CN106563115A - Herba leonuri biochemical mixture and preparation process - Google Patents

Herba leonuri biochemical mixture and preparation process Download PDF

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Publication number
CN106563115A
CN106563115A CN201610931581.XA CN201610931581A CN106563115A CN 106563115 A CN106563115 A CN 106563115A CN 201610931581 A CN201610931581 A CN 201610931581A CN 106563115 A CN106563115 A CN 106563115A
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parts
herba leonuri
water
mixture
preparation
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杨建平
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Mei Jialong Bio Tech Ltd Sichuan
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Mei Jialong Bio Tech Ltd Sichuan
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18Magnoliophyta (angiosperms)
    • A61K36/185Magnoliopsida (dicotyledons)
    • A61K36/53Lamiaceae or Labiatae (Mint family), e.g. thyme, rosemary or lavender
    • A61K36/533Leonurus (motherwort)
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18Magnoliophyta (angiosperms)
    • A61K36/185Magnoliopsida (dicotyledons)
    • A61K36/23Apiaceae or Umbelliferae (Carrot family), e.g. dill, chervil, coriander or cumin
    • A61K36/232Angelica
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18Magnoliophyta (angiosperms)
    • A61K36/185Magnoliopsida (dicotyledons)
    • A61K36/23Apiaceae or Umbelliferae (Carrot family), e.g. dill, chervil, coriander or cumin
    • A61K36/236Ligusticum (licorice-root)
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18Magnoliophyta (angiosperms)
    • A61K36/185Magnoliopsida (dicotyledons)
    • A61K36/48Fabaceae or Leguminosae (Pea or Legume family); Caesalpiniaceae; Mimosaceae; Papilionaceae
    • A61K36/484Glycyrrhiza (licorice)
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18Magnoliophyta (angiosperms)
    • A61K36/185Magnoliopsida (dicotyledons)
    • A61K36/73Rosaceae (Rose family), e.g. strawberry, chokeberry, blackberry, pear or firethorn
    • A61K36/736Prunus, e.g. plum, cherry, peach, apricot or almond
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18Magnoliophyta (angiosperms)
    • A61K36/88Liliopsida (monocotyledons)
    • A61K36/906Zingiberaceae (Ginger family)
    • A61K36/9068Zingiber, e.g. garden ginger
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/10Preparation or pretreatment of starting material
    • A61K2236/19Preparation or pretreatment of starting material involving fermentation using yeast, bacteria or both; enzymatic treatment
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/50Methods involving additional extraction steps
    • A61K2236/53Liquid-solid separation, e.g. centrifugation, sedimentation or crystallization

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  • Health & Medical Sciences (AREA)
  • Natural Medicines & Medicinal Plants (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Alternative & Traditional Medicine (AREA)
  • Biotechnology (AREA)
  • Botany (AREA)
  • Medical Informatics (AREA)
  • Medicinal Chemistry (AREA)
  • Microbiology (AREA)
  • Mycology (AREA)
  • Pharmacology & Pharmacy (AREA)
  • Epidemiology (AREA)
  • Animal Behavior & Ethology (AREA)
  • General Health & Medical Sciences (AREA)
  • Public Health (AREA)
  • Veterinary Medicine (AREA)
  • Medicines Containing Plant Substances (AREA)

Abstract

The invention relates to the field of medicines, and in particular relates to a herba leonuri biochemical mixture and a preparation process. The herba leonuri biochemical mixture is characterized by being prepared from the following raw materials in parts by weight: 475-485 parts of herba leonuri, 295-305 parts of radix angelica sinensis, 115-125 parts of rhizoma ligustici wallichii, 115-125 parts of peach kernels, 55-65 parts of baked ginger, 55-65 parts of honey-fried licorice root, and 50 million IU-150 million IU of cellulase. According to the herba leonuri biochemical mixture and the preparation process, the active ingredients can be easily leached out through decocting, the extracting effective ratio of the main ingredients is improved by 36% compared with that in the prior art, and thus the product quality and clinical application effect are greatly improved.

Description

A kind of Herba Leonuri biochemistry mixture and preparation technology
Technical field
The present invention relates to field of medicaments, more particularly to a kind of Herba Leonuri biochemistry mixture and preparation technology.
