CN106389604A - Method for preparing pericarpium citri reticulatae extract at room temperature - Google Patents
Method for preparing pericarpium citri reticulatae extract at room temperature Download PDFInfo
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- CN106389604A CN106389604A CN201610855123.2A CN201610855123A CN106389604A CN 106389604 A CN106389604 A CN 106389604A CN 201610855123 A CN201610855123 A CN 201610855123A CN 106389604 A CN106389604 A CN 106389604A
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- pericarpium citri
- citri reticulatae
- room temperature
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- reticulatae extract
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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)
- A61K36/75—Rutaceae (Rue family)
- A61K36/752—Citrus, e.g. lime, orange or lemon
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K31/00—Medicinal preparations containing organic active ingredients
- A61K31/70—Carbohydrates; Sugars; Derivatives thereof
- A61K31/7042—Compounds having saccharide radicals and heterocyclic rings
- A61K31/7048—Compounds having saccharide radicals and heterocyclic rings having oxygen as a ring hetero atom, e.g. leucoglucosan, hesperidin, erythromycin, nystatin, digitoxin or digoxin
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/0211—Solvent extraction of solids in combination with an electric or magnetic field
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/0261—Solvent extraction of solids comprising vibrating mechanisms, e.g. mechanical, acoustical
- B01D11/0265—Applying ultrasound
-
- 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
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- 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
- A61K2236/17—Preparation or pretreatment of starting material involving drying, e.g. sun-drying or wilting
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- 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
- A61K2236/331—Extraction 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
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- Health & Medical Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Natural Medicines & Medicinal Plants (AREA)
- Life Sciences & Earth Sciences (AREA)
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- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Acoustics & Sound (AREA)
- General Health & Medical Sciences (AREA)
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Abstract
The invention relates to a method for preparing a pericarpium citri reticulatae extract at room temperature. The method comprises the following steps: drying and pulverizing pericarpium citri reticulatae, and feeding the pericarpium citri reticulatae into an infrared plasma surface modification device, wherein the device comprises a sealed vacuum-pumping shell, an ultrasonic tank body arranged in the shell, as well as an infrared transmitting device and a plasma generating device which are arranged on the ultrasonic tank body; adding water into the ultrasonic body, adding hesperidin nanoparticles, and starting the ultrasonic device, the infrared transmitting device and the plasma generating device at a room temperature under a vacuum degree of 10-25mmHg, and performing extraction and filtration, thereby obtaining the pericarpium citri reticulatae extract. The method for preparing the pericarpium citri reticulatae extract at room temperature has the characteristics of low energy consumption, cleanness, environmental conservation and high yield.
Description
Technical field
The invention belongs to the extractive technique field of active ingredients from traditional Chinese medicinal is and in particular to Pericarpium Citri Reticulatae extract under a kind of room temperature
Preparation method.
Background technology
Chinese medicine is originating primarily from China, is to be used for preventing under instruction of Chinese Medicine theory, diagnose, treat disease or adjust human body
The medicine of function.Mostly be plant amedica, also have animal drugs, mineral drug and partly chemistry, biological drug.Processing work pressed by Chinese medicine
Skill is divided into Chinese patent medicine, Chinese crude drug.For Chinese crude drug, how efficiently to extract its effective ingredient be current study hotspot it
One.
For a long time, Chinese herbal medicine clinically is based on decocting preparation.Traditional decocting preparation extraction process is：Chinese crude drug
After harvesting, through flushing, dry, section, then add water infusion, and time-consuming, and produce substantial amounts of waste residue, medical material waste residue need through
Cross landfill disposal, be unfavorable for environmental protection.
With modern medicine in the infiltration of tcm field, success of arteannuin etc., it has been realised that traditional water
Pan-fried method, solvent supersonic extraction etc. may not be preferred plan, because during decocting, have lost many volatile oil etc.
Point, many unstable structures are also destroyed in 60 DEG C～100 DEG C of decoction process, and ultrasonic extraction will use solvent.Existing
Have in technology, also have and Effective Component of Chinese Medicine is extracted using chemical method, but exist and be unfavorable for environmental protection, high energy consumption, technological process
Long, recruitment takes the defects such as many, industrialization cost height.
In order to solve the defect of high temperature steaming extraction, also occur in that extract at room temperature technique, but existing extract at room temperature work
So that antibacterial can not be killed, there is potential safety hazard due to no high temperature steaming process in skill；And existing extract at room temperature process, have
Effect species activity is little, is difficult to be extracted in water, it usually needs adopt organic solvent extraction, adds catalyst, modifying agent etc.,
This way needs to be separated again, complex process, and can there is contaminated risk to effective ingredient, not environmentally, gives birth to
Produce high cost.
