CN108815317A - A kind of preparation process of radix tetrastigme freeze-dried powder - Google Patents

A kind of preparation process of radix tetrastigme freeze-dried powder Download PDF

Info

Publication number
CN108815317A
CN108815317A CN201810815195.3A CN201810815195A CN108815317A CN 108815317 A CN108815317 A CN 108815317A CN 201810815195 A CN201810815195 A CN 201810815195A CN 108815317 A CN108815317 A CN 108815317A
Authority
CN
China
Prior art keywords
freeze
radix tetrastigme
temperature
powder
dried powder
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201810815195.3A
Other languages
Chinese (zh)
Inventor
贺一
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Shanghai Wei Yi Biotechnology Co Ltd
Original Assignee
Shanghai Wei Yi Biotechnology Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Shanghai Wei Yi Biotechnology Co Ltd filed Critical Shanghai Wei Yi Biotechnology Co Ltd
Priority to CN201810815195.3A priority Critical patent/CN108815317A/en
Publication of CN108815317A publication Critical patent/CN108815317A/en
Pending legal-status Critical Current

Links

Classifications

    • 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)
    • A61K36/87Vitaceae or Ampelidaceae (Vine or Grape family), e.g. wine grapes, muscadine or peppervine
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K9/00Medicinal preparations characterised by special physical form
    • A61K9/14Particulate form, e.g. powders, Processes for size reducing of pure drugs or the resulting products, Pure drug nanoparticles
    • A61K9/19Particulate form, e.g. powders, Processes for size reducing of pure drugs or the resulting products, Pure drug nanoparticles lyophilised, i.e. freeze-dried, solutions or dispersions
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F26DRYING
    • F26BDRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
    • F26B1/00Preliminary treatment of solid materials or objects to facilitate drying, e.g. mixing or backmixing the materials to be dried with predominantly dry solids
    • F26B1/005Preliminary treatment of solid materials or objects to facilitate drying, e.g. mixing or backmixing the materials to be dried with predominantly dry solids by means of disintegrating, e.g. crushing, shredding, milling the materials to be dried
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F26DRYING
    • F26BDRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
    • F26B5/00Drying solid materials or objects by processes not involving the application of heat
    • F26B5/04Drying solid materials or objects by processes not involving the application of heat by evaporation or sublimation of moisture under reduced pressure, e.g. in a vacuum
    • F26B5/06Drying solid materials or objects by processes not involving the application of heat by evaporation or sublimation of moisture under reduced pressure, e.g. in a vacuum the process involving freezing
    • 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
    • A61K2236/13Preparation or pretreatment of starting material involving cleaning, e.g. washing or peeling
    • 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
    • A61K2236/15Preparation or pretreatment of starting material involving mechanical treatment, e.g. chopping up, cutting or grinding
    • 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
    • A61K2236/17Preparation or pretreatment of starting material involving drying, e.g. sun-drying or wilting

Landscapes

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

Abstract

The invention discloses a kind of preparation processes of radix tetrastigme freeze-dried powder, including step:1) it pre-processes, after fresh radix tetrastigme stem tuber is carried out ultrasonic cleaning, dried, is ground into coarse powder with roughing mill;2) pre-freeze is handled, at -60~-65 DEG C, 2~3h of pre-freeze;3) Freezing smashing, the radix tetrastigme coarse powder of pre-freeze is crushed again by further cooling make up to after -65 DEG C of glass transition temperature, radix tetrastigme freeze-dried powder after pulverized is classified and is collected by fish grading machine of gas flow screen, and the radix tetrastigme powder for not reaching 500 mesh fineness requirements, which returns to feed bin, to be continued to crush;4) vacuum freeze drying, -65 DEG C of condenser temperature, 10 ± 5Pa of freeze drying box pressure, using radiant heating method, the radix tetrastigme powder temperature of pre-freeze is strictly kept to be lower than -38 DEG C of plait point temperature in drying process, the effective component of the radix tetrastigme freeze-dried powder of preparation retains more complete, it is more preferable to take rear effect, it takes rear human body to be easier to absorb, be unlikely to deteriorate, the time that can be stored is longer.

