is 2BV/h;
C. by the ethanol elution of step b, vacuum drying, can obtain Fructus Hippophae effective site 5.1g, and wherein total triterpene contents 49%, total phenol content 36%, total effective parts content 85%.
A. sea buckthorn fruit being dried in the shade, pulverize, cross 50 mesh sieves, get the fruit powder 100g of pulverizing, is that 50% ethanol adopts heating in water bath to reflux by the concentration of 10 times of amounts of mass volume ratio, and bath temperature is 80 ℃, extracts 2 times, and time 2h, collect extracting solution, decompression recycling ethanol;
B. at temperature 45 C, step a extracting solution is concentrated into to mass concentration 0.067g crude drug/mL with vacuum rotary evaporator, keep stock solution pH3.1, again concentrated solution is carried out to purification with macroporous resin HPD-300, then the ethanol that water and volumetric concentration are 50% carries out eluting successively, collect ethanol elution, wherein the water elution volume is 3BV, and the washing flow velocity is 2BV/h, the ethanol elution volume is 2.5BV, and ethanol elution speed is 1BV/h;
C. by the ethanol elution of step b, vacuum drying, can obtain Fructus Hippophae effective site 4.5g, and wherein total triterpene contents 45%, total phenol content 39%, total effective parts content 84%.
A. sea buckthorn fruit being dried in the shade, pulverize, cross 40 mesh sieves, get the fruit powder 100g of pulverizing, is that 30% ethanol adopts heating in water bath to reflux by the concentration of 15 times of amounts of mass volume ratio, and bath temperature is 70 ℃, extracts 3 times, and time 1h, collect extracting solution, decompression recycling ethanol;
B. at temperature 45 C, step a extracting solution is concentrated into to mass concentration 0.067g crude drug/mL with vacuum rotary evaporator, uses Na
2CO
3Solution is regulated pH to 5, again concentrated solution is carried out to purification with macroporous resin HPD-450, then the ethanol that water and volumetric concentration are 30% carries out eluting successively, collect ethanol elution, wherein the water elution volume is 3BV, the washing flow velocity is 3BV/h, and the ethanol elution volume is 4BV, and ethanol elution speed is 4BV/h;
C. by the ethanol elution of step b, vacuum drying, can obtain Fructus Hippophae effective site 3.6g, and wherein total triterpene contents 35%, total phenol content 45%, total effective parts content 80%.
A. the sea-buckthorn pomace after oil expression is dried in the shade, pulverize, cross 50 mesh sieves, get the marc powder 100g of pulverizing, by the concentration of 10 times of amounts of mass volume ratio, be that 70% ethanol adopts heating in water bath to reflux, bath temperature is 60 ℃, extracts 3 times, time 3h, collect extracting solution, decompression recycling ethanol;
B. at temperature 45 C, step a extracting solution is concentrated into to mass concentration 0.067g crude drug/mL with vacuum rotary evaporator, uses saturated NaHCO
3Solution is regulated pH to 4, again concentrated solution is carried out to purification with macroporous resin HPD-600, then the ethanol that water and volumetric concentration are 70% carries out eluting successively, collect ethanol elution, wherein the water elution volume is 4BV, the washing flow velocity is 1BV/h, and the ethanol elution volume is 2BV, and ethanol elution speed is 1BV/h;
C. by the ethanol elution of step b, vacuum drying, can obtain Fructus Hippophae effective site 3.8g, and wherein total triterpene contents 47%, total phenol content 35%, total effective parts content 82%.
A. sea buckthorn fruit being dried in the shade, pulverize, cross 50 mesh sieves, get the fruit powder 100g of pulverizing, is that 50% ethanol adopts heating in water bath to reflux by the concentration of 10 times of amounts of mass volume ratio, and bath temperature is 85 ℃, extracts 3 times, and time 2h, collect extracting solution, decompression recycling ethanol;
B. at temperature 45 C, step a extracting solution is concentrated into to mass concentration 0.067g crude drug/mL with vacuum rotary evaporator, uses Na
2CO
3Solution is regulated pH to 6, again concentrated solution is carried out to purification with macroporous resin HPD-100, then the ethanol that water and volumetric concentration are 80% carries out eluting successively, collect ethanol elution, wherein the water elution volume is 3BV, the washing flow velocity is 1.5BV/h, and the ethanol elution volume is 3BV, and ethanol elution speed is 2BV/h;
C. by the ethanol elution of step b, vacuum drying, can obtain Fructus Hippophae effective site 5.5g, and wherein total triterpene contents 46%, total phenol content 32%, total effective parts content 78%.