Content of the invention
It is an object of the invention to provide under a kind of room temperature Pericarpium Citri Reticulatae extract preparation method, have that its energy consumption is low, clean ring
The little feature of guarantor, high income, effective ingredient purity height, receipts pollution.
The present invention the adopted technical scheme that solves the above problems is：The preparation method of Pericarpium Citri Reticulatae extract under a kind of room temperature,
Methods described includes：
Pulverize：Pericarpium Citri Reticulatae is dried, pulverizes, put in Infrared Plasma surface modification device；Described device includes：One is airtight
The housing of vacuum-pumping, the ultrasound wave cell body being arranged in housing and be arranged at the infrared emitting on ultrasound wave cell body
Device and plasma producing apparatus；
Addition water in described ultrasonic bath body, and add the nano_scale particle of Hesperidin, temperature adopts room temperature, vacuum 10-
25mmHg, starts ultrasonic unit, infrared transmitting device and plasma producing apparatus and is extracted, filter, obtain Pericarpium Citri Reticulatae and carry
Take thing.
Further, the addition of the nano_scale particle of described Hesperidin is respectively 3-10ppm, described nano_scale particle
Particle size range is respectively 5-50nm.
The operating frequency of described ultrasonic unit is 30-50KH, and ultrasonic power is：800-1200W.
Described infrared transmitting device output current 0.3-0.6 ampere, the Infrared irradiation of 750-850nm wavelength, every point
Clock 15-25 subpulse irradiates.
The supply frequency that described plasma producing apparatus adopt is 30-50KHz, and discharge voltage is 15-25KV.
Extraction time is 3-6 hour.
Preferably：The operating frequency of described ultrasonic unit is 40KH, and ultrasonic power is：1000W；Infrared ray is sent out
0.5 ampere of injection device output current, the Infrared irradiation of 800nm wavelength, 20 subpulses per minute irradiate；Described plasma is sent out
The supply frequency that generating apparatus adopt is 40KHz, and discharge voltage is 20KV.
Waste residue after filtration, can be as bio-fuel application it is also possible to make degradable wood moulding and mulch film product after being dried
Product.
The Pericarpium Citri Reticulatae extract that this method prepares, is calculated by dry product, containing Hesperidin >=5.0%, the receipts of effective ingredient
Rate is high.
Compared with prior art, it is an advantage of the current invention that：
The application reduces pollution using airtight housing it is ensured that medicine is extracted in production under clean production environment；Take out true
Empty device, reduces the oxidized probability of medical material effective ingredient, thus improving yield.
The application passes through infra-red radiation, plasma-activated, ultrasonic wave concussion, while killing antibacterial, to active substance table
Face is modified, and increases hydrophilic, is added to the water using nano level effective ingredient simultaneously, forms the nucleus reunited so that living
Property composition be easier be extracted from medical material, adopt in whole process and use water as Extraction solvent, without other to activity
Become branch to produce the material of impact, extraction of substance purity is high, not contaminated, and due to extract at room temperature, oxidized and volatilization can
Energy property is little, and effective ingredient is farthest retained, and further increases yield, thus improving the utilization rate of Chinese crude drug.
Filtering residue after extraction can reuse, environmental clean.
Specific embodiment
With reference to embodiment, the present invention is further illustrated.
Embodiment 1
Equipment therefor：For Infrared Plasma surface modification device, it includes the housing of vacuum extractor and sealing, in housing
It is provided with ultrasound wave cell body, infrared transmitting device and plasma producing apparatus, described infrared transmitting device and plasma
Body generating meanss may be contained within the top of ultrasound wave cell body.
The preparation method of Pericarpium Citri Reticulatae extract is as follows：
（1）Pulverize：Pericarpium Citri Reticulatae puts into clean high speed disintegrator after being dried at a temperature of 70 DEG C（Equipment manufacturer：Jiangsu Dongsheng machine
Tool company limited, type is FS300 type, similarly hereinafter）, after startup, pulverize 20 seconds after take out 1kg, be added to above-mentioned infrared grade from
In the ultrasonic bath body of daughter surface modification device, in groove, put into pure water 5kg, and add the nano_scale particle of Hesperidin, described
The addition of the nano_scale particle of Hesperidin is 5ppm, and particle diameter is 10nm, and temperature adopts room temperature, vacuum 20mmHg, starts super
Acoustic wave device, infrared transmitting device and plasma producing apparatus, wherein：
The operating frequency of described ultrasonic unit is 40KH, and ultrasonic power is：1000W；
0.5 ampere of infrared transmitting device output current, the Infrared irradiation of 800nm wavelength, 20 subpulses per minute irradiate；
The supply frequency that described plasma producing apparatus adopt is 40KHz, and discharge voltage is 20KV；
After 3 hours, after 3 hours, with filter screen filtration, obtain Pericarpium Citri Reticulatae extracting solution（The quality of Pericarpium Citri Reticulatae extracting solution is 5.5Kg）（Because old
Skin water absorption, can not all by water filtration out after filtration）, after testing, in Pericarpium Citri Reticulatae extracting solution, calculate by dry product, containing Pericarpium Citri junoriss
Glycosides is 5.0%（Establishing criteria：《Chinese Pharmacopoeia》2015 editions）, that is,：The quality of the Hesperidin extracting is 1kg × 5.0%=
0.05kg.