Description

A kind of preparation process of radix tetrastigme freeze-dried powder
Technical field
The present invention relates to a kind of preparation processes of radix tetrastigme freeze-dried powder.
Background technique
Radix tetrastigme (Tetrastigma hemsleyanum Diels et Gilg) belongs to Vitaceae Tetrastigma plant, Its underground root tuber and herb can all be used as medicine, and be the distinctive rare rare Chinese medicine in China, wherein producing the performance optimal of radix tetrastigme with Zhejiang. According to《Compendium of Materia Medica》It records, radix tetrastigme is cool in nature, nontoxic, sweet and slightly bitter taste, has the effect of clearing heat and detoxicating, promoting blood circulation by removing wind.In radix tetrastigme Chemical component is many kinds of, is known as " the natural composite plant antibiotic of wide spectrum ".The main chemical compositions of radix tetrastigme have flavones, Huang Ketoside, polysaccharide, steroid, amino acid, starch etc., by modern pharmacological studies have shown that radix tetrastigme has heat dissipation, qi-regulating, work Blood, tonifying spleen, removing toxic substances, wind-dispelling, anti-inflammatory, analgesia, antiviral, liver protection, strengthen immunity, it is antitumor the effects of;Radix tetrastigme is anti-swollen In tumor clinical application, by more cancer kind (lung cancer, breast cancer, gastric cancer, malignant lymphoma, liver cancer, kidney, nasopharyngeal carcinoma, uterus Cancer, chronic myelocytic leukemia, Huppert's disease etc.) clinical observation, according to the World Health Organization (WHO) to malignant tumour Curative effect determinate standard counts total effective rate up to 78.33%;Meanwhile discovery is used to treat infantile hyperpyrexia, chronic in conventional therapy Sphagitis, tonsillitis, hepatitis, pneumonia, gastritis, scrofula and snake bite etc. have special effect.Therefore food of Zhejiang Province drug Radix tetrastigme is included in Zhejiang Province's Chinese medicine preparation specification register by Surveillance Authority, and together with the units such as Chinese medicine management board of Zhejiang Province Radix tetrastigme Chinese medicine " new eight Zhe's " was classified as in 2018 to be widelyd popularize.
The eating method of traditional radix tetrastigme is fairly simple, generallys use decoction or dries levigation and swallows, but some suppression cancers Efficacy component depend merely on decocting and can not be precipitated, and drying levigation can be such that a big chunk effective component is lost, and cause drug effect concentration Not enough, the effective component for extracting radix tetrastigme is used to be taken, although effect is preferable, extraction process is complicated, extraction cost It is higher, it is difficult to carry out the popularization of large area;Therefore by radix tetrastigme at low temperature freeze preservation be made " radix tetrastigme freeze-dried powder " just at Only selection, this preparation process can retain the effective active composition of radix tetrastigme to greatest extent, and can make the patient side of taking Just, effect is good, solves the problems, such as that radix tetrastigme extracts complicated, expensive, popularization hardly possible.
Existing radix tetrastigme powder largely uses heated-air drying, and the effective component contained is allowed in radix tetrastigme to be largely lost;It adopts With antivacuum frozen drying, the inorganic salts contained in radix tetrastigme can be made as the drying of moisture is to surface migration, lead to three The Surface hardened layer of leaf blueness powder stirs difficulty when taking after mixing it with water, absorb after taking slowly, rear effect is taken in influence;The system of part freeze-dried powder The temperature of Preparation Method, pre-freeze and crushing not enough (- 40 DEG C or less), causes effective component to keep incomplete, partially containing thermal sensitivity Active constituent is lost.
Summary of the invention
The present invention effectively prevent effective component in radix tetrastigme to be lost in order to solve the above technical problems, providing one kind, is allowed to take It is more preferable with rear effect, greatly improve the preparation process of the quality of radix tetrastigme freeze-dried powder and the radix tetrastigme freeze-dried powder of effect.
The purpose of the present invention is what is be achieved through the following technical solutions:
A kind of preparation process of radix tetrastigme freeze-dried powder, including step:
1) it pre-processes
After fresh radix tetrastigme stem tuber is carried out ultrasonic cleaning, dried, coarse powder is ground into roughing mill;
2) pre-freeze is handled
At -60~-65 DEG C, 2~3h of pre-freeze;
3) Freezing smashing
