CN109045088A - A method of Radix Angelicae Sinensis effective component is extracted using diacolation technology - Google Patents

A method of Radix Angelicae Sinensis effective component is extracted using diacolation technology Download PDF

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CN109045088A
CN109045088A CN201811190770.1A CN201811190770A CN109045088A CN 109045088 A CN109045088 A CN 109045088A CN 201811190770 A CN201811190770 A CN 201811190770A CN 109045088 A CN109045088 A CN 109045088A
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medicinal material
diacolation
percolate
solution
radix angelicae
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赵磊
李冲
杨蕊菁
夏鹏飞
李娟�
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Gansu University of Chinese Medicine
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    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18—Magnoliophyta (angiosperms)
    • A61K36/185—Magnoliopsida (dicotyledons)
    • A61K36/23—Apiaceae or Umbelliferae (Carrot family), e.g. dill, chervil, coriander or cumin
    • A61K36/232—Angelica
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00—Isolation 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
    • A61K2236/10—Preparation or pretreatment of starting material
    • A61K2236/15—Preparation or pretreatment of starting material involving mechanical treatment, e.g. chopping up, cutting or grinding
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00—Isolation 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
    • A61K2236/30—Extraction of the material
    • A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
    • A61K2236/333—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using mixed solvents, e.g. 70% EtOH
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00—Isolation 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
    • A61K2236/30—Extraction of the material
    • A61K2236/39—Complex extraction schemes, e.g. fractionation or repeated extraction steps
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00—Isolation 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
    • A61K2236/50—Methods involving additional extraction steps
    • A61K2236/51—Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying

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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 discloses a kind of methods for extracting Radix Angelicae Sinensis effective component using diacolation technology, belong to active ingredients from traditional Chinese medicinal extractive technique field, and step includes: to crush immersion, a diacolation, secondary diacolation, three times diacolation and collection percolate.Front portion is contained the next step preparation that the more percolate of medicinal material effective component is first used for drug by the present invention, rear portion contains Extraction solvent of the less percolate of medicinal material effective component for second percolator Chinese medicine and is recycled, the percolate more containing medicinal material effective component first collected in second percolator is continued on for drug again to prepare in next step, rear portion percolate is used for the Extraction solvent of third percolator Chinese medicine, so circulation, while guaranteeing that medicinal material effective component extracts complete as far as possible, greatly utilize Extraction solvent, increase the utilization rate of solvent, reduce the dosage of Extraction solvent, the cost of Radix Angelicae Sinensis industrialized production is greatly saved.

