CN102512463A - Extraction method of nettle extract - Google Patents
Extraction method of nettle extract Download PDFInfo
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- CN102512463A CN102512463A CN2012100037863A CN201210003786A CN102512463A CN 102512463 A CN102512463 A CN 102512463A CN 2012100037863 A CN2012100037863 A CN 2012100037863A CN 201210003786 A CN201210003786 A CN 201210003786A CN 102512463 A CN102512463 A CN 102512463A
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Abstract
The invention relates to the technical field of medicaments, in particular to an extraction method of a nettle extract. The yield of the nettle extract obtained by the extraction method is 46.5 to 49.6 percent. The nettle extract can be used for preparing the medicaments for treating prostatitis, prostatomegaly, benign hyperplasia of prostate or high blood pressure and can effectively treat prostatitis, prostatomegaly, benign hyperplasia of prostate or high blood pressure. The effective rate of the nettle extract on acute prostatitis is 93.33 percent; the effective rate of the nettle extract on chronic prostatitis is 90.33 percent; the effective rate of the nettle extract on prostatomegaly is 89.0 percent; the effective rate of the nettle extract on benign hyperplasia of prostate is 90.67 percent; and the effective rate of the nettle extract on high blood pressure is 91.0 percent.
Description
Technical field
The present invention relates to medical technical field, particularly the method for distilling of Herba Urticae Cannabinae extract.
Background technology
Herba Urticae Cannabinae is a Urticaceae Herba Urticae Cannabinae wild herb for many years, and this plant is that traditional medicine is eaten the wild plant with usefulness, compositions such as its rich in proteins, polysaccharide, flavone compound, aminoacid.It is edible that this plant children can cook wild vegetable when tender, has medical value after the florescence.Herba Urticae Cannabinae has expelling wind for relieving convulsion, and the effect of the relieving constipation that helps digestion is used for rheumatic arthritis, puerperal convulsion, infantile convulsion, poliomyelitis sequela, hypertension, dyspepsia, constipation; External is controlled urticaria from the beginning of, venom.Modern study proves that Herba Urticae Cannabinae has better curative effect to the male prostate hyperplasia of prostate.On the clinical treatment, Herba Urticae Cannabinae is applied to treating urticaria, rheumatic arthritis already, adopts the modern science and technology deep processing; The polysaccharide active components that it is contained extracts, and is used for prostatitis, prostate hyperplasia; Benign prostatic hyperplasia, the treatment of aspects such as hypertension has better curative effect.
The Herba Urticae Cannabinae extract yield that present extraction process obtains is not high, therefore, a kind of method for distilling of Herba Urticae Cannabinae extract is provided, and has realistic meaning.
Summary of the invention
In view of this, the present invention provides a kind of method for distilling of Herba Urticae Cannabinae extract.The yield of the Herba Urticae Cannabinae extract that this method for distilling obtains is 46.5～49.6%, can be used for preparation treatment prostatitis, prostate hyperplasia, benign prostatic hyperplasia or hypertension drug.
In order to realize the foregoing invention purpose, the present invention provides following technical scheme:
The invention provides a kind of method for distilling of Herba Urticae Cannabinae extract, comprise the steps:
Step 1: get Herba Urticae Cannabinae and add excessive water hyperpressure extraction 8～10min under 300～500MPa, 15～35 ℃ condition, filtering and collecting filter liquid, being concentrated into relative density through first is 1.12～1.15 (70～80 ℃), obtains first extractum;
Step 2: get said first extractum after 3～5 ℃ of dialysis, collect to keep liquid, with the mixed solution of chloroform and n-butyl alcohol through sevage method deproteinization, collect water layer, it is 1.12～1.15 (70～80 ℃) that warp second is concentrated into relative density, obtains second extractum;
Step 3: getting said second extractum, to add concentration be ethanol precipitate with ethanol 20～24h of 80～95%, and sediment is collected in centrifugal back, adds the entry stirring and dissolving; Being concentrated into relative density through the 3rd is 1.12～1.18 (70～80 ℃); Obtain the 3rd extractum, filtering and collecting filter liquid promptly gets; In g/mL, said second extractum and alcoholic acid mass volume ratio are 1～3, and the mass volume ratio of said sediment and water is 1: 3～7.