（2）Waste residue：By step（1）Take out after gained waste residue is dried 4 hours at a temperature of 70 DEG C after filtration, can be used for firing
Material.
Comparative example 1：Use conventional methods and Pericarpium Citri Reticulatae is extracted, concrete grammar decocts for high temperature（It is old that 1Kg is dried
Skin, plus 5kg water, decoct；Filter after decoction）（100 DEG C, 5 hours）；Finally, extract obtained quality is 5kg, extracts
The quality of Hesperidin is 0.025kg.
Comparative example 2：
Comparative example 2 is differed only in embodiment 1, and in extraction process, the nanoscale being added without effective component extracting in water is micro-
Grain.
After testing, in Pericarpium Citri Reticulatae extracting solution, the quality containing Hesperidin is 0.023kg.
Embodiment 2
Method is as follows：
（1）Pulverize：Clean high speed disintegrator is put into, after startup, after pulverizing 20 seconds after Pericarpium Citri Reticulatae is dried at a temperature of 70 DEG C
Take out 1kg, be added to Infrared Plasma surface modification device, put into pure water 5Kg in instrument, be simultaneously introduced Hesperidin
Nano_scale particle, particle diameter is 20nm, and the addition of the nano_scale particle of described Hesperidin is 4ppm, and temperature adopts room temperature, vacuum
Degree 20mmHg, starts activation, after 3.5 hours, with filter screen filtration, obtains Pericarpium Citri Reticulatae extract, after testing, in Pericarpium Citri Reticulatae extracting solution, contain
Hesperidin 0.06kg.
（2）Waste residue：By step（1）Take out after gained waste residue is dried 4 hours at a temperature of 70 DEG C after filtration, can be used for firing
Material.
The other the same as in Example 1.
Embodiment 3
Method is as follows：
（1）Pulverize：Clean high speed disintegrator is put into after Pericarpium Citri Reticulatae is dried at a temperature of 70 DEG C（Equipment manufacturer：Jiangsu Dongsheng
Machinery Co., Ltd., type is FS300 type）, after startup, take out 1kg after pulverizing 20 seconds, be added to Infrared Plasma table
Surface modifying device, puts into pure water 5Kg in instrument, be simultaneously introduced the nano_scale particle of Hesperidin, and the nanoscale of described Hesperidin is micro-
The addition of grain is 5ppm, and particle diameter is 50nm, and temperature adopts room temperature, vacuum 20mmHg, starts activation, after 4 hours, with filtering
Net filtration, obtains Pericarpium Citri Reticulatae extract, after testing, in Pericarpium Citri Reticulatae extracting solution, 0.07kg containing Hesperidin.
（2）Waste residue：By step（1）Filter after gained waste residue is dried 4 hours at a temperature of 70 DEG C and take out, can be used for fuel.
The other the same as in Example 1.
Embodiment 4
Preparation method is 4.5 hours with embodiment 1, except for the difference that activationary time, gained Pericarpium Citri Reticulatae extract, and after testing, Pericarpium Citri Reticulatae carries
Take in liquid, 0.08kg containing Hesperidin.
Embodiment 5
Preparation method is 5 hours with embodiment 1, except for the difference that activationary time, gained Pericarpium Citri Reticulatae extract, and after testing, Pericarpium Citri Reticulatae extracts
In liquid, 0.086kg containing Hesperidin.
Embodiment 6
Preparation method is 5.5 hours with embodiment 1, except for the difference that activationary time, gained Pericarpium Citri Reticulatae extract, and after testing, Pericarpium Citri Reticulatae carries
Take in liquid, 0.089kg containing Hesperidin.
Comparative example 3：
Comparative example 3 is differed only in embodiment 6, in extraction process, is added without the nano_scale particle of Hesperidin in water.
After testing, in Rhizoma Coptidis extract, calculate by dry product, the quality of Hesperidin is 0.028kg.
Comparative example 4：
Comparative example 4 is differed only in embodiment 6, is not turned on plasma producing apparatus.
After testing, in Rhizoma Coptidis extract, calculate by dry product, the quality of Hesperidin is 0.027kg.
Comparative example 5：
Comparative example 5 is differed only in embodiment 6, is not turned on plasma producing apparatus and infrared transmitting device.
