CN105663179B - A kind of production method improving pinecone clear cream melting - Google Patents

A kind of production method improving pinecone clear cream melting Download PDF

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Publication number
CN105663179B
CN105663179B CN201610046192.9A CN201610046192A CN105663179B CN 105663179 B CN105663179 B CN 105663179B CN 201610046192 A CN201610046192 A CN 201610046192A CN 105663179 B CN105663179 B CN 105663179B
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pinecone
vacuum
clear cream
heating
mesh
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CN105663179A (en
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武俊明
付廷明
吴春芳
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JIANGSU ZHONGXING PHARMACEUTICAL CO Ltd
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JIANGSU ZHONGXING PHARMACEUTICAL CO Ltd
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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
    • A61K36/13Coniferophyta (gymnosperms)
    • A61K36/15Pinaceae (Pine family), e.g. pine or cedar
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K47/00Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
    • A61K47/30Macromolecular organic or inorganic compounds, e.g. inorganic polyphosphates
    • A61K47/36Polysaccharides; Derivatives thereof, e.g. gums, starch, alginate, dextrin, hyaluronic acid, chitosan, inulin, agar or pectin
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K9/00Medicinal preparations characterised by special physical form
    • A61K9/06Ointments; Bases therefor; Other semi-solid forms, e.g. creams, sticks, gels
    • 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
    • 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
    • A61K2236/30Extraction of the material
    • A61K2236/33Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
    • A61K2236/331Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using water, e.g. cold water, infusion, tea, steam distillation, decoction
    • 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
    • A61K2236/30Extraction of the material
    • A61K2236/39Complex extraction schemes, e.g. fractionation or repeated extraction steps
    • 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
    • A61K2236/51Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying
    • 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)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Pharmacology & Pharmacy (AREA)
  • Natural Medicines & Medicinal Plants (AREA)
  • Veterinary Medicine (AREA)
  • Public Health (AREA)
  • General Health & Medical Sciences (AREA)
  • Animal Behavior & Ethology (AREA)
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  • Alternative & Traditional Medicine (AREA)
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  • Microbiology (AREA)
  • Medical Informatics (AREA)
  • Botany (AREA)
  • Biotechnology (AREA)
  • Engineering & Computer Science (AREA)
  • Inorganic Chemistry (AREA)
  • Medicinal Preparation (AREA)
  • Medicines Containing Plant Substances (AREA)

Abstract

The invention discloses a kind of extracting method for improving pinecone clear cream melting index, it is 2~3 hours dry in 85~90 degree to include the following steps: that the pinecone to be processed is put into heated-air circulation oven by (1);(2) pinecone after drying is decocted, takes supernatant liquid filtering and obtains filtrate, crossed after filtering out precipitating and obtained decoction liquor is filtered by vacuum by the filter cloth of 400 mesh;(3) finished product clear cream required for smoke filtrate is completed by heating in vacuum sprinkling concentration.The present invention passes through 85~90 degree of dryings of the pinecone to quasi- decoction, the molecular structure of pinecone surface waxes is destroyed, influence of the waxes to clear cream melting is eliminated, is filtered by vacuum by 400 mesh filter clothes, the time for standing removal of impurities is not only greatly shortened, the production cycle is shortened.And effect at low cost is good.Heating in vacuum spray wine enrichment facility not only avoids the breeze occurred in Conventional concentration high temperature, improves the validity of drug, and operating method is simple, applied widely, condition is easy to control.