Said relative density is a material at 70～80 ℃ density and the water ratio 70～80 ℃ density.
Sevage method: the characteristics of utilizing protein degeneration in organic solvents such as trichloroethane; Is to mix at 1: 1 extracting solution and Sevage reagent [chloroform: n-butyl alcohol=5: 1 (V/V)] according to volume ratio; Vibration, centrifugal, the protein after the degeneration is between extracting solution and Sevage reagent intersection.The advantage of this method is a mild condition, can not cause the degeneration of polysaccharide.
In embodiment provided by the invention, the method for distilling of Herba Urticae Cannabinae extract provided by the invention, in the step 1, in g/mL, the mass volume ratio of said Herba Urticae Cannabinae and water is 1: 10～15.
In embodiment provided by the invention, the method for distilling of Herba Urticae Cannabinae extract provided by the invention, the 22mm semipermeable membrane is selected in said dialysis for use.
In embodiment provided by the invention, the method for distilling of Herba Urticae Cannabinae extract provided by the invention, said first concentrate, second concentrate or the 3rd simmer down at 70～80 ℃, vacuum is to concentrate under the condition of 0.06MPa.
In embodiment provided by the invention, the method for distilling of Herba Urticae Cannabinae extract provided by the invention, the volume ratio of chloroform and n-butyl alcohol is 5: 1 in the said mixed solution.
In embodiment provided by the invention, the method for distilling of Herba Urticae Cannabinae extract provided by the invention, the volume ratio that keeps liquid and said mixed solution described in the step 2 is 1: 1.
In embodiment provided by the invention, the method for distilling of Herba Urticae Cannabinae extract provided by the invention, collect water layer described in the step 2 after, said second also comprise through the filtering step of 300 order filter clothes before concentrating.
In embodiment provided by the invention, the method for distilling of Herba Urticae Cannabinae extract provided by the invention, centrifugal described in the step 3 is centrifugal 15min under the condition of 3000rpm.
In embodiment provided by the invention, the method for distilling of Herba Urticae Cannabinae extract provided by the invention, step 3 also comprises spray-dired step after filtering and collecting filtrating; Spray-dired EAT is 120 ℃, and leaving air temp is 80 ℃.
The Herba Urticae Cannabinae extract that the present invention also provides the said extracted method to obtain.
The application of Herba Urticae Cannabinae extract in preparation treatment prostatitis, prostate hyperplasia, benign prostatic hyperplasia or hypertension drug that the present invention also provides the said extracted method to obtain.
The invention provides a kind of method for distilling of Herba Urticae Cannabinae extract.The yield of the Herba Urticae Cannabinae extract that this method for distilling obtains is 46.5～49.6%, can be used for preparation treatment prostatitis, prostate hyperplasia, benign prostatic hyperplasia or hypertension drug.Herba Urticae Cannabinae extract provided by the invention can effectively be treated prostatitis, prostate hyperplasia, benign prostatic hyperplasia or hypertension.Its effective percentage to acute prostatitis is 93.33%, is 90.33% to the effective percentage of chronic prostatitis, is 89.0% to the effective percentage of prostate hyperplasia, is 90.67% to the effective percentage of benign prostatic hyperplasia, is 91.0% to hypertensive effective percentage.
The specific embodiment
The invention discloses a kind of method for distilling of Herba Urticae Cannabinae extract, those skilled in the art can use for reference this paper content, suitably improve technological parameter and realize.Special needs to be pointed out is that all similarly replace and change apparent to those skilled in the art, they all are regarded as and are included in the present invention.Method of the present invention and application are described through preferred embodiment; The related personnel obviously can change or suitably change and combination methods and applications as herein described in not breaking away from content of the present invention, spirit and scope, realizes and use technology of the present invention.
In the method for distilling of Herba Urticae Cannabinae extract provided by the invention, raw materials used and reagent all can be buied by market.