The radix tetrastigme coarse powder of pre-freeze is subjected to powder by further cooling make up to again after -65 DEG C of glass transition temperature Broken, the radix tetrastigme freeze-dried powder after being crushed is classified and is collected by fish grading machine of gas flow screen, does not reach 500 mesh fineness requirements Radix tetrastigme powder, which returns to feed bin, to be continued to crush;
4) vacuum freeze drying
The setting of vacuum freeze drier:
- 65 DEG C of condenser temperature, vacuum degree:Freeze drying box 10 ± 5Pa of pressure is tight in drying process using radiant heating method The plait point temperature that lattice keep the radix tetrastigme powder temperature of pre-freeze to be lower than -38 DEG C, in the drying process to avoid radix tetrastigme powder Temperature rises the fine structure too fast, the ice crystal thawing destruction freezing for forming pre-freeze is set up, and fine structure is made to collapse It falls into, blocks moisture distillation causes freeze-drying to fail.
The radix tetrastigme stem tuber that radix tetrastigme stem tuber selects growth to expire 4 years in the step 1) as a preferred technical solution,.
As a preferred technical solution, in the step 1), it is 20khz that the ultrasonication, which selects wave band,;The powder The coarse powder partial size being broken into is 20~30 mesh.
The eutectic point of step 2) the pre-freeze processing radix tetrastigme, plait point use electric-resistivity method as a preferred technical solution, It measures.
The specific test method of the electric-resistivity method is as a preferred technical solution,:With market universal tester general-purpose Table makees ohmer, and cryogenic temperature is counted as temperature element, is frozen in DW-450 super-low temperature pulverizator and completes, and when test visits thermometric Head and resistance electrode are inserted in parallel into the center of radix tetrastigme stem tuber, and keep the spacing of 2~3cm, draw freezing with conducting wire and set Standby rear access test macro passes through multimeter reading radix tetrastigme stem tuber synchronous with low-reading thermometer in temperature changing process Resistance value and temperature, the eutectic point for measuring radix tetrastigme is -43 DEG C, and plait point is -38 DEG C.
The step 3) selects deep cooling type super-low temperature pulverizator as a preferred technical solution, and the pulverizer system is with liquid Nitrogen is cold source, and smashed product, which has, to never degenerate, and is not aoxidized, even particle size distribution, the good feature of geometric figure.
Freezing smashing temperature is -80 DEG C in the step 3) as a preferred technical solution,.
Radiant heating is that the radix tetrastigme powder that will need to be freeze-dried is placed in the step 4) as a preferred technical solution, It on basin, is inserted between two panels heating plate, is allowed to and supply heat by heating plate radiation not with contact heater plate, Therefore heating plate can be heated to the temperature of permissible range or more, and by the temperature of dry radix tetrastigme powder be then maintained at allowable temperature it It is interior, distillation can be accelerated in this way and shorten drying time, the operation of dry front and back is also easy to, and is especially filled in Large Scale and Continuous drying It is more efficient in setting.
Advantages of the present invention:
1, the effective component of radix tetrastigme retains more complete, and it is more preferable to take rear effect.
2, when taking after mixing it with water, faster, stirring is easier rehydration the radix tetrastigme freeze-dried powder of this technique preparation, is taken rear human body and is easier to It absorbs.
3, the radix tetrastigme freeze-dried powder of this technique preparation is unlikely to deteriorate, and the time that can be stored is longer.Due to using above-mentioned skill Art scheme, a kind of preparation process of radix tetrastigme freeze-dried powder, including step:1) it pre-processes, fresh radix tetrastigme stem tuber is surpassed Sound wave cleaning after drying, is ground into coarse powder with roughing mill;2) pre-freeze is handled, at -60~-65 DEG C, 2~3h of pre-freeze;3) it freezes It crushes, the radix tetrastigme coarse powder of pre-freeze is crushed again by further cooling make up to after -65 DEG C of glass transition temperature, Radix tetrastigme freeze-dried powder after pulverized is classified and is collected by fish grading machine of gas flow screen, and the three of 500 mesh fineness requirements are not reached Leaf blueness powder, which returns to feed bin, to be continued to crush;4) vacuum freeze drying, the setting of vacuum freeze drier:- 65 DEG C of condenser temperature, vacuum Degree:Freeze drying box 10 ± 5Pa of pressure strictly keeps the radix tetrastigme powder temperature of pre-freeze using radiant heating method in drying process Degree is lower than -38 DEG C of plait point temperature, and the effective component of radix tetrastigme retains more complete, takes that rear effect is more preferable, three leaves of preparation When taking after mixing it with water, faster, stirring is easier rehydration green freeze-dried powder, is taken rear human body and is easier to absorb, is unlikely to deteriorate, the time that can be stored It is longer.