Background technology
Herba Leonuri biochemistry mixture has the effect of heat-clearing and toxic substances removing, antiphlogistic antibacterial, promoting blood flow to regulate menstruation, currently exists various benefits Female biochemistry mixture.
Herba Leonuri biochemistry mixture reduces the inflammation incidence rate of animal compared with injection antiinflammatory, reduces hyperpyrexia, puerperal and do not eat etc. three The incidence rate that connection is levied, while the output of lochia is much greater compared with injection.And need not have an injection, can save for raiser Make an appointment and manpower, while reduce animal stress, it is to avoid inflammatory tissue necrosis occurs.
Traditional decoction tazettine, i.e. Colchicine Herba Leonuri extract main component, content detection result 1.7%, Radix Glycyrrhizae Acid content 0.4%.Glycyrrhizic acid is topmost active component in Radix Glycyrrhizae.Glycyrrhizic acid and its series of products, to sarcoma, cancerous cell life Length has inhibitory action, and to the suppression ratio of acquired immune deficiency syndrome (AIDS) 90% is more up to, and has stronger increase immune function of human body effect.
For in the preparation of Herba Leonuri biochemistry mixture, precipitate with ethanol mode is usually directly added water to cook.But it is effective due to Chinese medicine Composition is often wrapped in plant cell wall, and using directly adding water to cook alcohol precipitating method, Chinese medicine has Chinese medicine extraction process Effect composition is wrapped up by cellulose, and cell wall is not destroyed in decoction process, and effective ingredient is difficult to be extracted, and extraction efficiency is low, is extracted When general temperature be 100 DEG C, effective ingredient is more easily damaged a part.
The content of the invention
In order to solve above technical problem, the present invention provides a kind of Herba Leonuri biochemistry mixture and preparation technology, and Herba Leonuri is biochemical to be closed Agent has blood circulation promoting and blood stasis dispelling, and promoting the flow of QI in the collateral by warming the meridian cures mainly prolonged lochia, abdominal pain due to blood stasis;Tazettine is decocted in Herba Leonuri biochemistry mixture to contain Amount 2.31%, glycyrrhizic acid content 0.54%, extraction efficiency improves 36%, and process is simple, easy to operate.
Solve a kind of Herba Leonuri biochemistry mixture in the present invention of above technical problem, it is characterised in that:The bonding agent is matched somebody with somebody Side includes the component of following weight portion:Herba Leonuri 475-485 parts, Radix Angelicae Sinensis 295-305 parts, Rhizoma Chuanxiong 115-125 parts, Semen Persicae 115- 125 parts, Rhizoma Zingiberis Preparatum 55-65 parts, Radix Glycyrrhizae Preparata 55-65 parts, the IU of cellulase 50,000,000-15,000 ten thousand, remaining is water.
Formula described in prioritization scheme includes the component of following weight portion:480 parts of the Herba Leonuri, 300 parts of Radix Angelicae Sinensis, Rhizoma Chuanxiong 120 parts, 120 parts of Semen Persicae, 60 parts of Rhizoma Zingiberis Preparatum, 60 parts of Radix Glycyrrhizae Preparata, the IU of cellulase 10,000,000, remaining is water.
It is more easy to extract using the Rhizoma Zingiberis Recens effective ingredient after processing, main component is more reliable.
The Herba Leonuri biochemistry mixture water content is 52-57%, and optimization water content is 55%.
In the present invention Herba Leonuri can all herbal medicine, effective ingredient be Herba Leonuri element, Herba Leonuri containing leonurine, stachydrine, Various alkaloids such as leonuridine, leonurinine and benzoic acid, potassium chloride etc..
Radix Angelicae Sinensis its roots can be used as medicine, and be one of the most frequently used Chinese medicine.With benefiting blood and regulating blood circulation, menstruction regulating and pain relieving is moisturize laxation, anti- The effect of cancer, anti-ageing anti-old, immunity.
Rhizoma Chuanxiong is the rhizome of samphire Rhizoma Chuanxiong, treats medicine first choice of headache.Menoxenia;Amenorrhea dysmenorrhea;Puerperal The stagnant raw meat pain of the stasis of blood;Abdominal mass lump;Pain in chest and hypochondrium;Dizziness of having a headache;Anemofrigid-damp arthralgia;Traumatic injury;Ulcer sores etc..