A. the sea-buckthorn pomace after extracting oil, pulverize, and crosses 50 mesh sieves, gets the fruit powder 100g of pulverizing, by the concentration of 8 times of amounts of mass volume ratio, is that 60% ethanol adopts heating in water bath to reflux, and bath temperature is 65 ℃, extracts 4 times, and time 2h, collect extracting solution, decompression recycling ethanol;
B. at temperature 45 C, step a extracting solution is concentrated into to mass concentration 0.067g crude drug/mL with vacuum rotary evaporator, uses saturated NaHCO
3Solution is regulated pH to 5, again concentrated solution is carried out to purification with macroporous resin HPD-700, then the ethanol that water and volumetric concentration are 30% carries out eluting successively, collect ethanol elution, wherein the water elution volume is 1BV, the washing flow velocity is 2BV/h, and the ethanol elution volume is 2BV, and ethanol elution speed is 1BV/h;
C. by the ethanol elution of step b, vacuum drying, can obtain Fructus Hippophae effective site 3.5g, and wherein total triterpene contents 44%, total phenol content 35%, total effective parts content 79%.
Embodiment 7
A. the central asian sea buckthorn fruit being dried in the shade, pulverize, cross 50 mesh sieves, get the fruit powder 100g of pulverizing, is that 80% ethanol adopts heating in water bath to reflux by the concentration of 15 times of amounts of mass volume ratio, and bath temperature is 95 ℃, extracts 3 times, and time 1h, collect extracting solution, decompression recycling ethanol;
B. at temperature 45 C, step a extracting solution is concentrated into to mass concentration 0.067g crude drug/mL with vacuum rotary evaporator, uses Na
2CO
3Solution is regulated pH to 7, then concentrated solution is carried out to purification by macroporous resin NKA-9 type, and the ethanol that then water and concentration are 80% carries out eluting successively, collect ethanol elution, wherein the water elution volume is 3BV, and the washing flow velocity is 4BV/h, the ethanol elution volume is 4BV, and ethanol elution speed is 4BV/h;
C. by the ethanol elution of step b, vacuum drying, can obtain Fructus Hippophae effective site 4.5g, and wherein total triterpene contents 40%, total phenol content 35%, total effective parts content 75% product.
Embodiment 8:2,2-azino-bis-(3-ethyl-benzothiazole-6-sulfonic acid) di-ammonium salts (ABTS) method is measured the experiment of central asian sea buckthorn effective site antioxidant activity:
The central asian sea buckthorn effective site that embodiment 1-7 is obtained, become 1mg/mL, 0.8mg/mL, 0.5mg/mL, 0.25mg/mL, 0.15mg/mL with 50% dissolve with ethanol solution, 0.1mg/mL solution, respectively get 16 μ L sample liquid in 96 orifice plates, and adding 184 μ L2,2-azino-bis-(3-ethyl-benzothiazole-6-sulfonic acid) di-ammonium salts (ABTS) free-atom aqueous solution is sample sets (A
t), and establish 3 groups parallel; Concentration is that 50% ethanol 16 μ L add 184 μ L2, and 2-azino-bis-(3-ethyl-benzothiazole-6-sulfonic acid) di-ammonium salts (ABTS) free-atom aqueous solution is blank group (A
0); 16 μ L sample liquid add 184 μ L, and concentration is that 50% alcoholic solution is background matched group (B), with vitamin C, does positive control, after lucifuge reaction 5min, in 734nm, measure absorbance, according to following formula, calculate clearance rate, use IC
50Software for calculation draws sample and positive control antioxidation IC
50Value, in Table 1:
Clearance rate (%)=[1-(A
t-B
t)/(A
0-B
0)] * 100%;
Table 1 central asian sea buckthorn effective site is removed the IC of 2,2-azino-bis-(3-ethyl-benzothiazole-6-sulfonic acid) di-ammonium salts (ABTS) free radical
50Table
Result shows: central asian sea buckthorn effective site has stronger oxidation resistance.
