CN1650971A - Preparation method of rape myricyl powder effective portion group - Google Patents
Preparation method of rape myricyl powder effective portion group Download PDFInfo
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- CN1650971A CN1650971A CN 200410084433 CN200410084433A CN1650971A CN 1650971 A CN1650971 A CN 1650971A CN 200410084433 CN200410084433 CN 200410084433 CN 200410084433 A CN200410084433 A CN 200410084433A CN 1650971 A CN1650971 A CN 1650971A
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Abstract
A process for preparing the active components of rape melissa powder includes pulverizing or wall-breaking, extracting in alcohol or propanol, concentrating the liquid extract, immersing the dregs in solvent, evaporating solvent, extracting in water, concentrating the liquid extract, dissolving liposoluble extract in alcohol, concentrating, drying to obtain water-soluble active components, mixing them together, and shaping.
Description
Technical field
The present invention relates to prepare from Brassica campestris L (Brassica campestris L) bee pollen (Pollen of BrassinCampestris L) method of Pollen Brassicae campestris effective part group, the Pollen Brassicae campestris effective part group can be used as the primary raw material of related symptoms medicines such as the sound of rain pattering behind preparation anti-prostatic hyperplasia, prostatitis and the frequent micturition that is caused by prostatic hyperplasia, prostatitis, urgent micturition, dysurea, the urine, urine retention, urethra stream are white, sexual dysfunction.
Background technology
Prostate is male's an attached gonad, and its excretory prostatic fluid is the important component part of seminal fluid.It is similar to chestnuts, is positioned at the bladder below, and urethra is just from its middle passing.And prostatic hyperplasia is the distinctive modal sufferer of a kind of chronic male senile patient.Because after people in middle age, intraprostatic connective tissue begins hypertrophy, the comparable normal body of gland of body of gland volume goes out 10-15 greatly doubly when serious, loose prostate stimulates compressing to cause urine urgency-frequency, and the sound of rain pattering is not well, dysuria and symptom, in the course of time also can cause many severe complications, as: urinary tract infection, vesical calculus, renal function injury etc.According to statistics, the male over 50 has existence over half prostatic hyperplasia in various degree, and sickness rate increases with the age, especially with the male's sickness rate after climacteric up to 75%, very big to old people's influence of healthy and quality of life.Prostatic hyperplasia is except that late period, critically ill patient need perform the operation, and Drug therapy is still the most basic and does not lose therapy measure.
At present, the medicine of treatment prostatic hyperplasia can be divided into alpha-blocking agent, 5 inhibitor, plant class preparation and other by the mechanism of action difference.But preceding two kinds of relaxing smooth muscles, the passive factor of releasing urinary tract obstruction is gone back relief of symptoms, plays the effect that takes stopgap measures, but can not reverse prostatic hyperplasia, can not effect a permanent cure.And plant class preparation can suppress the prostatic cell growth, makes the prostate retraction of increase, eliminates the mechanical factor of urethral obstruction, can be rated as and effects a permanent cure.Both domestic and external facts have proved, bee pollen and preparation thereof have good curative effect to prostatic hyperplasia, are the jinxs of prostatic hyperplasia.
Brassica campestris L is the Cruciferae Brassica plants, serves as annual or year this plant of SHENGCAO more of plantation purpose with the Semen Allii Tuberosi oil expression, and Brassica campestris L pollen is its another main economic product.The complicated component of Brassica campestris L pollen, except that as the nutritional supplement, also tool suppresses prostatic hyperplasia, regulates immunity, improves pharmacologically active such as carbohydrate metabolism.Pharmacological evaluation shows that Brassica campestris L pollen can significantly dwindle aged dog and increase volume and exuberant body of prostate, and can improve prostatic hyperplasia patient's symptom, dwindles prostate volume, reduces residual urine, obviously alleviates dysuria.With natural Brassica campestris L pollen is " QIANLIEKANG " preparation that raw material directly is prepared from, and is one of tangible medicine of present clinical treatment prostatic hyperplasia curative effect.
The anti-prostatic hyperplasia Pollen Preparations that external existing Sweden produces by timothy grass 26%, corn 26%, rye (Secale cereale L.) 19%, hazel 26%, bigcatkin willow 6%, Cortex Populi dividianae 6%, OX-eye Daisy 6% and pine 5% totally 8 kind of plant pollen mixed extraction, preparation form, cost an arm and a leg.
Because domestic Pollen Preparations directly is that raw material production forms with the Pollen Brassicae campestris at present, so its taking dose is big, and be difficult for preserving.
It is the pharmaceutical preparation raw material that the domestic people of having proposes with pollen (the not source plant of clear and definite pollen) extract, preparation anti-prostatic hyperplasia medicine, but, then can not guarantee three basic demands that medicine is effective, safe, stable as uncertain pollen source plant.For example to have put down in writing with the high efficiency pollen be raw material to Chinese patent CN 1391911A, extract the method for the pollen extract that obtains anti-prostatic hyperplasia with the acetone merceration, there is following shortcoming in this method: (1) is the used not clear and definite plant origin of pollen of preparation raw material at first, is difficult to set up meet as the medicine basic demand.(2) since acetone volatile, the response rate is extremely low, large-scale production as with acetone as extraction solvent, the production cost height.(3) owing to use acetone extraction, be about to extract without mistake separation purification and originate as pharmaceutical preparation, non-active ingredients fails to remove in the extract like this, and the content of effective ingredient in extract is low, can strengthen dose, makes troubles to the patient.