Below in conjunction with embodiment, further set forth the present invention:
The preparation of embodiment 1 Herba Urticae Cannabinae extract
Get urtica angustifolia medical material 100g, add 15 times of water gagings after the pulverizing, hyperpressure is 300MPa, and 15 ℃ were extracted 10 minutes; Extracting liquid filtering is 70 ℃ in temperature, and vacuum is to be concentrated into relative density 1.12 (70 ℃) under the condition of 0.06MPa; After concentrated solution cooled, in the bag filter of the 22mm semipermeable membrane of packing into, place the stainless steel cask that fills phosphate buffer; Under 5 ℃, dialyse, remove freshen and some small molecular weight impurities, during exchange buffering liquid 3-4 time.Get the reservation liquid in the bag filter, with sevage method deproteinization, remove the middle white flocculent deposit, the water intaking layer is 70 ℃ in temperature; Vacuum is that to be concentrated into relative density under the condition of 0.06MPa be 1.12 (70 ℃), obtains extractum 52g, adds 1 times and measures 95% ethanol precipitate with ethanol; Left standstill 20 hours, it is centrifugal to collect sediment, reclaims ethanol; Adding 3 times of water gaging stirring and dissolving again, is 70 ℃ in temperature, and vacuum is to be concentrated into relative density 1.12 (70 ℃) under the condition of 0.06MPa; Filter, spray drying promptly gets Herba Urticae Cannabinae extract 5.1g.
Herba Urticae Cannabinae extract to obtaining detects, and the result is following:
The discriminating of polysaccharide from urtica fissa: discrimination method is phenolsulfuric acid reagent reacting (positive), contains polysaccharide from urtica fissa in the Herba Urticae Cannabinae extract provided by the invention.
Polysaccharide from urtica fissa content: 46.5% (measuring) with the phenolsulfuric acid method
Polysaccharide from urtica fissa molecular weight determination: 53010Da (with reference to two appendix VH of pharmacopeia in 2010).
The preparation of embodiment 2 Herba Urticae Cannabinae extracts
Get Herba Urticae Cannabinae medical material 100g, add 10 times of water gagings after the pulverizing, hyperpressure is 500MPa, and 35 ℃ were extracted 8 minutes; Extracting liquid filtering is 80 ℃ in temperature, and vacuum is to be concentrated into relative density 1.15 (80 ℃) under the condition of 0.06MPa; After concentrated solution cooled, in the bag filter of the 22mm semipermeable membrane of packing into, place the stainless steel cask that fills phosphate buffer; Under 3 ℃, dialyse, remove freshen and some small molecular weight impurities, during exchange buffering liquid 3-4 time.Get the reservation liquid in the bag filter, with sevage method deproteinization, remove the middle white flocculent deposit, the water intaking layer is 80 ℃ in temperature; Vacuum is that to be concentrated into relative density under the condition of 0.06MPa be 1.15 (80 ℃), obtains extractum 54g, adds 3 times and measures 80% ethanol precipitate with ethanol; Left standstill 24 hours, it is centrifugal to collect sediment, reclaims ethanol; Adding 7 times of water gaging stirring and dissolving again, is 80 ℃ in temperature, and vacuum is to be concentrated into relative density 1.18 (80 ℃) under the condition of 0.06MPa; Filter, spray drying promptly gets Herba Urticae Cannabinae extract 5.5g.
Herba Urticae Cannabinae extract to obtaining detects, and the result is following:
The discriminating of polysaccharide from urtica fissa: discrimination method is phenolsulfuric acid reagent reacting (positive), contains polysaccharide from urtica fissa in the Herba Urticae Cannabinae extract provided by the invention.
Polysaccharide from urtica fissa content: 47.1% (measuring) with the phenolsulfuric acid method
Polysaccharide from urtica fissa molecular weight determination: 51980Da (with reference to two appendix VH of pharmacopeia in 2010).