Description

A method of Radix Angelicae Sinensis effective component is extracted using diacolation technology
Technical field
The invention belongs to active ingredients from traditional Chinese medicinal extractive technique fields, and in particular to a kind of to extract Radix Angelicae Sinensis using diacolation technology The method of effective component.
Background technique
When being classified as umbelliferae angelicaAngelica sinensis(Oliv.) dry root of Diels.With benefit The effect of blood promoting blood circulation, regulating menstruation and relieving pain, moistening intestines and relaxing bowels, it is used for blood deficiency chlorosis, dizziness palpitaition, irregular menstruation, amenorrhea and algomenorrhea etc..Investigation It learns, commercially available thick water circulation, danggui extract, danggui liujin gao etc. are all made of percolation extraction.Compared with cold-maceration, percolation is cold-maceration Development, that is, remain cold-maceration extract when be not required to heat, retain heat-sensitive ingredients and the volatilization of its extract to greatest extent Property ingredient the advantages of, and biggish concentration gradient can be kept at any time, increase its extraction efficiency, and also have equipment simple and behaviour Make convenient advantage.But traditional percolation, there is also required post processing extraction solvent consumption is big, Extraction solvent utilization rate is low to be lacked Point.
Summary of the invention
The object of the present invention is to provide a kind of methods for extracting Radix Angelicae Sinensis effective component using diacolation technology, to solve existing work as Return extracting method solvent usage amount big, the high problem of extraction cost.
In order to achieve the above object, the technical solution adopted by the present invention are as follows:
A method of Radix Angelicae Sinensis effective component is extracted using diacolation technology, is included the following steps:
Step 1:
It is averagely put into Radix Angelicae Sinensis pulverizing medicinal materials to 10-30 mesh in three percolators, organic solvent is added and impregnates；
Step 2: a diacolation:
The organic solvent that 12-14 times of medicinal material amount is added into first percolator carries out diacolation, first collects the infiltration of 3-5 times of medicinal material amount Liquid of filtering is solution A, continues to collect the percolate of 7-9 times of medicinal material amount to be solution B；
Step 3: secondary diacolation:
Second percolator is added in the solution B that step 2 is obtained, and the organic solvent that 3-5 times of medicinal material amount is added simultaneously is seeped It filters, the percolate for first collecting 4-6 times of medicinal material amount is solution C, continues to collect the percolate of 6-8 times of medicinal material amount to be solution D；
Step 4: diacolation three times
The solution D that step 3 is obtained is added in third percolator, and the organic solvent that 4-6 times of medicinal material amount is added simultaneously carries out Diacolation, the percolate for collecting 10-12 times of medicinal material amount altogether is solution E；
Step 5: collecting percolate:
By Step 2: three, four obtained solution A, C and E merge, drying obtains medicinal extract, measures yield of extract.
Step 2: the speed of diacolation described in three, four is 1-6 mL/kg/min.
Step 1 to organic solvent described in four is 60-80% ethanol solution.
The additional amount of organic solvent described in step 1 is 1-2 times of medicinal material weight.
Organic solvent soaking time described in step 1 is 1-4h.
The present invention having the beneficial effect that compared to the prior art
Front portion is contained the next step preparation that the more percolate of medicinal material effective component is first used for drug, latter portion by the present invention Extraction solvent point containing the less percolate of medicinal material effective component for second percolator Chinese medicine is recycled, then by the The percolate more containing medicinal material effective component first collected in two percolators continues on for drug and prepares in next step, latter portion The Extraction solvent for dividing percolate to be used for third percolator Chinese medicine so recycles, and mentions as far as possible in guarantee medicinal material effective component While taking complete, Extraction solvent is greatly utilized, increases the utilization rate of solvent, reduces the dosage of Extraction solvent, The cost of Radix Angelicae Sinensis industrialized production is greatly saved.
Compared with the method for traditional seepage pressure effects Radix Angelicae Sinensis medicinal material, about 2/ can be saved by extracting Radix Angelicae Sinensis medicinal material using this method 5 Extraction solvent；
Compared with the method for traditional seepage pressure effects Radix Angelicae Sinensis medicinal material, about 1/3 can be saved by extracting Radix Angelicae Sinensis medicinal material using this method Extraction time；
Using this method, shortening extraction time, on the basis of reducing post processing extraction solvent consumption, extraction efficiency and traditional seepage pressure effects Method is identical.
Specific embodiment
The present invention will be further described With reference to embodiment.
A method of Radix Angelicae Sinensis effective component is extracted using diacolation technology, is included the following steps:
Step 1:
It is averagely put into Radix Angelicae Sinensis pulverizing medicinal materials to 10-30 mesh in three percolators, organic solvent is added and impregnates；Since Radix Angelicae Sinensis is drunk The price of piece is higher than Radix Angelicae Sinensis crude drug price, when Radix Angelicae Sinensis is extracted in pharmaceutical factory, if will increase production cost using angelica sinensis, but if Using complete Radix Angelicae Sinensis medicinal material, then needing to impregnate for a long time could infiltrate Radix Angelicae Sinensis completely, will necessarily increase indirectly pharmaceutical factory at This, therefore Radix Angelicae Sinensis medicinal material needs to crush.When grinding medicinal materials, maximum medicine sieve is that the medicine of 10 mesh sieves, so Radix Angelicae Sinensis medicinal material is maximum For 10 mesh；Less than diacolation after the Radix Angelicae Sinensis medicinal material immersion of 30 mesh, since granularity is too small, Extraction solvent is difficult to flow down, therefore selects The Radix Angelicae Sinensis medicinal material of -30 mesh of 10 mesh.
Step 2: a diacolation:
The organic solvent that 12-14 times of medicinal material amount is added into first percolator carries out diacolation, first collects the infiltration of 3-5 times of medicinal material amount Liquid of filtering is solution A, continues to collect the percolate of 7-9 times of medicinal material amount to be solution B；
Step 3: secondary diacolation:
Second percolator is added in the solution B that step 2 is obtained, and the organic solvent that 3-5 times of medicinal material amount is added simultaneously is seeped It filters, the percolate for first collecting 4-6 times of medicinal material amount is solution C, continues to collect the percolate of 6-8 times of medicinal material amount to be solution D；
Step 4: diacolation three times