Description

A kind of production method improving pinecone clear cream melting
Technical field
The invention belongs to Chinese medicine preparation fields, and in particular to a kind of production method for improving pinecone clear cream melting.
Background technique
In pharmaceutical production, as needed, medicinal extract is processed into dry powder by commonly used dry technology, and dry technology generallys use Spray drying technology, the application constantly extension in the field of Chinese medicines, plays an important role in, drying principles are usual are as follows: Decoction liquor passes through the temperature for being heated to corresponding requirements, and the centrifugal type atomizer for being located at dry tower top is supplied to through product pump, utilizes height Speed centrifugation is atomized into medicinal extract the drop of corresponding requirements, uniformly sprays into drying tower, carries out big face with the hot-air for entering drying tower Product counter current contact, instantaneously completes drying and moulding, obtains dry powder-shaped product, and the extract dry powder that this technique is made has easily storage It deposits, transports, the advantages that long shelf-life.Good extract dry powder has good melting, but due to long-term production, in air Impurity is carried, impurity, which can remain in the duct and enter in drying tower, pollutes extract dry powder, influences product quality, causes to produce Extract dry powder melting out reduces.
At present for the processing step of pinecone clear cream are as follows: by adding water to cook twice the pinecone, 2~3 hours every time, merge Decocting liquid, staticly settles and filters, and then takes supernatant to be concentrated into relative density and obtains clear cream for 1.23~1.25, but due to standing Filtration time is long, and conventional high-temperature concentration is easy to appear breeze, reduces the validity of drug.
Summary of the invention
Goal of the invention: when to solve to prepare pinecone clear cream in the prior art, the production cycle is long, while being easy to appear in product Breeze reduces the melting and validity of drug, and the invention proposes a kind of method for improving pinecone clear cream melting, Ke Yiyou Effect lowers the production cycle, while improving the validity of drug, and operating method is simple, and applied widely, condition is easy to control.
Technical solution: to realize the above-mentioned technical purpose, the present invention proposes a kind of method for improving pinecone clear cream melting, packet Include following steps:
(1) pinecone to be processed is put into heated-air circulation oven 2~3 hours dry in 85~90 degree;
(2) pinecone after drying is decocted, takes supernatant liquid filtering and obtains filtrate, crossed decoction liquor after filtering out precipitating It is filtered by vacuum by the filter cloth of 400 mesh;
(3) finished product clear cream required for smoke filtrate is completed by heating in vacuum sprinkling concentration.
Preferably, be added in step (2), when decoction it is dry after 1.5~3 times of the pinecone of water decocted.
Specifically, in step (2), the pinecone is added water to cook twice, every time 2~3h, is then combined with decocting liquid and is decocted Boil liquid.
Wherein, in step (3), heating in vacuum sprinkling concentration includes at least secondary vacuum heating sprinkling concentration, and every level-one is true After sky heating sprinkling concentration, the clear cream of formation is collected, does not enter the sprinkling concentration of next stage heating in vacuum at the smoke filtrate of clear cream, In, every level-one vacuum degree is set as -0.05~-0.1MPa, and the aperture of spray head is 80~100 mesh, and temperature is 80~90 DEG C.Smoke filtrate The overwhelming majority has become clear cream after the sprinkling concentration of level-one heating in vacuum, not at the smoke filtrate of clear cream further across second level Clear cream is formed after heating in vacuum sprinkling concentration.General secondary vacuum heating sprinkling concentration can be all as clear cream, can basis Needs of production adjusts vacuum degree, drying temperature and spraying speed and sprays series to adjust required heating in vacuum.
Alternatively embodiment carries out flocculation sedimentation before the filter cloth vacuum filtration of 400 mesh, flocculation sedimentation Step are as follows: regulating liquid medicine pH is 4~8, stirring, chitosan is added when temperature is 40~60 DEG C, the amount that chitosan is added is every The pinecone after gram dry corresponds to the chitosan of 0.001~0.1g, and continuing stirring makes whole system become flocculation system, then right Material is stood;24~48 hours are stood after clarification, supernatant liquid filtering is taken and obtains the decoction liquor after flocculation sedimentation.In recent years, Some new materials, new technology (flocculation clarification technique) start the purification applied to Chinese medicine extract to replace traditional alcohol precipitation work Skill, to reduce production cost, shorten the production cycle, especially to the humidity resistance for improving product during preparation produces and stores Aspect has good effect, guarantees the content of preparation stability and effective component.There are many type of flocculant, there is tannic acid, bright Glue, 101 fruit juice clarifiers, ZTC clarifying agent, chitosan etc..Chitosan (a kind of Old Region) is that the part of chitin takes off second Acyl product, and the polysaccharide of unique natural alkalinity found so far, are the natural high molecular substances containing glycosaminoglycan, positively charged Lotus can settle suspended matter negatively charged in medical fluid (such as cellulose, pigment, tannin, bacterium).And good biocompatibility, and It can be biodegradable, catabolite is non-toxic, and the research application in field of traditional Chinese medicine pharmacy is very active at present, soaks for Chinese medicine The flocculation of extract is clarified, can play the role of it is certain isolate and purify, may replace Chinese materia medica preparation produce in alcohol precipitation process, subtract simultaneously The pollution of few environment.