Specific embodiment
The present invention will be further described below with reference to examples, but protection scope of the present invention is not limited solely to implement Example.
A kind of preparation process of radix tetrastigme freeze-dried powder, including step:
1) it pre-processes
After fresh radix tetrastigme stem tuber is carried out ultrasonic cleaning, dried, coarse powder is ground into roughing mill;
2) pre-freeze is handled
At -60~-65 DEG C, 2~3h of pre-freeze;
3) Freezing smashing
The radix tetrastigme coarse powder of pre-freeze is subjected to powder by further cooling make up to again after -65 DEG C of glass transition temperature Broken, the radix tetrastigme freeze-dried powder after being crushed is classified and is collected by fish grading machine of gas flow screen, does not reach 500 mesh fineness requirements Radix tetrastigme powder, which returns to feed bin, to be continued to crush;
4) vacuum freeze drying
The setting of vacuum freeze drier:
- 65 DEG C of condenser temperature, vacuum degree:Freeze drying box 10 ± 5Pa of pressure is tight in drying process using radiant heating method The plait point temperature that lattice keep the radix tetrastigme powder temperature of pre-freeze to be lower than -38 DEG C, in the drying process to avoid radix tetrastigme powder Temperature rises the fine structure too fast, the ice crystal thawing destruction freezing for forming pre-freeze is set up, and fine structure is made to collapse It falls into, blocks moisture distillation causes freeze-drying to fail.
The radix tetrastigme stem tuber that radix tetrastigme stem tuber selects growth to expire 4 years in the step 1).
In the step 1), it is 20khz that the ultrasonication, which selects wave band,;The coarse powder partial size being ground into be 20~ 30 mesh.
The eutectic point of step 2) the pre-freeze processing radix tetrastigme, plait point are measured using electric-resistivity method.
The specific test method of electric-resistivity method is:Make ohmer, cryogenic temperature with market universal tester multimeter It is counted as temperature element, is frozen in DW-450 super-low temperature pulverizator and completes, is inserted temperature probe is parallel with resistance electrode when test Enter the center of radix tetrastigme stem tuber, and keep the spacing of 2~3cm, accesses test macro after drawing freezing equipment with conducting wire, In temperature changing process, pass through the multimeter resistance value and temperature for reading radix tetrastigme stem tuber synchronous with low-reading thermometer, measurement three The eutectic point of Ye Qing is -43 DEG C, and plait point is -38 DEG C.
The step 3) selects deep cooling type super-low temperature pulverizator, and the pulverizer system is using liquid nitrogen as cold source, smashed production Product, which have, to never degenerate, and does not aoxidize, even particle size distribution, the good feature of geometric figure.
Freezing smashing temperature is -80 DEG C in the step 3).
Radiant heating is that the radix tetrastigme powder that will need to be freeze-dried is placed on basin in the step 4), is inserted into two Between piece heating plate, it is allowed to and supply heat by heating plate radiation, therefore heating plate can be heated to hold not with contact heater plate Perhaps temperature more than range, and be then maintained within allowable temperature by the temperature of dry radix tetrastigme powder, it can accelerate to distil in this way Shorten drying time, the operation of dry front and back is also easy to, especially more efficient in Large Scale and Continuous drying device.
Embodiment 1:
A kind of preparation process of radix tetrastigme freeze-dried powder, including step:
1) it pre-processes
After fresh radix tetrastigme stem tuber is carried out ultrasonic cleaning, dried, coarse powder is ground into roughing mill;
2) pre-freeze is handled
At -60 DEG C, pre-freeze 2h;
3) Freezing smashing
The radix tetrastigme coarse powder of pre-freeze is subjected to powder by further cooling make up to again after -65 DEG C of glass transition temperature Broken, the radix tetrastigme freeze-dried powder after being crushed is classified and is collected by fish grading machine of gas flow screen, does not reach 500 mesh fineness requirements Radix tetrastigme powder, which returns to feed bin, to be continued to crush;
4) vacuum freeze drying
The setting of vacuum freeze drier:
- 65 DEG C of condenser temperature, vacuum degree:Freeze drying box pressure 5Pa is strictly protected in drying process using radiant heating method The radix tetrastigme powder temperature for holding pre-freeze is lower than -38 DEG C of plait point temperature, to avoid radix tetrastigme powder temperature in the drying process Rise the fine structure too fast, the ice crystal thawing destruction freezing for forming pre-freeze is set up, collapses fine structure, hinder Disconnected water sublimed, causes freeze-drying to fail.
The radix tetrastigme stem tuber that radix tetrastigme stem tuber selects growth to expire 4 years in the step 1).
In the step 1), the ultrasonication select wave band be~;The coarse powder partial size being ground into is~mesh.
The eutectic point of step 2) the pre-freeze processing radix tetrastigme, plait point are measured using electric-resistivity method.
The specific test method of electric-resistivity method is:Make ohmer, cryogenic temperature with market universal tester multimeter It is counted as temperature element, is frozen in DW-450 super-low temperature pulverizator and completes, is inserted temperature probe is parallel with resistance electrode when test Enter the center of radix tetrastigme stem tuber, and keep the spacing of 2cm, test macro is accessed after drawing freezing equipment with conducting wire, in temperature It spends in change procedure, by the multimeter resistance value and temperature for reading radix tetrastigme stem tuber synchronous with low-reading thermometer, measures three leaves Green eutectic point is -43 DEG C, and plait point is -38 DEG C.
The step 3) selects deep cooling type super-low temperature pulverizator, and the pulverizer system is using liquid nitrogen as cold source, smashed production Product, which have, to never degenerate, and does not aoxidize, even particle size distribution, the good feature of geometric figure.
Freezing smashing temperature is -80 DEG C in the step 3).
Radiant heating is that the radix tetrastigme powder that will need to be freeze-dried is placed on basin in the step 4), is inserted into two Between piece heating plate, it is allowed to and supply heat by heating plate radiation, therefore heating plate can be heated to hold not with contact heater plate Perhaps temperature more than range, and be then maintained within allowable temperature by the temperature of dry radix tetrastigme powder, it can accelerate to distil in this way Shorten drying time, the operation of dry front and back is also easy to, especially more efficient in Large Scale and Continuous drying device.
Embodiment 2:
A kind of preparation process of radix tetrastigme freeze-dried powder, including step:
1) it pre-processes
After fresh radix tetrastigme stem tuber is carried out ultrasonic cleaning, dried, coarse powder is ground into roughing mill;
2) pre-freeze is handled
At -62 DEG C, pre-freeze 2.5h;
3) Freezing smashing
The radix tetrastigme coarse powder of pre-freeze is subjected to powder by further cooling make up to again after -65 DEG C of glass transition temperature Broken, the radix tetrastigme freeze-dried powder after being crushed is classified and is collected by fish grading machine of gas flow screen, does not reach 500 mesh fineness requirements Radix tetrastigme powder, which returns to feed bin, to be continued to crush;
4) vacuum freeze drying
The setting of vacuum freeze drier:
- 65 DEG C of condenser temperature, vacuum degree:Freeze drying box pressure 10Pa is strictly protected in drying process using radiant heating method The radix tetrastigme powder temperature for holding pre-freeze is lower than -38 DEG C of plait point temperature, to avoid radix tetrastigme powder temperature in the drying process Rise the fine structure too fast, the ice crystal thawing destruction freezing for forming pre-freeze is set up, collapses fine structure, hinder Disconnected water sublimed, causes freeze-drying to fail.
The radix tetrastigme stem tuber that radix tetrastigme stem tuber selects growth to expire 4 years in the step 1).
In the step 1), it is 20khz that the ultrasonication, which selects wave band,;The coarse powder partial size being ground into is 25 Mesh.
The eutectic point of step 2) the pre-freeze processing radix tetrastigme, plait point are measured using electric-resistivity method.
The specific test method of electric-resistivity method is:Make ohmer, cryogenic temperature with market universal tester multimeter It is counted as temperature element, is frozen in DW-450 super-low temperature pulverizator and completes, is inserted temperature probe is parallel with resistance electrode when test Enter the center of radix tetrastigme stem tuber, and keep the spacing of 2.5cm, accesses test macro after drawing freezing equipment with conducting wire, In temperature changing process, pass through the multimeter resistance value and temperature for reading radix tetrastigme stem tuber synchronous with low-reading thermometer, measurement three The eutectic point of Ye Qing is -43 DEG C, and plait point is -38 DEG C.