Summary of the invention
The extracting method that the purpose of this invention is to provide rape myricyl powder effective portion group, realize by following steps: be raw material with the Brassica campestris L pollen, Brassica campestris L pollen is pulverized or breaking cellular wall, soak with the ethanol more than 80% or acetone, chloroform, methanol, petroleum ether and to extract, extracting solution concentrates and promptly gets liposoluble extract; After Pollen Brassicae campestris after solvent soaking extracts is flung to solvent, add purified water and soak extraction, extracting solution concentrates and promptly gets water solubility extract.With the dissolve with ethanol of 40-60%, with petroleum ether or ethyl acetate, chloroform extraction 3-5 time, petroleum ether or ethyl acetate, chloroform extract concentrate, are drying to obtain fat-soluble effective site with liposoluble extract.With water solubility extract and 90% above 4: 1～2: 1 precipitate with ethanol of ethanol volume ratio, filter, filtrate concentrates back and 90% above 1: 2～1: 3 precipitate with ethanol of ethanol volume ratio, filtrate is 1: 3～1: 8 precipitate with ethanol with 90% above ethanol volume ratio again after reclaiming, sucking filtration, filtrate decompression reclaims, and is drying to obtain water solublity effective site.Above-mentioned precipitate with ethanol operation precipitate with ethanol temperature is advisable for 0-5 ℃, and the precipitate with ethanol time was advisable with 12-48 hour, and fat-soluble effective site and water solublity effective site are merged mixing by actual crude drug extracted amount, is the pollen effective part group.The preparation of this pollen effective part group preparation can be soft capsule, capsule, oral liquid.
The present invention is raw material with the Brassica campestris L pollen, Brassica campestris L (Brassica campestris L) is to be this plant of the annual Cheng Yuenian SHENGCAO of purpose with the Semen Allii Tuberosi oil expression, worldwide extensively plantation, China is rapeseed cultivation big country, cultivated area, annual production and consumption figure all rank first in the world, as raw material, aboundresources is easy to get with rape flower section, and annual production is more than 7,000,000 tons.The present invention is an extraction solvent with organic solvents such as ethanol, pollutes for a short time, and cost is low, and is easy to operate.Extract separates through organic solvent extraction, by the screening of animal body inner model, removes the composition of non-activity in the pollen, has kept tool anti-prostatic hyperplasia, prostatitic active component, and effective site is carried out quality control.The present invention is that solvent extracts its water-soluble portion with the purified water again after with its fat-soluble part of ethanol extraction, like this effective ingredient in the pollen is extracted fully, heighten the effect of a treatment, so the present invention has extremely strong practicality.Beneficial effect of the present invention is that also (1) carry out deep development to the Pollen Brassicae campestris preparation that definite curative effect is arranged clinically, clearly is crude drug with the Brassica campestris L pollen, the control quality of medicinal material.(2) with the Brassica campestris L pollen be raw material, the sound of rain pattering, urine retention, urethra flow symptom medicines such as white behind the frequent micturition that preparation anti-prostatic hyperplasia, prostatitis and prostatic hyperplasia, prostatitis cause, urgent micturition, dysurea, the urine, control quality, strengthened curative effect, improved safety.(3) strengthened competitiveness with imported medicine.(4) help taking of drug delivery, storage and patient.
The specific embodiment
The invention will be further described below in conjunction with embodiment.
Embodiment 1
Through feature chromogenic reaction and thin layer chromatography inspection, the fat-soluble active site of Brassica campestris L pollen of the present invention contains a large amount of sterols materials, vegetable fatty acid, small amounts of sugars, aminoacid, the water-soluble active position contains sugar, flavone, amino acids material, the content of fat-soluble active ingredient sterols material in the anti-prostatic hyperplasia medicine among the present invention of usefulness high effective liquid chromatography for measuring:
Instrument: Waters high performance liquid chromatogram instrument
Chromatographic column: C
18Post 4.6mm * 250mm
Mobile phase: acetonitrile-water (97: 3)
Detect wavelength: 210nm
Flow velocity: 1ml/min
The result: the content that records sterols is 15%-35%.
Measure amino acid content in the cole melissa powder valid target of the present invention with amino-acid analyzer: detect wavelength: 540nm, 470nm, condition: exchanger resin, day system 2169 (acid cations), buffer, pH3.3, pH4.2, pH5.20.Developer: 1,2,3-indantrione monohydrate.
The result: amino acid whose content is 2.0-20%.
Contain measurement wavelength 487nm with ultraviolet spectrophotometer by sugar in the phenolsulfuric acid method mensuration effective site of the present invention, record contents of saccharide 10-30%.
