CN103705577A - Antipyretic cold tablet crude drug volatile oil and extraction method thereof - Google Patents
Antipyretic cold tablet crude drug volatile oil and extraction method thereof Download PDFInfo
- Publication number
- CN103705577A CN103705577A CN201310746444.5A CN201310746444A CN103705577A CN 103705577 A CN103705577 A CN 103705577A CN 201310746444 A CN201310746444 A CN 201310746444A CN 103705577 A CN103705577 A CN 103705577A
- Authority
- CN
- China
- Prior art keywords
- peaks
- volatile oil
- retention time
- extraction
- temperature
- 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
Links
Images
Landscapes
- Extraction Or Liquid Replacement (AREA)
Abstract
The invention provides an extraction method of antipyretic cold tablet crude drug volatile oil. The antipyretic cold tablet crude drug volatile oil is extracted through a carbon dioxide supercritical extraction method. The extraction method particularly comprises the following steps: (1) taking schizonepeta spike and mint as crude drugs in percentage by weight of (40-60):(65-85); (2) crushing the crude drugs, placing in a carbon dioxide supercritical extraction kettle, extracting at the extraction pressure of 20-35 MPa, the extraction temperature of 40-50 DEG C and the delivery pump modulation frequency of 34 hertz for 1-4 hours, and drying under reduced pressure at the precipitating pressure of 5.2 MPa and the precipitating temperature of 45 DEG C to obtain the volatile oil. According to the invention, an optimal process for effectively extracting mint and schizonepeta spike volatile oil simultaneously is finally obtained by integrally surveying multiple parameters of a supercritical extraction process; the yield of the volatile oil is obviously superior to that under other process conditions at special parameters of the process; meanwhile, the process is relatively low in energy consumption and more saved in production cost, thereby providing a new intermediate extraction method for the production of an antipyretic cold tablet.
Description
Technical field
The present invention relates to antipyretic common cold tablet crude drug volatile oil and extracting method thereof.
Background technology
Antipyretic common cold tablet, original prescription is: Herba Schizonepetae 50g, Radix Saposhnikoviae 75g, Radix Angelicae Dahuricae 50g, Radix Bupleuri 50g, Radix Puerariae 125g, Herba Menthae 75g, Herba Taraxaci 100g, Radix Isatidis 125g, Herba Corydalis Bungeanae 100g, Radix Scutellariae 200g, Rhizoma Phragmitis 100g, Radix Scrophulariae 100g, Semen Armeniacae Amarum 75g, Radix Glycyrrhizae 50g.This medicine can clearing away heat and expelling pathogen in the exterior, the headache causing for affection of exogenous wind-cold, and nasal obstruction watery nasal discharge, fever is afraid of cold, cough hoarseness, pharyngodynia with dryness.
In the crude drug of antipyretic common cold tablet, Herba Schizonepetae, Herba Menthae are rich in volatile compound, in current extracting method, first two taste medical materials are adopted to extraction by steam distillation volatile oil, with medicinal residues decocting in water together with other medical materials, extract other active ingredient again, to avoid the loss of volatile ingredient.Before preparation, its volatile oil intermediate is fully mixed with other intermediate, make crude drug, finally make tablet.
Yet there are no the report that adopts carbon dioxide supercritical extraction method simultaneously to extract Herba Menthae and Herba Schizonepetae volatile oil.
Summary of the invention
The object of the present invention is to provide antipyretic common cold tablet crude drug volatile oil and extracting method thereof.The present invention is by Herba Menthae and Herba Schizonepetae while mixed extraction volatile oil, because the chemical composition containing in medical material after mixing is more complicated, and the plant structure of Herba Menthae and Herba Schizonepetae is not identical yet, in leaching process, the physics that may exist between osmotic pressure or chemical composition, chemical effect, may affect the extraction effect of two kinds of medical materials.For a kind of volatile oil mixed extraction method that can industrialized great production is provided, the present invention is studied both mixed extraction processes:
The extracting method that the invention provides antipyretic common cold tablet crude drug volatile oil, it is extracted by carbon dioxide supercritical fluid extraction method, and concrete operation step is as follows:
(1) get the crude drug of following weight proportion: Herba Schizonepetae: Herba Menthae=(40-60): (65-85);
(2) crude drug is pulverized, be placed in carbon dioxide supercritical fluid extraction still, at extracting pressure 20～35MPa, 40～50 ℃ of extraction temperature, 34 hertz of delivery pump frequency modulation, extraction 1～4h, after having extracted, again through resolving 1～3 time, resolve pressure 5.2MPa, 45 ℃ of resolution temperatures, drying under reduced pressure, obtains volatile oil.
