CN108079038B - Supercritical-based method for preparative separation of blumea balsamifera leaf blumea balsamifera tablets - Google Patents
Supercritical-based method for preparative separation of blumea balsamifera leaf blumea balsamifera tablets Download PDFInfo
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- CN108079038B CN108079038B CN201711408355.4A CN201711408355A CN108079038B CN 108079038 B CN108079038 B CN 108079038B CN 201711408355 A CN201711408355 A CN 201711408355A CN 108079038 B CN108079038 B CN 108079038B
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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)
- A61K36/28—Asteraceae or Compositae (Aster or Sunflower family), e.g. chamomile, feverfew, yarrow or echinacea
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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
- A61K2236/37—Extraction at elevated pressure or temperature, e.g. pressurized solvent extraction [PSE], supercritical carbon dioxide extraction or subcritical water extraction
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Abstract
The invention discloses a method for extracting blumea balsamifera tablets from blumea balsamifera leaves, which comprises the following steps: crushing fresh blumea balsamifera leaves into an extraction raw material, and filling the extraction raw material into a supercritical extraction kettle to be fully mixed with glass beads for extraction. The extraction temperature is 15-35 ℃, and CO is2Fluid pressure 25-35MPa, CO2The flow rate is 13-26L.h‑1And (4) extracting for 15-30min, and cooling and crystallizing the extract to obtain coarse mugwort tablet crystals. The research of the invention shows that the product yield and purity are improved by the supercritical extraction method compared with the prior art, the repeatability is good, the operation is convenient and quick, the safety is high, the energy is saved, the emission is reduced, and the method is suitable for industrial production.
Description
Technical Field
The invention relates to a traditional Chinese medicine extraction method, in particular to a high-efficiency preparation and separation technology of blumea balsamifera tablets, and particularly relates to a supercritical preparation and separation method of blumea balsamifera tablets in blumea balsamifera leaves.
Background
The blumea balsamifera (L.) DC is crystal prepared by extracting fresh leaves of Blumeabalsamiera (L.) DC of Compositae. Mainly distributed in south China, Fujian, Taiwan, Guizhou, Yunnan and other places. The moxa tablet has the effects of inducing resuscitation, refreshing mind, clearing heat and relieving pain. It is commonly used for coma, convulsion, apoplexy with phlegm syncope, sudden syncope due to qi depression, coma, conjunctival congestion, aphtha, sore throat and purulence in ear canal. The main component of the blumea balsamifera tablet is levo-borneol which has the functions of bacteriostasis, anti-inflammation, anti-thrombosis and the like, and can also regulate central nerve and protect brain tissues. The extraction and preparation yield of the L-borneol is small all the time.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a method for preparative separation of blumea balsamifera tablets in blumea balsamifera branches and leaves, which is simple in extraction method and high in recovery rate and purity and is based on supercritical extraction.
The technical scheme adopted by the invention for solving the technical problems is as follows: a method for preparative separation of blumea balsamifera tablets in blumea balsamifera branches and leaves based on supercritical extraction comprises the following steps:
a, crushing fresh blumea balsamifera leaves to serve as an extraction raw material, and filling the extraction raw material into a supercritical extraction kettle to be fully mixed with glass beads;
b, extraction conditions are as follows: the extraction temperature is 15-35 deg.C, and CO is added2Fluid pressure 25-35MPa, CO2The flow rate is 13-26L.h-1Then, the extraction time is 15-30 min.
c, collecting the extract, cooling and crystallizing to obtain the blumea balsamifera tablets.
Among these, the preferred extraction conditions are: temperature 25 ℃ CO2Fluid pressure 30MPa, CO2Flow rate of 20L.h-1And extracting for 20min to obtain an extract.
Compared with the prior art, the method for preparative separation of blumea balsamifera leaves based on supercritical extraction has the advantages that fresh blumea balsamifera leaves are crushed into extraction raw materials, and the extraction raw materials are filled into a supercritical extraction kettle to be fully mixed with glass beads for extraction. The extraction temperature is 15-35 ℃, and CO is2Fluid pressure 25-35MPa, CO2The flow rate is 13-26L.h-1And (4) extracting for 15-30min, and cooling and crystallizing the extract to obtain blumea balsamifera crystals. The method has simple process, and the folium Artemisiae Argyi extract rate is about 65-70% and the purity is about 60-65%.
The extraction method is obtained by screening, and the screening process is as follows:
the invention respectively uses dry blumea balsamifera leaves and fresh blumea balsamifera leaves which are crushed into extraction raw materials, the extraction raw materials of the dry blumea balsamifera leaves are directly put into a supercritical extraction kettle for extraction, the extraction raw materials of the fresh blumea balsamifera leaves are fully mixed with glass beads and then put into the supercritical extraction kettle for extraction, and the extraction conditions are screened as follows:
comparing the extraction rates, finding that the content difference between the dried blumea balsamifera leaves and the fresh blumea balsamifera leaves after crushing is large, and adopting the fresh blumea balsamifera leaves mixed with glass beads for extraction in order to prevent the fresh blumea balsamifera leaves from being bonded, wherein CO is used in the extraction process2Fluid pressure being the main influencing factor, CO2The flow rate is a secondary influence, and the extraction conditions are screened out.
Compared with the prior art, the extraction method of the invention has the following advantages:
Detailed Description
The present invention will be described in further detail with reference to examples.