Embodiment 2 Pollen Brassicae campestris effective site pharmacology tests of the present invention
1. fat-soluble effective site 500 grams and water solublity effective site 510 grams (pressing the crude drug extracted amount) mix, after getting SD kind rat adaptability and raising a week, the pentobarbital sodium 0.1ml/kg anesthesia of lumbar injection 0.3%, open abdomen, extract bilateral testes, leave and take 10 rats at random and only open abdomen and do not extract testis as sham operated rats.In operation one week of back, neuter is divided into model control group, positive drug control group, investigational agent at random, 10 every group.Except that sham operated rats, other the 3 groups of equal subcutaneous injection Testosterone Propionate of rat injection, 2.0mg/kg once a day, injected 30 days continuously.Dosage gastric infusion 30 days respectively in the according to the form below in the time of injection modeling medicine, model control group is irritated the stomach distilled water.
The influence of table 1 pair weight of prostate (n=10, X ± SD)
| Group | Dosage (the g crude drug/kg) | Body weight (g) | Prostate weight in wet base (mg) | Prostate weight in wet base (mg/100g body weight) |
| The normal control group | ????- | 361.38±18.91 * | ?405.50±44.40 * | 132.23±22.30 * |
| The model contrast | ????- | 348.93±20.61 | ?517.03±67.80 | 164.30±21.40 |
| Positive control | ????2 | 347.63±30.66 | ?488.80±57.35 * | 141.40±18.70 * |
| Investigational agent | ????2 | 340.91±25.16 | ?491.30±89.30 | 143.60±19.70 * |
Annotate: T check between group: compare with model group,
*P＜0.05;
*P＜0.01
The influence of table 2 pair prostate volume (n=10, X ± SD)
| Group | Dosage (the g crude drug/kg) | Prostate volume (cm 3) | Prostate volume (cm 3/ 100g body weight) |
| The normal control group | ????- | ????0.380±0.05 * | ??0.1060±0.0140 ** |
| The model contrast | ????- | ????0.517±0.08 | ??0.1482±0.0210 |
| Positive control | ????2 | ????0.464±0.047 * | ??0.1345±0.0135 * |
| Investigational agent | ????2 | ????0.452±0.066 * | ??0.1330±0.0152 * |
Annotate: T check between group: compare with model group,
*P＜0.05;
*P＜0.01
The influence (n=10) of table 3 pair prostatic hyperplasia degree
| Group | Dosage (the g crude drug/kg) | The prostatic hyperplasia degree | |||
| ????- | ????+ | ????++ | ????+++ | ||
| Normal control | ???- | ????10 | ????0 | ????0 | ????0 |
| The model contrast | ???- | ????0 | ????2 | ????4 | ????4 |
| Positive drug | ????2 | ????3 | ????3 | ????3 | ????1 |
| Investigational agent | ????2 | ????3 | ????3 | ????4 | ????0 |
Annotate: rank test: compare with model group,
*P＜0.05
Grade scale:
"-": prostate is normal
"+": prostate mild swelling, hypertrophy, no obvious inflammation.
" ++ ": prostatic hyperplasia, hypertrophy has mild inflammation.
" +++": the prostatic hyperplasia degree is heavier, loose, and has a matter to soak into.
Experimental result shows: the pollen extract of this law preparation has inhibitory action to the prostatic hyperplasia of rat, observes from the prostata tissue pathological changes, and the administration group is compared with model group, also has significantly to alleviate.
2. effective site excretion of urine test
Effective site reaches 54.7 ± 8.7% and 51.4 ± 22.1% respectively to diastole effect of rabbit urethral smooth muscle and rat bladder contraction during effective site 2.5mg/ml concentration.
Embodiment 3
Get Pollen Brassicae campestris 1000g, drying, mechanical activation comminution is extracted five times with 95% soak with ethanol.Each 24 hours, adding amount of alcohol is each 3000ml, merge extractive liquid,, extracting solution are concentrated into thick about 300ml, obtain liposoluble extract, in liposoluble extract, add 50-60% ethanol 600ml, add petroleum ether extraction 2-4 time behind the mixing, each 1500ml merges, extract is recycled to dried, gets fat-soluble effective site 114g.
Pollen after the ethanol lixiviate is flung to ethanol, add purified water and soak extraction four times, each 8 hours, the amount that adds purified water is each 3000ml, be concentrated into 900ml behind the extracting liquid filtering, obtain water solubility extract, adding 95% ethanol 450ml precipitate with ethanol in water solubility extract spends the night, filtration, filtrate are recycled to 1000ml, add 95% ethanol 2000ml precipitate with ethanol and spend the night, and filtration, filtrate are recycled to 1000ml, add 95% ethanol 4000ml precipitate with ethanol, placement is spent the night, and filtration, filtrate are concentrated into dried, gets water solublity effective site 133g.
114 fat-soluble effective sites of gram and 133 gram water solublity effective site mix homogeneously, promptly get the effective part group of cole melissa treated powder prostatosis.