Rhizoma Zingiberis Preparatum for Rhizoma Zingiberiss Preparation process product, warming the meridian for stopping bleeding;Warming middle-JIAO to relieve pain.
Semen Persicae Chinese medicine name, is rosaceous plant Fructus Persicae Prunus persica (L.) Batsch or Prunus davidiana Prunus The dry mature seed of davidiana (Carr.) Franch..Harvest after fruit maturation, remove sarcocarp and nucleocapsid, take out seed, Dry.Generally cultivate all parts of the country.With blood circulation promoting and blood stasis dispelling, loosening bowel to relieve constipation, effect of relieving cough and asthma.
Radix Glycyrrhizae Preparata used is the Radix Glycyrrhizae for processing in the present invention, and Radix Glycyrrhizae Preparata (mostly Mel is processed), property of medicine partial temperature is partial to In invigorating the spleen and replenishing QI, cold expelling stomach function regulating.
A kind of preparation method of Herba Leonuri biochemistry mixture in the present invention, comprises the following steps:
(1) Radix Angelicae Sinensis, Rhizoma Chuanxiong, Rhizoma Zingiberiss, Semen Persicae are ground into into 10 times of 85% alcohol dippings of amount of coarse powder overnight, filtration, filtrate It is standby;
(2) add appropriate purified water in multi-function extractor, add cellulase to stir, by Herba Leonuri, Chinese medicine of licorice root Add purified water just to impregnate and be defined after coarse powder, be heated to 35-40 DEG C and be incubated 12 hours, Chinese crude drug is decocted after softening, every time 80 DEG C 1 hour is decocted, filtered, repeatedly for three times, collecting decoction, and mixing with the filtrate in step (1);
Temperature is very big to the influential effect of cellulase, so as to have influence on the effect of final products.
(3) negative pressure filtration is used, is concentrated about to 1:1 concentration, adds 3 times of ethanol to stand 24 hours, considers, and filtrate reclaims second Alcohol, is concentrated into the extractum of relative density 1.1-1.2;
(4) extractum is made into 1:14 mixture.
Negative pressure filtration is more in hgher efficiency than traditional centrifugal filtration in the present invention, filters clarity more preferable.
Granular size is 10 mesh after the raw material of Chinese medicine coarse powder.
The negative pressure is -10Pa.
Ethanol, heating recovery ethanol are reclaimed under the negative pressure, heating-up temperature is 80 DEG C.
The water added toward extraction pot for the first time in the step (1) is the 30% of Chinese medicine weight.
The water is purified water.
Using after the technique for adding cellulase in the present invention, energy centering crude drug cell wall has decomposition, effective ingredient Leaching is easily decocted, main component extracts effective percentage and improves 36% than tradition, this energy large increase product quality and clinic make Use effect.
Herba Leonuri biochemistry mixture has blood circulation promoting and blood stasis dispelling in the present invention, and promoting the flow of QI in the collateral by warming the meridian cures mainly prolonged lochia, abdominal pain due to blood stasis Deng.Apply in animals such as cattle, horse, pig, sheep.It is mainly used in treating and preventing puerperal infection etc..Horse, cattle 200-300ml/ heads, sheep, Pig 25-30ml/ heads.
Specific embodiment
Below with specific embodiment come to the technical scheme further instruction in the present invention.
Experiment equipment used in following examples:Multi-function extractor (extraction pot, negative pressure filter, medicinal liquid temporary storage jar, wine Smart temporary storage jar), test tube, filter paper, neutral alumina column (100-120 mesh), chromatography cylinder, electronic balance, volumetric flask, ultra-violet lamp, Hair dryer, silica GF254 lamellae;
Experiment reagent:N-butyl alcohol, hydrochloric acid, ethanol, stachydrine hydrochloride reference substance, glycyrrhizic acid reference substance, potassium iodide, butanone, Formic acid, aluminum chloride, are all purchase on market.