The utility model has the advantages that compared with prior art, the present invention before decoction by being added in the preparation process of pinecone clear cream 85~90 degree of dry steps, can effectively destroy the molecular structure of pinecone surface waxes, eliminate waxes and dissolve to clear cream Property influence, by 400 mesh filter clothes be filtered by vacuum, not only greatly shorten stand removal of impurities time, shorten the production cycle. And effect at low cost is good.Heating in vacuum spray wine enrichment facility not only avoids the breeze occurred in Conventional concentration high temperature, improves The validity of drug, and operating method is simple, and applied widely, condition is easy to control.
Specific embodiment
Below by specific embodiment, the present invention will be described in detail.
Embodiment 1 includes the following steps: present embodiment discloses a kind of method for improving pinecone clear cream melting
(1) pinecone to be processed is put into heated-air circulation oven 2 hours dry in 90 DEG C of degree;
(2) pinecone after drying is decocted, be added when decoction it is dry after 2 times of the pinecone of water decocted, decoct Twice, 2~3h every time, is then combined with decocting liquid and obtains decoction liquor, and decoction liquor is filtered by vacuum by the filter cloth of 400 mesh;
(3) smoke filtrate is set as -0.05MPa by secondary vacuum heating sprinkling concentration, vacuum degree, and the aperture of spray head is 100 Mesh, temperature are 90 DEG C, after every level-one heating in vacuum sprinkling concentration, the clear cream of formation are collected, under not entering at the smoke filtrate of clear cream The sprinkling concentration of level-one heating in vacuum, smoke filtrate overwhelming majority after the sprinkling concentration of level-one heating in vacuum have become clear cream, not Clear cream is formed after heating sprinkling concentration further across secondary vacuum at the smoke filtrate of clear cream.
Embodiment 2
The method and embodiment 1 of the present embodiment are essentially identical, unlike, in order to be eliminated as much as the impurity in medical fluid, Flocculation sedimentation being carried out before the filter cloth vacuum filtration of 400 mesh, the flocculation sedimentation the step of are as follows: regulating liquid medicine pH is 7, stirring, Chitosan is added when temperature is 60 DEG C, the pinecone after the amount that chitosan is added is every gram dry is poly- corresponding to the shell of 0.005g Sugar, continuing stirring makes whole system become flocculation system, then stands to material;24 hours are stood after clarification, takes supernatant Filter the decoction liquor after obtaining flocculation sedimentation.
Embodiment 3 includes the following steps: present embodiment discloses a kind of method for improving pinecone clear cream melting
(1) pinecone to be processed is put into heated-air circulation oven 2 hours dry in 85 DEG C of degree;
(2) pinecone after drying is decocted, be added when decoction it is dry after 2 times of the pinecone of water decocted, decoct Twice, 2~3h every time, is then combined with decocting liquid and obtains decoction liquor, and decoction liquor is filtered by vacuum by the filter cloth of 400 mesh;
(3) smoke filtrate is set as -0.1MPa by secondary vacuum heating sprinkling concentration, vacuum degree, and the aperture of spray head is 100 Mesh, temperature are 85 DEG C, after every level-one heating in vacuum sprinkling concentration, the clear cream of formation are collected, under not entering at the smoke filtrate of clear cream The sprinkling concentration of level-one heating in vacuum, smoke filtrate overwhelming majority after the sprinkling concentration of level-one heating in vacuum have become clear cream, not Clear cream is formed after heating sprinkling concentration further across secondary vacuum at the smoke filtrate of clear cream.
Embodiment 4
The method and embodiment 1 of the present embodiment are essentially identical, unlike, in order to be eliminated as much as the impurity in medical fluid, Flocculation sedimentation being carried out before the filter cloth vacuum filtration of 400 mesh, the flocculation sedimentation the step of are as follows: regulating liquid medicine pH is 6, stirring, Chitosan is added when temperature is 60 DEG C, the pinecone after the amount that chitosan is added is every gram dry is poly- corresponding to the shell of 0.005g Sugar, continuing stirring makes whole system become flocculation system, then stands to material;24 hours are stood after clarification, takes supernatant Filter the decoction liquor after obtaining flocculation sedimentation.Comparative example: by adding water to cook twice the pinecone, 2~3 hours every time, merge Decocting liquid, staticly settles and filters, and then takes supernatant to be concentrated into relative density and obtains clear cream for 1.23~1.25.
The dissolution rate of the pinecone clear cream of Examples 1 to 5 preparation and the clear cream of comparative example preparation is investigated, as a result as follows:
Project Embodiment 1 Embodiment 2 Embodiment 3 Embodiment 4 Comparative example
Dissolution rate 85% 89% 87% 91% 55%
Meanwhile the clear cream of the pinecone clear cream of Examples 1 to 5 preparation and comparative example preparation is dissolved in 80~90 DEG C of water respectively In, detect its melting, it can be seen that the pinecone clear cream of Examples 1 to 5 preparation dissolves rapidly and the appearance without breeze, and right The pinecone clear cream of ratio breeze then occurs and there are the undissolved phenomenons in part.
In conclusion heating in vacuum spray wine enrichment facility not only avoids the breeze occurred in Conventional concentration high temperature, improve The validity of drug, and operating method is simple, and applied widely, condition is easy to control.
The above content is combine specific preferred embodiment to further description made by invention, and it cannot be said that originally The specific implementation of invention is only limited to these instructions.For those of ordinary skill in the art to which the present invention belongs, not Under the premise of being detached from present invention think of, a number of simple deductions or replacements can also be made, all shall be regarded as belonging to protection of the invention Range.