The preparation of embodiment 3 Herba Urticae Cannabinae extracts
Get Herba Urticae Cannabinae medical material 100g, add 13 times of water gagings after the pulverizing, hyperpressure is 400MPa, and 25 ℃ were extracted 9 minutes; Extracting liquid filtering is 73 ℃ in temperature, and vacuum is to be concentrated into relative density 1.13 (70 ℃) under the condition of 0.06MPa; After concentrated solution cooled, in the bag filter of the 22mm semipermeable membrane of packing into, place the stainless steel cask that fills phosphate buffer; Under 4 ℃, dialyse, remove freshen and some small molecular weight impurities, during exchange buffering liquid 3-4 time.Get the reservation liquid in the bag filter, with sevage method deproteinization, remove the middle white flocculent deposit, the water intaking layer is 73 ℃ in temperature; Vacuum is that to be concentrated into relative density under the condition of 0.06MPa be 1.13 (70 ℃), obtains extractum 50g, adds 1.5 times and measures 90% ethanol precipitate with ethanol; Left standstill 22 hours, it is centrifugal to collect sediment, reclaims ethanol; Adding 5 times of water gaging stirring and dissolving again, is 73 ℃ in temperature, and vacuum is to be concentrated into relative density 1.15 (70 ℃) under the condition of 0.06MPa; Filter, spray drying promptly gets Herba Urticae Cannabinae extract 4.9g.
Herba Urticae Cannabinae extract to obtaining detects, and the result is following:
The discriminating of polysaccharide from urtica fissa: discrimination method is phenolsulfuric acid reagent reacting (positive), contains polysaccharide from urtica fissa in the Herba Urticae Cannabinae extract provided by the invention.
Polysaccharide from urtica fissa content: 46.8% (measuring) with the phenolsulfuric acid method
Polysaccharide from urtica fissa molecular weight determination: 56850Da (with reference to two appendix VH of pharmacopeia in 2010).
The preparation of embodiment 4 Herba Urticae Cannabinae extracts
Get urtica angustifolia medical material 100g, add 12 times of water gagings after the pulverizing, hyperpressure is 350MPa, and 30 ℃ were extracted 8 minutes; Extracting liquid filtering is 78 ℃ in temperature, and vacuum is to be concentrated into relative density 1.14 (80 ℃) under the condition of 0.06MPa; After concentrated solution cooled, in the bag filter of the 22mm semipermeable membrane of packing into, place the stainless steel cask that fills phosphate buffer; Under 5 ℃, dialyse, remove freshen and some small molecular weight impurities, during exchange buffering liquid 3-4 time.Get the reservation liquid in the bag filter, with sevage method deproteinization, remove the middle white flocculent deposit, the water intaking layer is 78 ℃ in temperature; Vacuum is that to be concentrated into relative density under the condition of 0.06MPa be 1.14 (80 ℃), obtains extractum g, adds 2.3 times and measures 85% ethanol precipitate with ethanol; Left standstill 23 hours, it is centrifugal to collect sediment, reclaims ethanol; Adding 4 times of water gaging stirring and dissolving again, is 78 ℃ in temperature, and vacuum is to be concentrated into relative density 1.16 (80 ℃) under the condition of 0.06MPa; Filter, spray drying promptly gets Herba Urticae Cannabinae extract 5.3g.
Herba Urticae Cannabinae extract to obtaining detects, and the result is following:
The discriminating of polysaccharide from urtica fissa: discrimination method is phenolsulfuric acid reagent reacting (positive), contains polysaccharide from urtica fissa in the Herba Urticae Cannabinae extract provided by the invention.
Polysaccharide from urtica fissa content: 49.6% (measuring) with the phenolsulfuric acid method
Polysaccharide from urtica fissa molecular weight determination: 57140Da (with reference to two appendix VH of pharmacopeia in 2010).
Embodiment 5 evaluating drug effects
Test group: the Herba Urticae Cannabinae extract that the embodiment of the invention 1 to 4 provides, prostatitis, prostate hyperplasia, benign prostatic hyperplasia, each 300 patient of hypertension are treated; Take every day three times, take 2～4g at every turn;
The positive drug matched group: positive drug is treated prostatitis, prostate hyperplasia, benign prostatic hyperplasia, each 300 patient of hypertension; Every day three times, take 4～8, every 0.5g at every turn.