Embodiment 1
Chemical combination agent prescription includes the component of following weight portion:475 parts of Herba Leonuri, 295 parts of Radix Angelicae Sinensis, 115 parts of Rhizoma Chuanxiong, Semen Persicae 115 parts, 55 parts of Rhizoma Zingiberis Preparatum, 55 parts of Radix Glycyrrhizae Preparata, the IU of cellulase 50,000,000, remaining is water, and Herba Leonuri biochemistry mixture water content is 55%, Water is purified water.
Concrete preparation method such as following steps:
(1) Radix Angelicae Sinensis, Rhizoma Chuanxiong, Rhizoma Zingiberiss, Semen Persicae are ground into into 10 times of 85% alcohol dippings of amount of coarse powder overnight, filtration, filtrate It is standby.
(2) add appropriate purified water in multi-function extractor, add cellulase to stir, by Herba Leonuri, Chinese medicine of licorice root Add purified water just to impregnate and be defined after coarse powder, be heated to 35 DEG C and be incubated 12 hours, Chinese crude drug decocts three times after softening, every time 80 DEG C decoct 1 hour, filter, collecting decoction;Decocting liquid mixes again with the filtrate in step (1);Granule is big after raw material of Chinese medicine coarse powder Little is 10 mesh.
(3) negative pressure filtration is used, is concentrated about to 1:1 concentration, adds 3 times of ethanol to stand 24 hours, considers, and filtrate reclaims second Alcohol, is concentrated into the extractum of relative density 1.1;Negative pressure is -10Pa.80 DEG C of recovery condensing units are heated under negative pressure condition and reclaim second Alcohol;
(4) extractum is made into 1:14 mixture.
Embodiment 2
Chemical combination agent prescription includes the component of following weight portion:485 parts of Herba Leonuri, 305 parts of Radix Angelicae Sinensis, 125 parts of Rhizoma Chuanxiong, Semen Persicae 125 parts, 65 parts of Rhizoma Zingiberis Preparatum, 65 parts of Radix Glycyrrhizae Preparata, the IU of cellulase 150,000,000, remaining is water, and Herba Leonuri biochemistry mixture water content is 52%, water is purified water.
Concrete preparation method such as following steps:
(1) Radix Angelicae Sinensis, Rhizoma Chuanxiong, Rhizoma Zingiberiss, Semen Persicae are ground into into 10 times of 85% alcohol dippings of amount of coarse powder overnight, filtration, filtrate It is standby.
(2) add appropriate purified water in multi-function extractor, add cellulase to stir, by Herba Leonuri, Chinese medicine of licorice root Add purified water just to impregnate and be defined after coarse powder, be heated to 40 DEG C and be incubated 12 hours, Chinese crude drug decocts three times after softening, every time 80 DEG C decoct 1 hour, filter, collecting decoction;Decocting liquid mixes again with the filtrate in step (1);Granule is big after raw material of Chinese medicine coarse powder Little is 10 mesh.
(3) negative pressure filtration is used, is concentrated about to 1:1 concentration, adds 3 times of ethanol to stand 24 hours, considers, and filtrate reclaims second Alcohol, is concentrated into the extractum of relative density 1.2;Negative pressure is -10Pa.80 DEG C of recovery condensing units are heated under negative pressure condition and reclaim second Alcohol;
(4) extractum is made into 1:14 mixture.
Embodiment 3
Chemical combination agent prescription includes the component of following weight portion:
480 parts of Herba Leonuri, 300 parts of Radix Angelicae Sinensis, 120 parts of Rhizoma Chuanxiong, 120 parts of Semen Persicae, 60 parts of Rhizoma Zingiberis Preparatum, 60 parts of Radix Glycyrrhizae (processing), fiber The IU of plain enzyme 100,000,000, remaining is water, and Herba Leonuri biochemistry mixture water content is 57%, and water is purified water.
Concrete preparation method such as following steps:
(1) Radix Angelicae Sinensis, Rhizoma Chuanxiong, Rhizoma Zingiberiss, Semen Persicae are ground into into 10 times of 85% alcohol dippings of amount of coarse powder overnight, filtration, filtrate It is standby.
(2) add appropriate purified water in multi-function extractor, add cellulase to stir, by Herba Leonuri, Chinese medicine of licorice root Add purified water just to impregnate and be defined after coarse powder, be heated to 38 DEG C and be incubated 12 hours, Chinese crude drug decocts three times after softening, every time 80 DEG C decoct 1 hour, filter, collecting decoction;Decocting liquid mixes again with the filtrate in step (1);Granule is big after raw material of Chinese medicine coarse powder Little is 10 mesh.