After testing, in Rhizoma Coptidis extract, calculate by dry product, the quality of Hesperidin is 0.026kg.
In addition to the implementation, present invention additionally comprises there being other embodiment, all employing equivalents or equivalence replacement
The technical scheme that mode is formed, all should fall within the scope of the hereto appended claims.
Claims (9)
1. under a kind of room temperature Pericarpium Citri Reticulatae extract preparation method it is characterised in that：Methods described includes：
Pericarpium Citri Reticulatae is dried, pulverizes, put in Infrared Plasma surface modification device；Described device includes：One airtight can
The housing of evacuation, the ultrasound wave cell body being arranged in housing and be arranged at the infrared transmitting device on ultrasound wave cell body
And plasma producing apparatus；
Addition water in described ultrasonic bath body, and add the nano_scale particle of Hesperidin, temperature adopts room temperature, vacuum 10-
25mmHg, starts ultrasonic unit, infrared transmitting device and plasma producing apparatus, is extracted, and filters, obtains Pericarpium Citri Reticulatae and carry
Take thing.
2. under a kind of room temperature according to claim 1 Pericarpium Citri Reticulatae extract preparation method it is characterised in that：Described Hesperidin
Nano_scale particle addition be 3-10ppm.
3. under a kind of room temperature according to claim 1 Pericarpium Citri Reticulatae extract preparation method it is characterised in that：Described ultrasound wave
The operating frequency of device is 30-50KH, and ultrasonic power is：800-1200W.
4. under a kind of room temperature according to claim 1 Pericarpium Citri Reticulatae extract preparation method it is characterised in that：Infrared emitting
Device output current 0.3-0.6 ampere, the Infrared irradiation of 750-850nm wavelength, 15-25 subpulse per minute irradiates.
5. under a kind of room temperature according to claim 1 Pericarpium Citri Reticulatae extract preparation method it is characterised in that：Described plasma
The supply frequency that body generating meanss adopt is 30-50KHz, and discharge voltage is 15-25KV.
6. under a kind of room temperature according to claim 1 Pericarpium Citri Reticulatae extract preparation method it is characterised in that：Extraction time is
3-6 hour.
7. under a kind of room temperature according to claim 1 Pericarpium Citri Reticulatae extract preparation method it is characterised in that：Described ultrasound wave
The operating frequency of device is 40KH, and ultrasonic power is：1000W；0.5 ampere of infrared transmitting device output current, 800nm ripple
Long Infrared irradiation, 20 subpulses per minute irradiate；The supply frequency that described plasma producing apparatus adopt is 40KHz,
Discharge voltage is 20KV.
8. under a kind of room temperature according to claim 1 Pericarpium Citri Reticulatae extract preparation method it is characterised in that：Gained after filtration
After waste residue is dried at a temperature of 60-80 DEG C, for as fuel or as building materials raw material.
9. under a kind of room temperature according to claim 1 Pericarpium Citri Reticulatae extract preparation method it is characterised in that：Described nanoscale
The particle size range of microgranule is 5-50nm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610855123.2A CN106389604A (en) | 2016-09-28 | 2016-09-28 | Method for preparing pericarpium citri reticulatae extract at room temperature |
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| CN201610855123.2A CN106389604A (en) | 2016-09-28 | 2016-09-28 | Method for preparing pericarpium citri reticulatae extract at room temperature |
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| CN201610855123.2A Pending CN106389604A (en) | 2016-09-28 | 2016-09-28 | Method for preparing pericarpium citri reticulatae extract at room temperature |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107224749A (en) * | 2017-06-22 | 2017-10-03 | 杨勇 | A kind of filter of compound chrysanthemum tea |
| CN107930182A (en) * | 2017-12-29 | 2018-04-20 | 内蒙古金旭生物科技有限公司 | A kind of active substance of plant extraction element |
-
2016
- 2016-09-28 CN CN201610855123.2A patent/CN106389604A/en active Pending
Non-Patent Citations (3)
| Title |
|---|
| 周志坚: "《大学物理教程》", 30 January 2015 * |
| 朱思明等: ""陈皮中橙皮苷的超声法提取与结晶"", 《食品工业科技》 * |
| 王琛 等: "《高分子材料改性技术》", 30 April 2007 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107224749A (en) * | 2017-06-22 | 2017-10-03 | 杨勇 | A kind of filter of compound chrysanthemum tea |
| CN107930182A (en) * | 2017-12-29 | 2018-04-20 | 内蒙古金旭生物科技有限公司 | A kind of active substance of plant extraction element |
| CN107930182B (en) * | 2017-12-29 | 2024-05-24 | 山西鑫旭生物科技有限公司 | Plant active substance extraction element |
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Application publication date: 20170215 |