Claims (5)

1. a kind of method for improving pinecone clear cream melting, which comprises the steps of:
(1) pinecone to be processed is put into heated-air circulation oven 2~3 hours dry in 85~90 degree;
(2) pinecone after drying is decocted, takes supernatant liquid filtering and obtains filtrate, cross the decoction that filters out and will obtain after precipitating Liquid is filtered by vacuum by the filter cloth of 400 mesh;
(3) finished product clear cream required for smoke filtrate is completed by heating in vacuum sprinkling concentration.
2. the method according to claim 1, wherein in step (2), when decoction be added it is dry after the pinecone 1.5 ~3 times of water is decocted.
3. the method according to claim 1, wherein the pinecone adds water to cook twice, often in step (2) Secondary 2~3h is then combined with decocting liquid and obtains decoction liquor.
4. the method according to claim 1, wherein heating in vacuum sprinkling concentration includes at least two in step (3) Grade heating in vacuum sprinkling concentration collects the clear cream of formation after the sprinkling concentration of every level-one heating in vacuum, not at the smoke filtrate of clear cream into Entering the sprinkling concentration of next stage heating in vacuum, wherein every level-one vacuum degree is set as -0.05~-0.1MPa, and the aperture of spray head is 80~ 100 mesh, temperature are 80~90 DEG C.
5. the method according to claim 1, wherein it is heavy to carry out flocculation before the filter cloth vacuum filtration of 400 mesh The step of shallow lake, flocculation sedimentation are as follows: regulating liquid medicine pH is 4~8, and chitosan, chitosan is added when temperature is 40~60 DEG C in stirring The amount of addition is chitosan of the pinecone after every gram of drying corresponding to 0.001~0.1g, and continuing stirring makes whole system become wadding Solidifying system, then stands material;24-48 hour are stood after clarifying, supernatant liquid filtering is taken and obtains pan-fried after flocculation sedimentation Boil liquid.
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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101015572A (en) * 2007-02-07 2007-08-15 哈尔滨工业大学 Extraction method of korean pine cone extractive
CN101181312A (en) * 2007-11-28 2008-05-21 哈尔滨医科大学 Method for preparing korean pine cone extract
CN101773527A (en) * 2010-03-04 2010-07-14 大理学院 Pinecone extractive of Yunnan Pinus and preparation method and medicinal application thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101015572A (en) * 2007-02-07 2007-08-15 哈尔滨工业大学 Extraction method of korean pine cone extractive
CN101181312A (en) * 2007-11-28 2008-05-21 哈尔滨医科大学 Method for preparing korean pine cone extract
CN101773527A (en) * 2010-03-04 2010-07-14 大理学院 Pinecone extractive of Yunnan Pinus and preparation method and medicinal application thereof

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
正交试验法优选云南松松塔总黄酮的提取工艺;李冬梅 等;《中国实验方剂学杂志》;20130131;第19卷(第1期);第37-39页
红松松塔多糖提取工艺优化及其含量测定;杨鑫 等;《中成药》;20110228;第33卷(第2期);第351-353页

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