The solution D that step 3 is obtained is added in third percolator, and the organic solvent that 4-6 times of medicinal material amount is added simultaneously carries out Diacolation, the percolate for collecting 10-12 times of medicinal material amount altogether is solution E；
Step 5: collecting percolate:
By Step 2: three, four obtained solution A, C and E merge, drying obtains medicinal extract, measures yield of extract.
Step 2: the speed of diacolation described in three, four is 1-6 mL/kg/min.
Step 1 to organic solvent described in four is 60-80% ethanol solution.
The additional amount of organic solvent described in step 1 is 1-2 times of medicinal material weight.
Organic solvent soaking time described in step 1 is 1-4h.When the Radix Angelicae Sinensis medicinal material of -30 mesh of 10 mesh of seepage pressure effects, medicinal material It impregnates 1-4h and impregnates 12h or more, the seepage pressure effects time is identical, therefore we select to start diacolation after impregnating 1-4h, in this way The time of Radix Angelicae Sinensis seepage pressure effects can greatly be shortened.
Embodiment 1:
The accurate Radix Angelicae Sinensis medicinal material 150.105g for weighing 10-30 mesh in first percolator, is soaked using the ethanol solution of 225mL70% 3h is steeped, 70% ethanol solution using 1800mL is Extraction solvent, with the flow velocity diacolation of 4 mL/kg/min, first collects 4.3 times of medicines The percolate of material amount, that is, 650mL percolate is denoted as solution A1, be further continued for collect 7.3 times of percolates i.e. 1100mL percolate be denoted as it is molten Liquid B1；
The accurate Radix Angelicae Sinensis medicinal material 150.083g for weighing -30 mesh of 10 mesh, uses the ethanol solution of 225mL70% in second percolator 3h is impregnated, solution B is used1The ethanol solution 700mL of 1100mL and 70% is seeped as Extraction solvent with the flow velocity of 4 mL/kg/min It filters, the percolate, that is, 800mL percolate for first collecting 5.3 times of medicinal material amounts is denoted as solution A2, it is further continued for collecting 6 times of percolates i.e. 900mL percolate is denoted as solution B2；
The accurate Radix Angelicae Sinensis medicinal material 150.004g for weighing 10-30 mesh in third percolator, is soaked using the ethanol solution of 225mL70% 3h is steeped, solution B is used2The ethanol solution 800mL of 900mL and 70% is as Extraction solvent, with the flow velocity diacolation of 4 mL/kg/min, The i.e. 1700mL percolate of percolate for collecting 11.3 times of medicinal material amounts is denoted as solution A3；
Merge solution A1、A2And A3, the method for medicinal extract constant weight is dried to the progress of this part percolate yield of extract using 105 DEG C Measurement, the yield of extract for obtaining this part percolate is 0.51g/g.
Embodiment 2:
The accurate Radix Angelicae Sinensis medicinal material 150.008g for weighing 20-30 mesh in first percolator, is soaked using the ethanol solution of 300mL60% 1h is steeped, 60% ethanol solution using 1800mL is Extraction solvent, with the flow velocity diacolation of 1 mL/kg/min, first collects 3 times of medicinal materials The percolate of amount, that is, 450mL percolate is denoted as solution A1, it is further continued for 9 times of i.e. 1350mL percolates of percolate of collection and is denoted as solution B1；
The accurate Radix Angelicae Sinensis medicinal material 150.083g for weighing 20-30 mesh in second percolator, is soaked using the ethanol solution of 300mL60% 1h is steeped, solution B is used1The ethanol solution 450mL of 1350mL and 60% is as Extraction solvent, with 1mL/(minkg) flow velocity seep It filters, the percolate, that is, 600mL percolate for first collecting 4 times of medicinal material amounts is denoted as solution A2, it is further continued for collecting 8 times of i.e. 1200mL of percolate Percolate is denoted as solution B2；
The accurate Radix Angelicae Sinensis medicinal material 150.041g for weighing 20-30 mesh in third percolator, is soaked using the ethanol solution of 300mL60% 1h is steeped, solution B is used2The ethanol solution 600mL of 1200mL and 60% is seeped as Extraction solvent with the flow velocity of 1 mL/kg/min It filters, the i.e. 1800mL percolate of percolate for collecting 12 times of medicinal material amounts is denoted as solution A3；
Merge solution A1、A2And A3, the method for medicinal extract constant weight is dried to the progress of this part percolate yield of extract using 105 DEG C Measurement, the yield of extract for obtaining this part percolate is 0.47g/g.
Embodiment 3:
The accurate Radix Angelicae Sinensis medicinal material 150.039g for weighing 10-20 mesh in first percolator, is soaked using the ethanol solution of 150mL80% 4h is steeped, 80% ethanol solution using 2100mL is Extraction solvent, with the flow velocity diacolation of 6 mL/kg/min, first collects 5 times of medicinal materials The percolate of amount, that is, 750mL percolate is denoted as solution A1, it is further continued for 9 times of i.e. 1350mL percolates of percolate of collection and is denoted as solution B1；
The accurate Radix Angelicae Sinensis medicinal material 150.153g for weighing 10-20 mesh in second percolator, is soaked using the ethanol solution of 150mL80% 4h is steeped, solution B is used1The ethanol solution 750mL of 1350mL and 80% is seeped as Extraction solvent with the flow velocity of 6 mL/kg/min It filters, the percolate, that is, 900mL percolate for first collecting 6 times of medicinal material amounts is denoted as solution A2, it is further continued for collecting 8 times of i.e. 1200mL of percolate Percolate is denoted as solution B2；
The accurate Radix Angelicae Sinensis medicinal material 150.002g for weighing 10-20 mesh in third percolator, is soaked using the ethanol solution of 150mL80% 4h is steeped, solution B is used2The ethanol solution 900mL of 1200mL and 80% is seeped as Extraction solvent with the flow velocity of 6 mL/kg/min It filters, the percolate, that is, 2100mL percolate for first collecting 14 times of medicinal material amounts is denoted as solution A3；
Merge solution A1、A2And A3, the method for medicinal extract constant weight is dried to the progress of this part percolate yield of extract using 105 DEG C Measurement, the yield of extract for obtaining this part percolate is 0.49g/g.
Embodiment is summarized:
This batch of test medicinal material is measured into its extract using Radix Angelicae Sinensis alcohol-soluble determination of extractives method in 2015 editions " Chinese Pharmacopoeia ", Obtaining its yield of extract is 0.49g/g, by the experimental result of this method it is found that being mentioned using this method seepage pressure effects Radix Angelicae Sinensis medicinal material Take rate identical as official method, in the case where guaranteeing that its recovery rate is constant, this method can not be heated medicinal material, protect its heat Quick ingredient and volatile component.By Experimental comparison it is found that traditional permeating extraction extract Radix Angelicae Sinensis need 11 times of medicinal material amounts with On Extraction solvent, the extraction time of 40h or so.Same a collection of Radix Angelicae Sinensis medicinal material is extracted using this method, it is only necessary to 8 times of medicinal material amounts The Extraction solvent of left and right, the extraction time of 25h or so, the Radix Angelicae Sinensis medicinal material medicinal extract amount that two kinds of diacolation methods obtain is identical, Ke Yi While guaranteeing extraction efficiency, a large amount of Extraction solvents and extraction time are saved, greatly saves the production cost in pharmaceutical factory.