Example 1
Crushing fresh blumea balsamifera leaves as an extraction raw material, weighing 500g, and putting into a supercritical extraction kettle to be fully mixed with glass beads. At an extraction pressure of 30MPa, a temperature of 20 ℃ and CO2Flow rate of 15L.h-1And obtaining the semitransparent crystal blumea balsamifera extract extracted from fresh blumea balsamifera leaves for 15 min. The purity of the extract was 57.69%, and the extraction rate was 63.34%.
Example 2
Essentially the same as in example 1, except that the CO concentration was adjusted at an extraction pressure of 27MPa, a temperature of 30 ℃ and2flow rate of 20L.h-1And the extraction is obtained under the condition of 20 min. The purity of the extract was 59.31%, and the extraction rate was 64.62%.
Example 3
Essentially the same as in example 1, except that the CO concentration was adjusted at an extraction pressure of 33MPa, a temperature of 35 ℃ and2flow rate of 15L.h-1And the extract is obtained under the condition of 25 min. The purity of the extract was 64.01% and the extraction rate was 68.45%.
Example 4
Essentially the same as in example 1, except that CO was added at an extraction pressure of 30MPa, a temperature of 25 ℃ and2flow rate 20L.h-1And the extraction is obtained under the condition of 20 min. The purity of the extract was 65.12% and the extraction rate was 70.23%.
Example 5
Essentially the same as in example 1, except that the CO concentration was adjusted at an extraction pressure of 33MPa, a temperature of 18 ℃ and2flow 16L.h-1And the extraction is obtained under the condition of 15 min. The purity of the extract was 59.82%, and the extraction rate was 64.85%.
Example 6
Essentially the same as in example 1, except that the CO concentration was adjusted at an extraction pressure of 20MPa, a temperature of 30 ℃ and2flow rate of 20L.h-1And the extract is obtained under the condition of 25 min. The purity of the extract was 63.41% and the extraction rate was 62.11%.
The purity of the blumea balsamifera tablets in the blumea balsamifera leaf extract is measured according to a content measuring method of the blumea balsamifera tablets (L-borneol) in the 'Chinese pharmacopoeia' of 2015 edition. According to the determination of gas chromatography, the chromatographic column is a polyethylene glycol 20000(PEG-20M) capillary column (the column length is 30M, the inner diameter is 0.53mm, the membrane thickness is 1.0 μ M), the FID detector is used, the detector temperature is 200 ℃, the column temperature is 170 ℃, the sample injection amount is 1 μ l, the standard substance external standard method is quantitative, the purity of the blumea balsamifera leaf extract is about 60-65%, and the main component is L-borneol. The calculation formula of the productive rate theta of the blumea balsamifera (L-borneol) is as follows:
wherein: m 1-quality of levo-borneol crystal product
m2 mass of L-borneol in blumea balsamifera leaf before extraction
The method provided by the invention can be used for better improving the product yield and purity of the blumea balsamifera tablets, is convenient and rapid to operate, high in safety, energy-saving and emission-reducing, and is suitable for industrial production.
Claims (1)
1. A preparation method of blumea balsamifera leaf blumea tablets is characterized by comprising the following steps: comprises the following steps: pulverizing fresh folium Blumeae Balsamiferae into raw material, placing the raw material into supercritical extraction kettle, mixing with glass beads, extracting, collecting extractive solution and residue respectively, cooling extractive solution, crystallizing to obtain folium Blumeae Balsamiferae tablet,
wherein, supercritical CO2The extraction conditions were: temperature 25 ℃ CO2Fluid pressure 30MPa, CO2Flow rate of 20L.h-1And the extraction time is 20 min.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106266133A (en) * | 2016-09-18 | 2017-01-04 | 厦门市香妃美业化妆品有限公司 | Miao Ethnomedicine preparation tightening pubococcygeus and preparation method thereof |
| WO2017173611A1 (en) * | 2016-04-07 | 2017-10-12 | 北京路德凯奇商贸有限责任公司 | Pharmaceutical product for treating tumor and combined immune defect, and preparation and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2017173611A1 (en) * | 2016-04-07 | 2017-10-12 | 北京路德凯奇商贸有限责任公司 | Pharmaceutical product for treating tumor and combined immune defect, and preparation and application thereof |
| CN106266133A (en) * | 2016-09-18 | 2017-01-04 | 厦门市香妃美业化妆品有限公司 | Miao Ethnomedicine preparation tightening pubococcygeus and preparation method thereof |
Non-Patent Citations (1)
| Title |
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| 滇桂艾纳香超临界萃取物成分分析及在卷烟中的应用;董伟;《食品工业》;20091231(第02期);55-56 * |
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Address after: 214028 Changjiang South Road, new Wu District, Wuxi, Jiangsu Province, No. 12 Co-patentee after: JINGXI JIMIN KEXIN GROUP Co.,Ltd. Patentee after: Wuxi Jiyu Shanhe Pharmaceutical Co., Ltd Address before: 214028 No. 12 Changjiang South Road, New District, Jiangsu, Wuxi Co-patentee before: JINGXI JIMIN KEXIN GROUP Co.,Ltd. Patentee before: WUXI JIMIN KEXIN SHANHE PHARMACEUTICAL Co.,Ltd. |
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