Acute prostatitis:
Cure: transference cure, local swelling is disappeared, and does not have and touches a tender spot, continuous more than 3 times examination of prostatic fluid be normally;
Effectively: doing well,improving, but the prostatic fluid routine examination does not still reach arm's length standard;
Invalid: after treating for 1 week, symptom and sign does not still have the improver.
Chronic prostatitis:
Cure: subjective symptoms disappears; The prostate tenderness disappears during palpation, quality deliquescing or improvement; The test of location segmentation urine is normal; Prostatic fluid microscopy leukocyte count＜10/HPF, antibacterial culturing is negative, and continuous review is normal more than 2 times.
Effectively: subjective symptoms disappears or partial symptoms is improved, disappeared; Normal or the improvement of palpation prostate; Prostatic fluid microscopy leukocyte count still＞10/HPF, take a favorable turn before the treatment, or antibacterial culturing is still positive.
Invalid: symptom and prostatic fluid microscopy all do not have improvement.
Prostate hyperplasia:
Recovery from illness: main clinic symptoms disappears, unobstructed micturition, urine flow rate parameter normally or normal basically, residual urine amount＜20ml, nocturia number of times＜2 time, prostate volume is near normally or before dwindling more than 1/4;
Effectively: symptom disappears basically, and it is conscious unobstructed to urinate, and urine flow rate parameter is near normal, residual urine amount＜50ml or more preceding minimizing 1/2, and nocturia＜3 time, prostate volume has and dwindles; Or urine flow rate parameter has improvement before the treatment, before residual urine amount is less than treatment, and the more preceding minimizing of nocturia number of times;
Invalid: symptom does not have improvement, and urine flow rate, residual urine amount do not have change.
(Benign Prostatic Hyperplasia is histology's noun BPH) to benign prostatic hyperplasia, refers to betide the prostate-urethra peripheral region, is the lysis of characteristic with substrate and epithelial hyperplasia.BPH is one of modal disease of elderly men.Usually (Low urinary tract symptoms LUTS), comprising: frequent micturition, urgent micturition, nocturia, urine stream are unable, urine stream interrupts and the urine retention sense to show as a series of bothersome lower urinary tract symptoms clinically.These symptoms can influence its quality of life through daily routines and the nighttime sleep that disturbs patient.
Curative effect determinate standard:
Recovery from illness: clinical symptom disappearance, physical examination, rectal touch, urinalysis >=90% patient recover normal.
Take a turn for the better: clinical symptom relief, physical examination, rectal touch, urinalysis >=60% patient are tending towards normal.
Invalid: before and after the treatment, inspection such as clinical symptoms and physical examination, rectal touch, urinalysis does not have improvement or does not have obviously and improve, and it is normal that≤30% patient is tending towards.
Hypertension:
Curative effect determinate standard:
Recovery from illness: >=90% patient's controlling of blood pressure is below horizontal at 140/90mmHg, does not have obvious clinical symptoms;
Take a turn for the better: >=60% patient's controlling of blood pressure is below horizontal at 140/90mmHg, clinical symptom relief;
Invalid: it is below horizontal that≤30% patient's blood pressure does not reach 140/90mmHg, and clinical symptoms does not have improvement or do not have obviously and improve.
The result sees table 1.
Table 1 frog peel extract provided by the invention or the frog skeleton extract test of pesticide effectiveness
Can know that by table 1 result the Herba Urticae Cannabinae extract that the embodiment of the invention 1 to 4 provides is compared with the positive drug matched group, the effective percentage of acute prostatitis is increased to 93.33% by 78.0%; Effective percentage to chronic prostatitis is increased to 90.33% by 74.67%; Effective percentage to prostate hyperplasia is increased to 89.0% by 78.33%; Effective percentage to benign prostatic hyperplasia is increased to 90.67% by 75.67%; Hypertensive effective percentage is increased to 91.0% by 73.33%, and difference all has significance (P＜0.05).