The step 3) selects deep cooling type super-low temperature pulverizator, and the pulverizer system is using liquid nitrogen as cold source, smashed production Product, which have, to never degenerate, and does not aoxidize, even particle size distribution, the good feature of geometric figure.
Freezing smashing temperature is -80 DEG C in the step 3).
Radiant heating is that the radix tetrastigme powder that will need to be freeze-dried is placed on basin in the step 4), is inserted into two Between piece heating plate, it is allowed to and supply heat by heating plate radiation, therefore heating plate can be heated to hold not with contact heater plate Perhaps temperature more than range, and be then maintained within allowable temperature by the temperature of dry radix tetrastigme powder, it can accelerate to distil in this way Shorten drying time, the operation of dry front and back is also easy to, especially more efficient in Large Scale and Continuous drying device.
Embodiment 3:
A kind of preparation process of radix tetrastigme freeze-dried powder, including step:
1) it pre-processes
After fresh radix tetrastigme stem tuber is carried out ultrasonic cleaning, dried, coarse powder is ground into roughing mill;
2) pre-freeze is handled
At -65 DEG C, pre-freeze 3h;
3) Freezing smashing
The radix tetrastigme coarse powder of pre-freeze is subjected to powder by further cooling make up to again after -65 DEG C of glass transition temperature Broken, the radix tetrastigme freeze-dried powder after being crushed is classified and is collected by fish grading machine of gas flow screen, does not reach 500 mesh fineness requirements Radix tetrastigme powder, which returns to feed bin, to be continued to crush;
4) vacuum freeze drying
The setting of vacuum freeze drier:
- 65 DEG C of condenser temperature, vacuum degree:Freeze drying box pressure 15Pa is strictly protected in drying process using radiant heating method The radix tetrastigme powder temperature for holding pre-freeze is lower than -38 DEG C of plait point temperature, to avoid radix tetrastigme powder temperature in the drying process Rise the fine structure too fast, the ice crystal thawing destruction freezing for forming pre-freeze is set up, collapses fine structure, hinder Disconnected water sublimed, causes freeze-drying to fail.
The radix tetrastigme stem tuber that radix tetrastigme stem tuber selects growth to expire 4 years in the step 1).
In the step 1), it is 20khz that the ultrasonication, which selects wave band,;The coarse powder partial size being ground into is 30 Mesh.
The eutectic point of step 2) the pre-freeze processing radix tetrastigme, plait point are measured using electric-resistivity method.
The specific test method of electric-resistivity method is:Make ohmer, cryogenic temperature with market universal tester multimeter It is counted as temperature element, is frozen in DW-450 super-low temperature pulverizator and completes, is inserted temperature probe is parallel with resistance electrode when test Enter the center of radix tetrastigme stem tuber, and keep the spacing of 3cm, test macro is accessed after drawing freezing equipment with conducting wire, in temperature It spends in change procedure, by the multimeter resistance value and temperature for reading radix tetrastigme stem tuber synchronous with low-reading thermometer, measures three leaves Green eutectic point is -43 DEG C, and plait point is -38 DEG C.
The step 3) selects deep cooling type super-low temperature pulverizator, and the pulverizer system is using liquid nitrogen as cold source, smashed production Product, which have, to never degenerate, and does not aoxidize, even particle size distribution, the good feature of geometric figure.
Freezing smashing temperature is -80 DEG C in the step 3).
Radiant heating is that the radix tetrastigme powder that will need to be freeze-dried is placed on basin in the step 4), is inserted into two Between piece heating plate, it is allowed to and supply heat by heating plate radiation, therefore heating plate can be heated to hold not with contact heater plate Perhaps temperature more than range, and be then maintained within allowable temperature by the temperature of dry radix tetrastigme powder, it can accelerate to distil in this way Shorten drying time, the operation of dry front and back is also easy to, especially more efficient in Large Scale and Continuous drying device.
Finally it should be noted that:Above embodiments are only to illustrate the present invention and not limit technology described in the invention Scheme;Therefore, although this specification is referring to above-mentioned each embodiment, the present invention has been described in detail, this Field it is to be appreciated by one skilled in the art that still can modify to the present invention or equivalent replacement;And all do not depart from this The technical solution and its improvement of the spirit and scope of invention, should all cover within the scope of the claims of the present invention.