Further, in step (1), Herba Schizonepetae: Herba Menthae=50:75.
Further, in step (2), extracting pressure 30～32MPa, 45～47 ℃ of extraction temperature, extraction 3～3.5h; Resolve 1 time.
Further, in step (2), extracting pressure 30MPa, 45 ℃ of extraction temperature, extraction 3h.
The volatile oil that the present invention also provides said extracted method to prepare, described volatile oil detects through gas chromatography mass spectrometry technology, contains 18 principal character peaks in its chromatogram, is respectively:
No. 1 peak, retention time is 3.07 ± 0.05min; No. 2 peaks, retention time is 3.18 ± 0.05min; No. 3 peaks, retention time is 3.5 ± 0.1min; No. 4 peaks, retention time is 5.6 ± 0.1min; No. 5 peaks, retention time is 8.9 ± 0.1min; No. 6 peaks, retention time is 9.2 ± 0.1min; No. 7 peaks, retention time is 11.3 ± 0.1min; No. 8 peaks, retention time is 12.4 ± 0.1min; No. 9 peaks, retention time is 12.7 ± 0.1min; No. 10 peaks, retention time is 13.2 ± 0.1min; No. 11 peaks, retention time is 15.5 ± 0.1min; No. 12 peaks, retention time is 15.5 ± 0.1min; No. 13 peaks, retention time is 19.6 ± 0.1min; No. 14 peaks, retention time is 24.1 ± 0.1min; No. 15 peaks, retention time is 27.2 ± 0.1min; No. 16 peaks, retention time is 29.3 ± 0.1min; No. 17 peaks, retention time is 29.7 ± 0.1min; No. 18 peaks, retention time is 31.1 ± 0.1min;
Wherein, detection method concrete operations are as follows:
(1) get volatile oil, prepare need testing solution;
(2) by need testing solution inject gas chromatograph, detect, chromatographic condition is as follows:
Chromatographic column: quartz capillary column;
Injector temperature: 270 ℃;
Heating schedule: 80 ℃ of maintenance 3min of initial column temperature, are warming up to 105 ℃ with 10 ℃/min and keep 20min, then be warming up to 230 ℃ with 15 ℃/min;
Helium flow velocity: 1ml/min;
Split ratio: 20:1;
Mass Spectrometer Method: electron bombardment ionization source, ionizing energy is 70eV, sweep limits 35-400amu.
Further, in described chromatogram, the peak area at each principal character peak accounts for total peak area percentage ratio and is:
No. 1 peak is 5.0-7.0%; No. 2 peaks are 15.0-18.5%, and No. 3 peaks are 4.5-6.0; No. 4 peaks are 0.3-1.2%; No. 5 peaks are 17.0-23.0%, and No. 6 peaks are 0.5-0.9%; No. 7 peaks are 0.5-0.7%; No. 8 peaks are 16.0-19.5; No. 9 peaks are 8.0-11.5%; No. 10 peaks are 1.3-1.7%; No. 11 peaks are 1.7-2.7%; No. 12 peaks are 0.5-0.7%; No. 13 peaks are 1.2-1.5%; No. 14 peaks are 0.5-1.0%; No. 15 peaks are 3.0-4.2%; No. 16 peaks are 2.2-3.3%; No. 17 peaks are 2.5-3.3%; No. 18 peaks are 2.3-3.1%.
Further, chromatograph and mass spectrometer interface temperature: 250 ℃; Ion source temperature: 250 ℃.
Further, in Mass Spectrometer Method, solvent delay 3min.
Further, described quartz capillary column packing is 5% phenyl/95% methyl polysiloxane.
Further, in step (1), need testing solution solvent for use is ethyl acetate.
The present invention is by the integrated survey to supercritical extraction process many kinds of parameters, finally obtained effectively extracting the optimised process of Herba Menthae and Herba Schizonepetae volatile oil simultaneously, under the special parameter of this technique, volatile oil yield is significantly better than other process conditions, simultaneously, this process energy consumption is lower, comparatively saves production cost, and for antipyretic common cold tablet, produces new intermediate extracting method is provided.