(3) negative pressure filtration is used, is concentrated about to 1:1 concentration, adds 3 times of ethanol to stand 24 hours, considers, and filtrate reclaims second Alcohol, is concentrated into the extractum of relative density 1.2;Negative pressure is -10Pa.80 DEG C of recovery condensing units are heated under negative pressure condition and reclaim second Alcohol;
(4) extractum is made into 1:14 mixture.
Embodiment 4
Content in preparation method such as embodiment 1, chemical combination agent prescription includes the component of following weight portion:
478 parts of Herba Leonuri, 298 parts of Radix Angelicae Sinensis, 118 parts of Rhizoma Chuanxiong, 118 parts of Semen Persicae, 58 parts of Rhizoma Zingiberis Preparatum, 58 parts of Radix Glycyrrhizae Preparata, cellulose The IU of enzyme 120,000,000, remaining is water, and Herba Leonuri biochemistry mixture water content is 56%, and water is purified water.
Embodiment 5
Content in preparation method such as embodiment 1, chemical combination agent prescription includes the component of following weight portion:
482 parts of Herba Leonuri, 302 parts of Radix Angelicae Sinensis, 122 parts of Rhizoma Chuanxiong, 122 parts of Semen Persicae, 62 parts of Rhizoma Zingiberis Preparatum, 62 parts of Radix Glycyrrhizae Preparata, cellulose The IU of enzyme 80,000,000, remaining is water, and Herba Leonuri biochemistry mixture water content is 54%, and water is purified water.
Embodiment 6
Content in preparation method such as embodiment 1, chemical combination agent prescription includes the component of following weight portion:
480 parts of Herba Leonuri, 300 parts of Radix Angelicae Sinensis, 120 parts of Rhizoma Chuanxiong, 120 parts of Semen Persicae, 60 parts of Rhizoma Zingiberis Preparatum, 60 parts of Radix Glycyrrhizae Preparata, cellulose The IU of enzyme 60,000,000, remaining is water, and Herba Leonuri biochemistry mixture water content is 53%, and water is purified water.
Embodiment 7
Content in preparation method such as embodiment 1, chemical combination agent prescription includes the component of following weight portion:
484 parts of Herba Leonuri, 304 parts of Radix Angelicae Sinensis, 124 parts of Rhizoma Chuanxiong, 116 parts of Semen Persicae, 59 parts of Rhizoma Zingiberis Preparatum, 64 parts of Radix Glycyrrhizae Preparata, cellulose The IU of enzyme 140,000,000, remaining is water.
Test one
If experimental group 1,2 and 3, the initial feature of the pig in experiment is the same, experimental group 1 is the traditional Herba Leonuri biochemistry mixture of feeding (mother and sons' peace (Herba Leonuri biochemistry mixture), the effective company of Hefei strength animal drug), experimental group 2 is the Herba Leonuri life in the feeding present invention Bonding agent, experiment 3 is blank group.
Concrete consumption and result such as table 1 below:
Table 1
As can be seen from the above table, the chemical combination that the effect of the Herba Leonuri biochemistry mixture in the present invention is far longer than in tradition is fed Agent, and do not feed the situation of bonding agent.Because Chinese medicine extraction process is adopted and directly adds water to cook alcohol precipitating method, Chinese medicine Effective ingredient is wrapped up by cellulose, and effective ingredient is difficult to be extracted in decoction process, and extraction efficiency is low, and general temperature is during extraction 100 DEG C, effective ingredient is more easily damaged a part.Middle the effective elements of the medicine in the present invention is often wrapped in plant cell wall In, traditional handicraft is directly decocted, and cell wall is not destroyed, and traditional Chinese medicine extyaction recovery rate is relatively low;Using addition cellulase Technique after, can centering crude drug cell wall have a decomposition, effective ingredient is easily decocted and leached, in the case of negative pressure is decocted, Temperature is lower, and effective ingredient is not easily susceptible to destruction.