Claims (8)

1. a kind of preparation process of radix tetrastigme freeze-dried powder, which is characterized in that including step:
1) it pre-processes
After fresh radix tetrastigme stem tuber is carried out ultrasonic cleaning, dried, coarse powder is ground into roughing mill;
2) pre-freeze is handled
At -60~-65 DEG C, 2~3h of pre-freeze;
3) Freezing smashing
The radix tetrastigme coarse powder of pre-freeze is crushed again by further cooling make up to after -65 DEG C of glass transition temperature, Radix tetrastigme freeze-dried powder after pulverized is classified and is collected by fish grading machine of gas flow screen, and the three of 500 mesh fineness requirements are not reached Leaf blueness powder, which returns to feed bin, to be continued to crush;
4) vacuum freeze drying
The setting of vacuum freeze drier:
- 65 DEG C of condenser temperature, vacuum degree:Freeze drying box 10 ± 5Pa of pressure is strictly protected in drying process using radiant heating method The radix tetrastigme powder temperature for holding pre-freeze is lower than -38 DEG C of plait point temperature.
2. the preparation process of radix tetrastigme freeze-dried powder as described in claim 1, it is characterised in that:Radix tetrastigme block in the step 1) The radix tetrastigme stem tuber that stem selects growth to expire 4 years.
3. the preparation process of radix tetrastigme freeze-dried powder as described in claim 1, it is characterised in that:It is described super in the step 1) It is 20khz that sonicated, which selects wave band,;The coarse powder partial size being ground into is 20~30 mesh.
4. the preparation process of radix tetrastigme freeze-dried powder as described in claim 1, it is characterised in that:Step 2) the pre-freeze processing three The eutectic point of Ye Qing, plait point are measured using electric-resistivity method.
5. the preparation process of radix tetrastigme freeze-dried powder as claimed in claim 4, it is characterised in that:The electric-resistivity method is specifically tested Method is:Make ohmer with market universal tester multimeter, cryogenic temperature is counted as temperature element, and it is ultralow to be frozen in DW-450 It is completed in warm pulverizer, when test is inserted in parallel into temperature probe and resistance electrode the center of radix tetrastigme stem tuber, and keeps 2 The spacing of~3cm accesses test macro after drawing freezing equipment with conducting wire, in temperature changing process, by multimeter and low The synchronous resistance value and temperature for reading radix tetrastigme stem tuber of temperature thermometer, the eutectic point for measuring radix tetrastigme is -43 DEG C, plait point is - 38℃。
6. the preparation process of radix tetrastigme freeze-dried powder as described in claim 1, it is characterised in that:The step 3) selects deep cooling type Super-low temperature pulverizator, the pulverizer system is using liquid nitrogen as cold source.
7. the preparation process of radix tetrastigme freeze-dried powder as described in claim 1, it is characterised in that:Freezing smashing in the step 3) Temperature is -80 DEG C.
8. the preparation process of radix tetrastigme freeze-dried powder as described in claim 1, it is characterised in that:Radiant heating in the step 4) Be that the radix tetrastigme powder that will need to be freeze-dried is placed on basin, be inserted between two panels heating plate, be allowed to not with heating plate Contact, and heat is supplied by heating plate radiation, therefore heating plate can be heated to the temperature of permissible range or more, and by dry three The temperature of leaf blueness powder is then maintained within allowable temperature, can be accelerated distillation in this way and be shortened drying time, the operation of dry front and back Also it is easy to, it is especially more efficient in Large Scale and Continuous drying device.
CN201810815195.3A 2018-07-23 2018-07-23 A kind of preparation process of radix tetrastigme freeze-dried powder Pending CN108815317A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201810815195.3A CN108815317A (en) 2018-07-23 2018-07-23 A kind of preparation process of radix tetrastigme freeze-dried powder