Embodiment 4
Get Pollen Brassicae campestris 1500g, wall breaking pulverization extracts 6 times with soaked in absolute ethyl alcohol, each 24 hours, add amount of alcohol and be 4500g, merge extractive liquid, at every turn, extracting solution makes and is concentrated into thick about 500ml, obtain liposoluble extract, in liposoluble extract, add 50-60% ethanol 1000ml, add petroleum ether extraction behind the mixing five times, each 2000ml, combining extraction liquid, be concentrated into dried, fat-soluble effective site 168g.
Pollen after the ethanol lixiviate is got is flung to ethanol.Add purified water and soak extraction four times, each 8 hours, the amount that adds purified water is 4500ml at every turn, and extracting liquid filtering is concentrated into 1300ml, obtains water solubility extract, adding dehydrated alcohol 2000ml precipitate with ethanol in water solubility extract spends the night, filtration, filtrate are recycled to 1300ml, add dehydrated alcohol 5200ml precipitate with ethanol, and placement is spent the night, filtration, filtrate are concentrated into dried, get water solublity effective site 180.7g.
168 fat-soluble effective sites of gram and 180.7 gram water solublity effective site mix homogeneously, promptly get the effective part group of cole melissa treated powder prostatosis.
Embodiment 5
Get Pollen Brassicae campestris 1000g, drying, mechanical activation comminution is extracted five times with 95% soak with ethanol.Each 24 hours, adding amount of alcohol is each 3000ml, merge extractive liquid,, extracting solution are concentrated into thick about 300ml, obtain liposoluble extract, in liposoluble extract, add 50-60% ethanol 600ml, add chloroform extraction three times behind the mixing, each 2500ml merges, extract is recycled to dried, gets fat-soluble effective site 124g.
Pollen after the ethanol lixiviate is flung to ethanol, add purified water and soak extraction four times, each 8 hours, the amount that adds purified water is each 3000ml, be concentrated into 900ml behind the extracting liquid filtering, obtain water solubility extract, adding 95% ethanol 450ml precipitate with ethanol in water solubility extract spends the night, filtration, filtrate are recycled to 1000ml, add 95% ethanol 2000ml precipitate with ethanol and spend the night, and filtration, filtrate are recycled to 1000ml, add 95% ethanol 4000ml precipitate with ethanol, placement is spent the night, and filtration, filtrate are recycled to dried, gets water solublity effective site 127g.
124 fat-soluble effective sites of gram and 127 gram water solublity effective site mix homogeneously, promptly get the effective part group of cole melissa treated powder prostatosis.
Embodiment 6
Get Pollen Brassicae campestris 1500g, wall breaking pulverization extracts 6 times with soaked in absolute ethyl alcohol, each 24 hours, add amount of alcohol and be 4500g, merge extractive liquid, at every turn, extracting solution makes and is concentrated into thickly, and about 500ml obtains liposoluble extract, in liposoluble extract, add 50-60% ethanol 1000ml, add chloroform extraction four times behind the mixing, each 2000ml, combining extraction liquid, be recycled to dried, fat-soluble effective site 154g.
Pollen after the ethanol lixiviate is got is flung to ethanol.Add purified water and soak extraction four times, each 8 hours, the amount that adds purified water is 4500ml at every turn, and extracting liquid filtering is concentrated into 1300ml, obtains water solubility extract, adding dehydrated alcohol 2000ml precipitate with ethanol in water solubility extract spends the night, filtration, filtrate are recycled to 1300ml, add dehydrated alcohol 5200ml precipitate with ethanol, and placement is spent the night, filtration, filtrate are recycled to dried, get water solublity effective site 172g.
154 fat-soluble effective sites of gram and 172 gram water solublity effective site mix homogeneously, promptly get the effective part group of cole melissa treated powder prostatosis.
Embodiment 7
Get Pollen Brassicae campestris 1000g, drying, mechanical activation comminution is extracted five times with 95% soak with ethanol.Each 24 hours, adding amount of alcohol is each 3000ml, merge extractive liquid,, extracting solution are concentrated into thick about 300ml, obtain liposoluble extract, in liposoluble extract, add 50-60% ethanol 600ml, add ethyl acetate extraction behind the mixing three times, each 3000ml merges, extract is recycled to dried, gets fat-soluble effective site 132g.
Pollen after the ethanol lixiviate is flung to ethanol, add purified water and soak extraction four times, each 8 hours, the amount that adds purified water is each 3000ml, be concentrated into 900ml behind the extracting liquid filtering, obtain water solubility extract, adding 95% ethanol 450ml precipitate with ethanol in water solubility extract spends the night, filtration, filtrate are recycled to 1000ml, add 95% ethanol 2000ml precipitate with ethanol and spend the night, and filtration, filtrate are recycled to 1000ml, add 95% ethanol 4000ml precipitate with ethanol, placement is spent the night, and filtration, filtrate are recycled to dried, gets water solublity effective site 130g.
132 fat-soluble effective sites of gram and 130 gram water solublity effective site mix homogeneously, promptly get the effective part group of cole melissa treated powder prostatosis.