Test two
According to the content in test one above, pan-fried tazettine in experiment 1 and the present invention and glycyrrhizic acid are measured respectively:
Testing result:Traditional 01112 testing result 1.7%, glycyrrhizic acid content 0.4%;Tazettine is decocted after modified technique Content 2.31%, glycyrrhizic acid content 0.54%, extraction efficiency improves 36%.
Above testing result is the data measured with the method for inspection of efficient liquid phase,
Wherein Colchicine Content determination step is as follows:
1st, instrument and reagent
Shimadzu LC-16 high performance liquid chromatograph (LC-16 liquid chromatography pumps, CTO-16 column ovens, DGU-20A5R degassers, SPD-16 UV-visible detectors, LabSolutions Essentia-Lite chromatographic work stations), Colchicine control in examine Institute, methanol chromatographically pure, water are distilled water.
2 continuous modes
Chromatographic condition and system suitability:It is filler with octyl silane group silica gel;With methanol-water (40: 60) it is mobile phase;Column temperature:25℃;Detection wavelength is 254mn.Number of theoretical plate is calculated by Colchicine peak and is not less than 5000, autumn waters -- limid eyes Celestial alkali should meet the requirements with the separating degree of adjacent chromatographic peak.
It is prepared by reference substance solution:Colchicine reference substance is taken, it is accurately weighed, it is dissolved in water and quantitatively every lml is made in dilution In solution containing about 10ug, as reference substance solution.
It is prepared by sample solution:Precision is weighed and (is approximately equivalent to Colchicine lmg) in right amount, in putting 100ml measuring bottles, is added water suitable Amount, ultrasonic 15min Colchicine dissolving, is diluted with water to scale, shakes up, and filters, and takes subsequent filtrate as need testing solution.
Determine
Start shooting by Shimadzu LC-16 high performance liquid chromatograph rule of operation, adjust temperature and flow, reach analysis condition and base After line is steady, respectively precision measures (or auto injection) need testing solution and each 10ul of reference substance solution injects chromatograph of liquid, Record chromatogram.Content is calculated by external standard method, is obtained final product.
As a result calculate
The Colchicine Content (w) represented with mass percent:
In formula:CRThe concentration of-reference substance, mg/ml;
AXThe peak area of-sample;
ARThe peak area of-reference substance;
N-diluted sample multiple;
The quality of m-sample, mg.
Wherein, glycyrrhizic acid content is determined as follows:
1 instrument and reagent
Shimadzu LC-16 high performance liquid chromatograph (LC-16 liquid chromatography pumps, CTO-16 column ovens, DGU-20A5R degassers, SPD-16 UV-visible detectors, LabSolutions Essentia-Lite chromatographic work stations), Colchicine control in examine It is pure that institute, methanol chromatographically pure, water are distilled water, ammonium acetate analyzes the analysis of pure and mild glacial acetic acid.
2 continuous modes
Chromatographic condition and system suitability:With octadecylsilane chemically bonded silica as filler;Methanol -0.2mol/L Spirit of Mindererus .-glacial acetic acid (67: 33: 1) is mobile phase;Detection wavelength is 250nm.Number of theoretical plate presses the calculating of glycyrrhizic acid peak should not Less than 2000.
It is prepared by reference substance solution:Extracting liquorice acid mono-ammonium reference substance 10mg, it is accurately weighed, in putting 50ml measuring bottles, with flowing Phase 45ml, supersound process makes to dissolve and be diluted to scale, shakes up, obtain final product (per the 1ml 0.2mg of reference substance containing monoammonium glycyrrhizinate, folding Conjunction glycyrrhizic acid is 0.1959mg).
It is prepared by sample solution:Accurately weighed this product is appropriate, in being placed in 50ml measuring bottles, plus the 45ml that makes an appointment that flows, supersound process (power 250W, frequency 20kHz) 30 minutes, takes out, and lets cool, plus mobile phase is to scale, shakes up, and filtration, precision takes subsequent filtrate 10ml, in putting 25ml measuring bottles, plus mobile phase is diluted to scale, shakes up, and obtains final product.
Determine
Start shooting by Shimadzu LC-16 high performance liquid chromatograph rule of operation, adjust temperature and flow, reach analysis condition and base After line is steady, respectively precision measures (or auto injection) need testing solution and each 10ul of reference substance solution injects chromatograph of liquid,
Record chromatogram.Content is calculated by external standard method, is obtained final product.