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201810815195.3A CN108815317A (en) 2018-07-23 2018-07-23 A kind of preparation process of radix tetrastigme freeze-dried powder

Publications (1)

Publication Number Publication Date
CN108815317A true CN108815317A (en) 2018-11-16

Family

ID=64140460

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201810815195.3A Pending CN108815317A (en) 2018-07-23 2018-07-23 A kind of preparation process of radix tetrastigme freeze-dried powder

Country Status (1)

Country Link
CN (1) CN108815317A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113144053A (en) * 2020-11-23 2021-07-23 王春燕 A multifunctional radix Apioris Fortunei powder for preventing and treating various diseases

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101791361A (en) * 2009-12-24 2010-08-04 胡馨尹 Vacuum freeze-drying process for retaining medicative active components of traditional Chinese medicine of radix tetrastigme
CN102846698A (en) * 2012-08-20 2013-01-02 浙江中医药大学中药饮片有限公司 Wall-broken radix tetrastigme oral decoction pieces
CN103948668A (en) * 2014-03-20 2014-07-30 武义寿仙谷中药饮片有限公司 Preparation method of radix tetrastigme powder

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101791361A (en) * 2009-12-24 2010-08-04 胡馨尹 Vacuum freeze-drying process for retaining medicative active components of traditional Chinese medicine of radix tetrastigme
CN102846698A (en) * 2012-08-20 2013-01-02 浙江中医药大学中药饮片有限公司 Wall-broken radix tetrastigme oral decoction pieces
CN103948668A (en) * 2014-03-20 2014-07-30 武义寿仙谷中药饮片有限公司 Preparation method of radix tetrastigme powder

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
谭韩英,仇厚援,等: "不同冻干辅料对蜂王浆共晶点的影响", 《食品工业科技》 *
阿里巴巴生意经: "《https://baike.1688.com/doc/view-d2264639.html》", 8 July 2009 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113144053A (en) * 2020-11-23 2021-07-23 王春燕 A multifunctional radix Apioris Fortunei powder for preventing and treating various diseases

Similar Documents

Publication Publication Date Title
CN102793733B (en) Ginseng royal jelly chewable tablets and preparation method thereof
CN102716348B (en) Method for preparing superfine rhizoma gastrodiae powder by vacuum freeze drying
CN104258178A (en) Medicine for treating lung cancer pleural effusion and preparation method of medicine
CN108815317A (en) A kind of preparation process of radix tetrastigme freeze-dried powder
CN112826852B (en) Preparation method of high-content coptis chinensis powder
CN102716175B (en) Superfine eucommia ulmoides powder and preparation method thereof
CN113144053A (en) A multifunctional radix Apioris Fortunei powder for preventing and treating various diseases
CN104547209A (en) Preparation method of traditional Chinese medicine composition
CN105412827A (en) Medicine for treating liver cancer and preparation method for medicine
CN105362766A (en) Miraculous pill of ledebouriella and preparation method of pill
CN104840511A (en) Method for drying astragalus membranaceus traditional Chinese medicinal material
CN105030847A (en) Preparation method of nanometer Chinese herbal medicine ultrafine powder
CN104687042B (en) Composite aloe deobstruent and preparation method thereof
CN107617098A (en) One kind treats psoriasic composition
CN105412536A (en) Rhinitis treating pill and preparation method thereof
CN104383516A (en) Shaoyang cold treatment granules and preparation method for same
CN104524265A (en) Junbai ganyan granules and preparation method thereof
CN105708873A (en) Chinese astilbe herb ultra-fine powder decoction pieces and preparation method thereof
CN116077577A (en) Preparation method of heat clearing medicinal composition
CN105213513A (en) A kind of tumour eliminating and analgesic plaster and preparation method thereof
CN116115716A (en) Traditional Chinese medicine composition of lung-heat clearing and phlegm eliminating soup
CN104474089A (en) Wuweixianglian pill and preparation method thereof
CN102961532A (en) Traditional Chinese medicine for treating anaphylactoid purpura
CN104107253B (en) A kind of Chinese medicine treating pityriasis rubra pilaris
CN113925926A (en) Traditional Chinese medicine composition for treating breast cancer

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
WD01 Invention patent application deemed withdrawn after publication
WD01 Invention patent application deemed withdrawn after publication

Application publication date: 20181116