Embodiment 8
Get Pollen Brassicae campestris 1500g, wall breaking pulverization extracts 6 times with soaked in absolute ethyl alcohol, each 24 hours, add amount of alcohol and be 4500g, merge extractive liquid, at every turn, extracting solution makes and is concentrated into thickly, and about 500ml obtains liposoluble extract, in liposoluble extract, add 50-60% ethanol 1000ml, add ethyl acetate extraction behind the mixing five times, each 2500ml, combining extraction liquid, be recycled to dried, fat-soluble effective site 152g.
Pollen after the ethanol lixiviate is got is flung to ethanol.Add purified water and soak extraction four times, each 8 hours, the amount that adds purified water is 4500ml at every turn, and extracting liquid filtering is concentrated into 1300ml, obtains water solubility extract, adding dehydrated alcohol 2000ml precipitate with ethanol in water solubility extract spends the night, filtration, filtrate are recycled to 1300ml, add dehydrated alcohol 5200ml precipitate with ethanol, and placement is spent the night, filtration, filtrate are recycled to dried, get water solublity effective site 181g.
152 fat-soluble effective sites of gram and 181 gram water solublity effective site mix homogeneously, promptly get the effective part group of cole melissa treated powder prostatosis.
Embodiment 9
Get Pollen Brassicae campestris 1000g, drying, mechanical activation comminution is soaked extraction five times with acetone.Each 24 hours, adding amounts of acetone is each 3000ml, merge extractive liquid,, extracting solution are concentrated into thick about 300ml, obtain liposoluble extract, in liposoluble extract, add 50-60% ethanol 600ml, add petroleum ether extraction behind the mixing four times, each 1500ml merges, extract is recycled to dried, gets fat-soluble effective site 127g.
Pollen behind the acetone extraction is flung to acetone, add purified water and soak extraction four times, each 8 hours, the amount that adds purified water is each 3000ml, be concentrated into 900ml behind the extracting liquid filtering, obtain water solubility extract, adding 95% ethanol 450ml precipitate with ethanol in water solubility extract spends the night, filtration, filtrate are recycled to 1000ml, add 95% ethanol 2000ml precipitate with ethanol and spend the night, and filtration, filtrate are recycled to 1000ml, add 95% ethanol 4000ml precipitate with ethanol, placement is spent the night, and filtration, filtrate are recycled to dried, gets water solublity effective site 125g.
127 fat-soluble effective sites of gram and 125 gram water solublity effective site mix homogeneously, promptly get the effective part group of cole melissa treated powder prostatosis.
Embodiment 10
Get Pollen Brassicae campestris 1000g, drying, mechanical activation comminution is soaked extraction five times with acetone.Each 24 hours, adding amounts of acetone is each 3000ml, merge extractive liquid,, extracting solution are concentrated into thick about 300ml, obtain liposoluble extract, in liposoluble extract, add 50-60% ethanol 600ml, add chloroform extraction four times behind the mixing, each 1500ml merges, extract is recycled to dried, gets fat-soluble effective site 134g.
Pollen behind the acetone extraction is flung to acetone, add purified water and soak extraction four times, each 8 hours, the amount that adds purified water is each 3000ml, be concentrated into 900ml behind the extracting liquid filtering, obtain water solubility extract, adding 95% ethanol 450ml precipitate with ethanol in water solubility extract spends the night, filtration, filtrate are recycled to 1000ml, add 95% ethanol 2000ml precipitate with ethanol and spend the night, and filtration, filtrate are recycled to 1000ml, add 95% ethanol 4000ml precipitate with ethanol, placement is spent the night, and filtration, filtrate are recycled to dried, gets water solublity effective site 135g.
134 fat-soluble effective sites of gram and 135 gram water solublity effective site mix homogeneously, promptly get the effective part group of cole melissa treated powder prostatosis.
Embodiment 11
Get Pollen Brassicae campestris 1500g, wall breaking pulverization soaks extraction 6 times with acetone, each 24 hours, add amounts of acetone and be 4500g, merge extractive liquid, at every turn, extracting solution makes and is concentrated into thickly, and about 500ml obtains liposoluble extract, in liposoluble extract, add 50-60% ethanol 1000ml, add ethyl acetate extraction behind the mixing four times, each 2000ml, combining extraction liquid, be recycled to dried, fat-soluble effective site 142g.
Pollen after acetone extraction is got is flung to acetone.Add purified water and soak extraction four times, each 8 hours, the amount that adds purified water is 4500ml at every turn, and extracting liquid filtering is concentrated into 1300ml, obtains water solubility extract, adding dehydrated alcohol 2000ml precipitate with ethanol in water solubility extract spends the night, filtration, filtrate are recycled to 1300ml, add dehydrated alcohol 5200ml precipitate with ethanol, and placement is spent the night, filtration, filtrate are recycled to dried, get water solublity effective site 161g.
142 fat-soluble effective sites of gram and 161 gram water solublity effective site mix homogeneously, promptly get the effective part group of cole melissa treated powder prostatosis.