Fruit calculates
State;;;Neither dead nor alive glycyrrhizic acid content (w):
In formula:CRThe concentration of-reference substance, mg/ml;
AXThe peak area of-sample;
ARThe peak area of-reference substance;
N-diluted sample multiple;
The quality of m-sample, mg.
More than it is known that the decoction narcissus alkali content of the Herba Leonuri raw compounds in the present invention and glycyrrhizic acid content are high, It is stable.
Presently preferred embodiments of the present invention is the foregoing is only, not to limit the present invention, all essences in the present invention Any modification, equivalent and improvement made within god and principle etc., should be included within the scope of the present invention.

Claims (9)

1. a kind of Herba Leonuri biochemistry mixture, it is characterised in that:The chemical combination agent prescription includes the component of following weight portion:Herba Leonuri 475-485 parts, Radix Angelicae Sinensis 295-305 parts, Rhizoma Chuanxiong 115-125 parts, Semen Persicae 115-125 parts, Rhizoma Zingiberis Preparatum 55-65 parts, Radix Glycyrrhizae Preparata 55-65 Part, the IU-15000IU of cellulase 50,000,000, remaining is water.
2. a kind of Herba Leonuri biochemistry mixture according to claim 1, it is characterised in that:The formula includes following weight portion Component:480 parts of the Herba Leonuri, 300 parts of Radix Angelicae Sinensis, 120 parts of Rhizoma Chuanxiong, 120 parts of Semen Persicae, 60 parts of Rhizoma Zingiberis Preparatum, 60 parts of Radix Glycyrrhizae Preparata, cellulose Enzyme 1000IU, remaining is water.
3. a kind of Herba Leonuri biochemistry mixture according to claim 1 and 2, it is characterised in that:The Herba Leonuri biochemistry mixture is aqueous Measure as 52-57%, optimization water content is 55%.
4. the preparation method of a kind of Herba Leonuri biochemistry mixture according to claim 1, it is characterised in that:Comprise the following steps:
(1) Radix Angelicae Sinensis, Rhizoma Chuanxiong, Rhizoma Zingiberis Preparatum, Semen Persicae are ground into into 10 times of 85% alcohol dippings of amount of coarse powder overnight, are filtered, filtrate is standby;
(2) add water in extraction pot, add cellulase and stir, just soak water is added after Herba Leonuri, Radix Glycyrrhizae Preparata coarse powder Stain is defined, and is heated to 35-40 DEG C and is incubated 12 hours, and Chinese crude drug is decocted after softening, and every time 80 DEG C of decoctions, 1 hour, filters, repeatedly Three times, collecting decoction, and mix with the filtrate in step (1);
(3) negative pressure filtration is used, the mass concentration ratio for being concentrated into medicine and water is 1:1 concentration, adds 3 times of ethanol to stand 24 hours, Filter, filtrate recycling ethanol is concentrated into the extractum of relative density 1.1-1.2;
(4) it is 1 extractum to be made into Chinese crude drug and water quality ratio:14 mixture;
(5) packaging, transport or storage.
5. the preparation method of a kind of Herba Leonuri biochemistry mixture according to claim 4, it is characterised in that:The step (1) and Granular size is 10 mesh after coarse powder in step (2).
6. the preparation method of a kind of Herba Leonuri biochemistry mixture according to claim 4, it is characterised in that:The negative pressure for- 10Pa。
7. a kind of preparation method of the biochemical mixture of Herba Leonuri according to claim 4 or 6, it is characterised in that:Under the negative pressure Ethanol, heating recovery ethanol are reclaimed, heating-up temperature is 80 DEG C.
8. the preparation method of a kind of Herba Leonuri biochemistry mixture according to claim 4, it is characterised in that:In the step (1) The water for adding toward extraction pot for the first time is the 30% of Chinese medicine weight.
9. a kind of preparation method of the biochemical mixture of Herba Leonuri according to claim 4 or 8, it is characterised in that:The water is pure Change water.
CN201610931581.XA 2016-10-31 2016-10-31 Herba leonuri biochemical mixture and preparation process Pending CN106563115A (en)

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