Comprehensive The above results, the Herba Urticae Cannabinae extract that the embodiment of the invention 1 to 4 provides is compared with the positive drug matched group, has significantly improved drug effect.
The above only is a preferred implementation of the present invention; Should be pointed out that for those skilled in the art, under the prerequisite that does not break away from the principle of the invention; Can also make some improvement and retouching, these improvement and retouching also should be regarded as protection scope of the present invention.
Claims (10)
1. the method for distilling of a Herba Urticae Cannabinae extract is characterized in that, comprises the steps:
Step 1: get Herba Urticae Cannabinae and add excessive water hyperpressure extraction 8～10min under 300～500MPa, 15～35 ℃ condition, filtering and collecting filter liquid, being concentrated into relative density through first is 1.12～1.15, obtains first extractum;
Step 2: get said first extractum after 3～5 ℃ of dialysis, collect to keep liquid, with the mixed solution of chloroform and n-butyl alcohol through sevage method deproteinization, collect water layer, it is 1.12～1.15 that warp second is concentrated into relative density, obtains second extractum;
Step 3: getting said second extractum, to add concentration be ethanol precipitate with ethanol 20～24h of 80～95%, and sediment is collected in centrifugal back, adds the entry stirring and dissolving, and being concentrated into relative density through the 3rd is 1.12～1.18, obtains the 3rd extractum, and filtering and collecting filter liquid promptly gets; In g/mL, said second extractum and alcoholic acid mass volume ratio are 1～3, and the mass volume ratio of said sediment and water is 1: 3～7.
2. method for distilling according to claim 1 is characterized in that, in the step 1, in g/mL, the mass volume ratio of said Herba Urticae Cannabinae and water is 1: 10～15.
3. method for distilling according to claim 1 is characterized in that the 22mm semipermeable membrane is selected in said dialysis for use.
4. method for distilling according to claim 1 is characterized in that, said first concentrate, second concentrate or the 3rd simmer down at 70～80 ℃, vacuum is to concentrate under the condition of 0.06MPa.
5. method for distilling according to claim 1 is characterized in that, the volume ratio of chloroform and n-butyl alcohol is 5: 1 in the said mixed solution.
6. method for distilling according to claim 1 is characterized in that, the volume ratio that keeps liquid and said mixed solution described in the step 2 is 1: 1.
7. method for distilling according to claim 1 is characterized in that, collect water layer described in the step 2 after, said second also comprise through the filtering step of 300 order filter clothes before concentrating.
8. method for distilling according to claim 1 is characterized in that, centrifugal described in the step 3 is centrifugal 15min under the condition of 3000rpm.
9. the Herba Urticae Cannabinae extract that the method for distilling that provides according to claim 1 to 8 obtains.
10. the application of Herba Urticae Cannabinae extract according to claim 9 in preparation treatment prostatitis, prostate hyperplasia, benign prostatic hyperplasia or hypertension drug.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105106520A (en) * | 2015-10-06 | 2015-12-02 | 常州亚当生物技术有限公司 | Healthcare product |
| CN108578446A (en) * | 2018-04-26 | 2018-09-28 | 太阳树（厦门）生物工程有限公司 | A kind of production method of low lead nettle extract |
| CN109700836A (en) * | 2019-03-05 | 2019-05-03 | 江西中医药大学 | A kind of anti-prostatic hyperplasia plateau nettle extract, preparation method and applications |
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2012
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105106520A (en) * | 2015-10-06 | 2015-12-02 | 常州亚当生物技术有限公司 | Healthcare product |
| CN108578446A (en) * | 2018-04-26 | 2018-09-28 | 太阳树（厦门）生物工程有限公司 | A kind of production method of low lead nettle extract |
| CN109700836A (en) * | 2019-03-05 | 2019-05-03 | 江西中医药大学 | A kind of anti-prostatic hyperplasia plateau nettle extract, preparation method and applications |
| CN109700836B (en) * | 2019-03-05 | 2021-08-24 | 江西中医药大学 | Plateau nettle extract for resisting prostatic hyperplasia as well as preparation method and application thereof |
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| CN102512463B (en) | 2014-04-16 |
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