The central asian sea buckthorn effective site that embodiment 1-7 is obtained, with dmso solution to 100mg/mL, get LB solid medium 20mL, be heated to boiling in microwave oven, be cooled to 37 ℃ of left and right of temperature, add staphylococcus aureus bacterium liquid 1mL, be layered on uniformly on culture dish, after the culture medium cooled and solidified, punch on culture medium with diameter 6mm iron pipe, add 20 μ L central asian sea buckthorn effective site solution in hole, absorb fully to culture medium until solution, put into constant incubator, 37 ℃ of placement 24h of temperature, measure antibacterial circle diameter, in Table 2:
Table 2 central asian sea buckthorn effective site staphylococcus aureus Bactericidal test diameter table
Result shows: central asian sea buckthorn effective site has certain inhibition staphylococcus aureus activity.
Claims (3)
1. the preparation method of a central asian sea buckthorn effective site, is characterized in that the central asian sea buckthorn raw material is the marc after sea buckthorn fruit or oil expression, and concrete operations follow these steps to carry out:
A. the marc after central asian sea buckthorn fruit or oil expression is dried in the shade, pulverize, cross the 40-50 mesh sieve, get the fruit powder of pulverizing, the concentration of doubly measuring with mass volume ratio 5-15 is that 30-90% ethanol heating in water bath refluxes, and bath temperature is 60-95 ℃, extract 1-4 time, time 1-3h, collect extracting solution, decompression recycling ethanol;
B. step a extracting solution is concentrated into to mass concentration 0.067g crude drug/mL, uses saturated NaHCO
3Or Na
2CO
3Solution is adjusted pH to 3-7, again concentrated solution is carried out to purification with macroporous resin, then the ethanol that water and volumetric concentration are 30%-80% carries out eluting successively, collect ethanol elution, wherein the water elution volume is 1-3 BV, the washing flow velocity is 1-4BV/h, and the ethanol elution volume is 1-4BV, and ethanol elution speed is 1-4BV/h;
C. by the ethanol elution of step b, vacuum drying, can obtain central asian sea buckthorn total effective parts content 75-85%, total triterpene contents 35-50% in total effective parts wherein, total phenol content 32-45%.
2. the method for claim 1, is characterized in that with vacuum rotary evaporator, step a extracting solution being concentrated into to mass concentration 0.067g crude drug/mL in step b.
3. the method for claim 1, is characterized in that the macroporous resin in step b is HPD-100, HPD-300, HPD-450, HPD-600, HPD-700, AB-8 or NKA-9 type.
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| CN104127356A (en) * | 2014-08-07 | 2014-11-05 | 中国科学院新疆理化技术研究所 | Sea-buckthorn oropharynx antibacterial and antiphlogistic compositional liquid and preparation method thereof |
| CN104666377A (en) * | 2015-02-02 | 2015-06-03 | 泉州市中医院 | Extraction and purification technology of total triterpenoids in scandent schefflera stem and leaf |
| CN106333977A (en) * | 2015-07-06 | 2017-01-18 | 陕西天奎生物医药科技有限公司 | Natural drug composition for treatment of osteoporotic fracture and/or osteoarthritis and application thereof |
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| CN106333977B (en) * | 2015-07-06 | 2020-02-21 | 陕西天奎生物医药科技有限公司 | Natural pharmaceutical composition for treating osteoporotic fracture and/or osteoarthritis and application thereof |
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| CN111789873A (en) * | 2020-08-04 | 2020-10-20 | 中国科学院西北高原生物研究所 | Method for extracting high-content seabuckthorn triterpenic acid extract |
| CN111789873B (en) * | 2020-08-04 | 2022-05-27 | 中国科学院西北高原生物研究所 | Method for extracting high-content seabuckthorn triterpenic acid extract |
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