Embodiment 12
Get Pollen Brassicae campestris 1000g, drying, mechanical activation comminution is soaked extraction five times with methanol.Each 24 hours, adding quantity of methyl alcohol is each 3000ml, merge extractive liquid,, extracting solution are concentrated into thick about 300ml, obtain liposoluble extract, in liposoluble extract, add 50-60% ethanol 600ml, add petroleum ether extraction behind the mixing five times, each 1500ml merges, extract is recycled to dried, gets fat-soluble effective site 135g.
Pollen after the methanol lixiviate is flung to methanol, add purified water and soak extraction four times, each 8 hours, the amount that adds purified water is each 3000ml, be concentrated into 900ml behind the extracting liquid filtering, obtain water solubility extract, adding 95% ethanol 450ml precipitate with ethanol in water solubility extract spends the night, filtration, filtrate are recycled to 1000ml, add 95% ethanol 2000ml precipitate with ethanol and spend the night, and filtration, filtrate are recycled to 1000ml, add 95% ethanol 4000ml precipitate with ethanol, placement is spent the night, and filtration, filtrate are recycled to dried, gets water solublity effective site 123g.
135 fat-soluble effective sites of gram and 123 gram water solublity effective site mix homogeneously, promptly get the effective part group of cole melissa treated powder prostatosis.
Embodiment 13
Get Pollen Brassicae campestris 1000g, drying, mechanical activation comminution is soaked extraction five times with methanol.Each 24 hours, adding quantity of methyl alcohol is each 3000ml, merge extractive liquid,, extracting solution are concentrated into thick about 300ml, obtain liposoluble extract, in liposoluble extract, add 50-60% ethanol 600ml, add chloroform extraction four times behind the mixing, each 1500ml merges, extract is recycled to dried, gets fat-soluble effective site 128g.
Pollen after the methanol lixiviate is flung to methanol, add purified water and soak extraction four times, each 8 hours, the amount that adds purified water is each 3000ml, be concentrated into 900ml behind the extracting liquid filtering, obtain water solubility extract, adding 95% ethanol 450ml precipitate with ethanol in water solubility extract spends the night, filtration, filtrate are recycled to 1000ml, add 95% ethanol 2000ml precipitate with ethanol and spend the night, and filtration, filtrate are recycled to 1000ml, add 95% ethanol 4000ml precipitate with ethanol, placement is spent the night, and filtration, filtrate are recycled to dried, gets water solublity effective site 126g.
128 fat-soluble effective sites of gram and 126 gram water solublity effective site mix homogeneously, promptly get the effective part group of cole melissa treated powder prostatosis.
Embodiment 14
Get Pollen Brassicae campestris 1500g, wall breaking pulverization soaks extraction 6 times with methanol, each 24 hours, add quantity of methyl alcohol and be 4500g, merge extractive liquid, at every turn, extracting solution makes and is concentrated into thickly, and about 500ml obtains liposoluble extract, in liposoluble extract, add 50-60% ethanol 1000ml, add ethyl acetate extraction behind the mixing four times, each 2000ml, combining extraction liquid, be recycled to dried, fat-soluble effective site 156g.
Pollen after the methanol lixiviate is got is flung to methanol.Add purified water and soak extraction four times, each 8 hours, the amount that adds purified water is 4500ml at every turn, and extracting liquid filtering is concentrated into 1300ml, obtains water solubility extract, adding dehydrated alcohol 2000ml precipitate with ethanol in water solubility extract spends the night, filtration, filtrate are recycled to 1300ml, add dehydrated alcohol 5200ml precipitate with ethanol, and placement is spent the night, filtration, filtrate are recycled to dried, get water solublity effective site 154g.
156 fat-soluble effective sites of gram and 154 gram water solublity effective site mix homogeneously, promptly get the effective part group of cole melissa treated powder prostatosis.
Embodiment 15
Get Pollen Brassicae campestris 1000g, drying, mechanical activation comminution is soaked extraction five times with petroleum ether.Each 24 hours, adding the petroleum ether amount was each 3000ml, merge extractive liquid,, be recycled to dried, fat-soluble effective site 136g.
Pollen after the petroleum ether lixiviate is flung to petroleum ether, add purified water and soak extraction four times, each 8 hours, the amount that adds purified water is each 3000ml, be concentrated into 900ml behind the extracting liquid filtering, obtain water solubility extract, adding 95% ethanol 450ml precipitate with ethanol in water solubility extract spends the night, filtration, filtrate are recycled to 1000ml, add 95% ethanol 2000ml precipitate with ethanol and spend the night, and filtration, filtrate are recycled to 1000ml, add 95% ethanol 4000ml precipitate with ethanol, placement is spent the night, and filtration, filtrate are recycled to dried, gets water solublity effective site 135g.
136 fat-soluble effective sites of gram and 135 gram water solublity effective site mix homogeneously, promptly get the effective part group of cole melissa treated powder prostatosis.