Claims (5)

1. a kind of method for extracting Radix Angelicae Sinensis effective component using diacolation technology, it is characterised in that include the following steps:
It is impregnated Step 1: crushing:
It is averagely put into Radix Angelicae Sinensis pulverizing medicinal materials to 10-30 mesh in three percolators, organic solvent is added and impregnates；
Step 2: a diacolation:
The organic solvent that 12-14 times of medicinal material amount is added into first percolator carries out diacolation, first collects the infiltration of 3-5 times of medicinal material amount Liquid of filtering is solution A, continues to collect the percolate of 7-9 times of medicinal material amount to be solution B；
Step 3: secondary diacolation:
Second percolator is added in the solution B that step 2 is obtained, and the organic solvent that 3-5 times of medicinal material amount is added simultaneously is seeped It filters, the percolate for first collecting 4-6 times of medicinal material amount is solution C, continues to collect the percolate of 6-8 times of medicinal material amount to be solution D；
Step 4: diacolation three times:
The solution D that step 3 is obtained is added in third percolator, and the organic solvent that 4-6 times of medicinal material amount is added simultaneously carries out Diacolation, the percolate for collecting 10-14 times of medicinal material amount altogether is solution E；
Step 5: collecting percolate:
By Step 2: three, four obtained solution A, C and E merge, drying obtains medicinal extract, measures yield of extract.
2. the method for extracting Radix Angelicae Sinensis effective component using diacolation technology as described in claim 1, it is characterised in that: Step 2: Three, the speed of diacolation described in four is 1-6mL/kg/min.
3. the method for extracting Radix Angelicae Sinensis effective component using diacolation technology as claimed in claim 1 or 2, it is characterised in that: step Organic solvent described in one to four is 60-80% ethanol solution.
4. the method for extracting Radix Angelicae Sinensis effective component using diacolation technology as claimed in claim 3, it is characterised in that: in step 1 The additional amount of the organic solvent is 1-2 times of medicinal material weight.
5. the method for extracting Radix Angelicae Sinensis effective component using diacolation technology as claimed in claim 4, it is characterised in that: in step 1 The organic solvent soaking time is 1-4h.
CN201811190770.1A 2018-10-12 2018-10-12 A method of Radix Angelicae Sinensis effective component is extracted using diacolation technology Pending CN109045088A (en)

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CN111804004A (en) * 2020-08-03 2020-10-23 于瀛 Extraction and leaching method of traditional Chinese medicine

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111804004A (en) * 2020-08-03 2020-10-23 于瀛 Extraction and leaching method of traditional Chinese medicine
CN111804004B (en) * 2020-08-03 2021-07-20 于瀛 Extraction and leaching method of traditional Chinese medicine

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Application publication date: 20181221