Embodiment 16
Get Pollen Brassicae campestris 1000g, drying, mechanical activation comminution is extracted five times with 95% soak with ethanol.Each 24 hours, adding amount of alcohol is each 3000ml, and merge extractive liquid,, extracting solution are concentrated into thick about 300ml, obtain liposoluble extract, in liposoluble extract, add 50-60% ethanol 600ml, add 1: 1 kieselguhr mixing drying after, add Petroleum ether extraction four times, each 1500ml, merge, be recycled to dried, fat-soluble effective site 124g.
Pollen after the ethanol lixiviate is flung to ethanol, add purified water and soak extraction four times, each 8 hours, the amount that adds purified water is each 3000ml, be concentrated into 900ml behind the extracting liquid filtering, obtain water solubility extract, adding 95% ethanol 450ml precipitate with ethanol in water solubility extract spends the night, filtration, filtrate are recycled to 1000ml, add 95% ethanol 2000ml precipitate with ethanol and spend the night, and filtration, filtrate are recycled to 1000ml, add 95% ethanol 4000ml precipitate with ethanol, placement is spent the night, and filtration, filtrate are recycled to dried, gets water solublity effective site 130g.
124 fat-soluble effective sites of gram and 130 gram water solublity effective site mix homogeneously, promptly get the effective part group of cole melissa treated powder prostatosis.
Embodiment 17
Get Pollen Brassicae campestris 1500g, wall breaking pulverization extracts 6 times with soaked in absolute ethyl alcohol, each 24 hours, add amount of alcohol and be 4500g, merge extractive liquid, at every turn, extracting solution makes and is concentrated into thickly, and about 500ml obtains liposoluble extract, in liposoluble extract, add 50-60% ethanol 1000ml, add 1: 1 kieselguhr behind the mixing, add Petroleum ether extraction after the mixing drying three times, each 3000ml, merge, be recycled to dried, fat-soluble effective site 163g.
Pollen after the ethanol lixiviate is got is flung to ethanol.Add purified water and soak extraction four times, each 8 hours, the amount that adds purified water is 4500ml at every turn, and extracting liquid filtering is concentrated into 1300ml, obtains water solubility extract, adding dehydrated alcohol 2000ml precipitate with ethanol in water solubility extract spends the night, filtration, filtrate are recycled to 1300ml, add dehydrated alcohol 5200ml precipitate with ethanol, and placement is spent the night, filtration, filtrate are recycled to dried, get water solublity effective site 169g.
163 fat-soluble effective sites of gram and 169 gram water solublity effective site mix homogeneously, promptly get the effective part group of cole melissa treated powder prostatosis.
Embodiment 18
Get Pollen Brassicae campestris 1000g, drying, mechanical activation comminution is soaked extraction five times with methanol.Each 24 hours, adding quantity of methyl alcohol is each 3000ml, and merge extractive liquid,, extracting solution are concentrated into thick about 300ml, obtain liposoluble extract, in liposoluble extract, add 50-60% ethanol 600ml, add 1: 1 kieselguhr behind the mixing, add Petroleum ether extraction after the mixing drying five times, each 2500ml, merge, extracting solution is recycled to dried, gets fat-soluble effective site 133g.
Pollen after the methanol lixiviate is flung to methanol, add purified water and soak extraction four times, each 8 hours, the amount that adds purified water is each 3000ml, be concentrated into 900ml behind the extracting liquid filtering, obtain water solubility extract, adding 95% ethanol 450ml precipitate with ethanol in water solubility extract spends the night, filtration, filtrate are recycled to 1000ml, add 95% ethanol 2000ml precipitate with ethanol and spend the night, and filtration, filtrate are recycled to 1000ml, add 95% ethanol 4000ml precipitate with ethanol, placement is spent the night, and filtration, filtrate are recycled to dried, gets water solublity effective site 138g.
133 fat-soluble effective sites of gram and 138 gram water solublity effective site mix homogeneously, promptly get the effective part group of cole melissa treated powder prostatosis.
Claims (12)
1. the extracting method of rape myricyl powder effective portion group, be to be raw material with the Brassica campestris L pollen, use organic solvent extraction, it is characterized in that: after the in advance dry and pulverization process of Brassica campestris L pollen, the reuse organic solvent soaks, extraction, carry out according to the following steps: (1) extracting solution concentrates and promptly gets liposoluble extract again, with the dissolve with ethanol of liposoluble extract with 40-60%, petroleum ether extraction, extract concentrate, are drying to obtain fat-soluble effective site; (2) after the Brassica campestris L pollen after solvent soaking is extracted is flung to solvent, add purified water and soak and extract, extracting solution concentrates and promptly gets water solubility extract, ethanol mixing more than water solubility extract and 90% is carried out precipitate with ethanol, filter, filtrate decompression reclaims, and is drying to obtain water solublity effective site; (3) fat-soluble effective site and water solublity effective site are pressed the actual crude drug extracted amount merging of pollen mixing, be rape myricyl powder effective portion group.
2. the extracting method of rape myricyl powder effective portion group according to claim 1 is characterized in that: step 1. in liposoluble extract carry out 3-5 dissolve with ethanol and petroleum ether or ethyl acetate, chloroform extraction.
3. the extracting method of rape myricyl powder effective portion group according to claim 1, it is characterized in that: the 2. middle precipitate with ethanol operation of step is carried out according to the following steps: 1. the ethanol more than the water solubility extract and 90% carried out precipitate with ethanol in 4: 1 by volume～2: 1 one time, filter, 2. the ethanol more than the concentrated back of filtrate and 90% carried out the secondary precipitate with ethanol in 1: 2 by volume～1: 3, filter, 3. filtrate was carried out precipitate with ethanol in 1: 3 by volume～1: 8 three times with 90% above ethanol after concentrating again.
4. according to the extracting method of claim 1 and 3 described rape myricyl powder effective portion groups, it is characterized in that: the described precipitate with ethanol time is 12-48 hour.
5. according to the extracting method of claim 1 and 3 described rape myricyl powder effective portion groups, it is characterized in that: the precipitate with ethanol temperature is 0-5 ℃ in the described precipitate with ethanol operation.
6. the extracting method of rape myricyl powder effective portion group according to claim 1, it is characterized in that: the content of described fat-soluble effective site in Brassica campestris L pollen is mass fraction 5%-35%.
7. according to the extracting method of claim 1 and 6 described rape myricyl powder effective portion groups, it is characterized in that: fat-soluble effective site mainly contains materials such as phytosterol, vegetable fatty acid, aminoacid, and wherein sterols material and fatty acid material are mass fraction 20-80% at fat-soluble effective site content.
8. the extracting method of rape myricyl powder effective portion group according to claim 1, it is characterized in that: the content of described water solublity effective site in Brassica campestris L pollen is mass fraction 5-45%.
9. according to the extracting method of claim 1 and 8 described rape myricyl powder effective portion groups, it is characterized in that: described water solublity effective site contains materials such as aminoacid, flavone, saccharide, wherein amino acid content is mass fraction 2-20%, contents of saccharide is that mass fraction is 10-50%, and flavones content is mass fraction 5-30%.
10. the extracting method of rape myricyl powder effective portion group according to claim 1, it is characterized in that: the mass fraction yield of fat-soluble effective site in the Brassica campestris L pollen crude drug is 5-19%.
11. the extracting method of rape myricyl powder effective portion group according to claim 1 is characterized in that: the mass fraction yield of water solublity effective site in the Brassica campestris L pollen crude drug is 8-22%.
12. want the extracting method of the arbitrary described rape myricyl powder effective portion group of 1-11 according to right, it is characterized in that: treatment anti-prostatic hyperplasia, the prostatitic preparation of effective part group preparation are soft capsule, capsule, oral liquid.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100362941C (en) * | 2005-09-28 | 2008-01-23 | 苏明寿 | Soup seasoning possessing full nutrition and health care function |
| CN101978864A (en) * | 2010-09-28 | 2011-02-23 | 中国农业科学院蜜蜂研究所 | Rape bee-pollen extract and use thereof |
| CN102688178A (en) * | 2011-05-06 | 2012-09-26 | 湖南明园蜂业科技有限公司 | Application of rape bee pollen extract in anti-aging skin care products |
| CN103540397A (en) * | 2012-07-13 | 2014-01-29 | 北京市蜂业公司 | Extraction method of fat substances rich in pollen |
| CN108593826A (en) * | 2018-06-04 | 2018-09-28 | 中国农业科学院蜜蜂研究所 | A method of differentiating Bee Pollen source |
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2004
- 2004-11-19 CN CNB2004100844336A patent/CN1325069C/en not_active Expired - Fee Related
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100362941C (en) * | 2005-09-28 | 2008-01-23 | 苏明寿 | Soup seasoning possessing full nutrition and health care function |
| CN101978864A (en) * | 2010-09-28 | 2011-02-23 | 中国农业科学院蜜蜂研究所 | Rape bee-pollen extract and use thereof |
| CN101978864B (en) * | 2010-09-28 | 2013-04-10 | 中国农业科学院蜜蜂研究所 | Rape bee-pollen extract and use thereof |
| CN102688178A (en) * | 2011-05-06 | 2012-09-26 | 湖南明园蜂业科技有限公司 | Application of rape bee pollen extract in anti-aging skin care products |
| CN102688178B (en) * | 2011-05-06 | 2013-08-21 | 湖南明园蜂业科技有限公司 | Application of rape bee pollen extract in anti-aging skin care products |
| CN103540397A (en) * | 2012-07-13 | 2014-01-29 | 北京市蜂业公司 | Extraction method of fat substances rich in pollen |
| CN103540397B (en) * | 2012-07-13 | 2015-01-21 | 北京市蜂业公司 | Extraction method of fat substances rich in pollen |
| CN108593826A (en) * | 2018-06-04 | 2018-09-28 | 中国农业科学院蜜蜂研究所 | A method of differentiating Bee Pollen source |
| CN108593826B (en) * | 2018-06-04 | 2020-05-19 | 中国农业科学院蜜蜂研究所 | Method for identifying source of bee pollen |
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|---|---|
| CN1325069C (en) | 2007-07-11 |
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