Accompanying drawing explanation
The detection collection of illustrative plates of Fig. 1 volatile oil intermediate of the present invention (sample A)
The detection collection of illustrative plates of Fig. 2 volatile oil intermediate of the present invention (sample B)
The detection collection of illustrative plates of Fig. 3 volatile oil intermediate of the present invention (sample C)
The specific embodiment
The supercritical extraction instrument using in the present invention, purchased from Guangzhou Mei Chen company, is 2L supercritical extraction instrument.Certainly, as long as under identical extraction principle, use other supercritical extraction instrument also can reach effect of the present invention.
Embodiment 1 extracting method of the present invention
Take Herba Menthae 300g, Herba Schizonepetae 200g after pulverizing, mix homogeneously, is placed in carbon dioxide supercritical fluid extraction still, at extracting pressure 30MPa, 45 ℃ of extraction temperature, 34 hertz of delivery pump frequency modulation, extraction 3h, then resolve once, resolve pressure 5.2MPa, 45 ℃ of resolution temperatures, resolve thing through drying under reduced pressure, obtain volatile oil.
In the present invention, select 45 ℃ as resolution temperature, it is the minimum temperature that can make carbon dioxide separated with volatile oil.
The screening of embodiment 2 supercritical extraction process of the present invention
1 reagent
Analytical pure ethyl acetate (Tianjin all generations), industrial CO2(Guangzhou Gas Factory)
2 instruments
DSQ II gas chromatograph-mass spectrometer (GC-MS) (U.S. match Mo Feishier company), Rotary Evaporators (Japanese Shimadzu company), 2L supercritical extraction instrument (Guangzhou Mei Chen company).
3 methods
3.1 extracting method optimizations
Get a certain amount of Herba Menthae and Herba Schizonepetae medical material, after pulverizing, cross 40 mesh sieves.Take the medical material after pulverizing, Herba Menthae 300g, Herba Schizonepetae 200g, mix homogeneously, pack extraction kettle into, resolving under 34 hertz of pressure 5.2MPa, 45 ℃ of resolution temperatures, delivery pump frequency modulation, by table 1 condition, extract, collect extract precise weighing, calculate extraction ratio and analyze and optimize optimised process.Below the investigation test of each set condition, all according to embodiment 1 flow operations.
The different extraction conditions sample of table 1 yield
Yield=extract weight/inventory * 100%
Known according to the above results, condition 12 extraction ratios of the present invention are up to 5.06%, are secondly the extraction ratio 4.98% of condition 10, and both extraction ratios are all higher, are obviously better than other each groups; Yet, in condition 12, extraction temperature, extracting pressure and extraction time are all higher than condition 10, but both extraction ratio there was no significant differences, therefore, the parameter of optimum condition 10 of the present invention, that is: extracting pressure 30MPa, 45 ℃ of extraction temperature, resolve pressure 5.2MPa, 45 ℃ of resolution temperatures, extraction time 3h, 34 hertz of delivery pump frequency modulation.
Whether reasonable for verifying above-mentioned condition, the present invention repeats to extract 2 times by this condition, and result is as follows:
Table 2 repeats to extract sample yield
The detection of embodiment 3 volatile oil
1. need testing solution preparation
Get respectively 3 batches of volatile oil intermediate (embodiment 1 preparation), with crossing 0.22 μ m filter membrane after acetic acid ethyl dissolution, obtain need testing solution.
2, analytical method
Chromatographic column: DB-5MS quartz capillary column [30m * 0.25mm * 0.25um]; Injector temperature: 270 ℃; Heating schedule: 80 ℃ of initial column temperatures, keep 3min, with 10 ℃/min, be warming up to 105 ℃ and keep 20min, then be warming up to 230 ℃ with 15 ℃/min; Carrier gas: high-pure helium, flow velocity 1ml/min; Input mode: split sampling; Split ratio: 20:1; Sample size: 1ul.Chromatograph and mass spectrometer interface temperature: 250 ℃; Ionization mode: electron bombardment ionization source; Monitoring mode: full scan; Sweep limits: 35-400; Ionizing energy: 70eV; Solvent delay: 3min; Ion source temperature: 250 ℃; Spectrum storehouse: INST2005.
Get need testing solution, by above-mentioned gas chromatography mass spectrometry methods analyst.
3, testing result
3 batches of volatile oil intermediate are detected, and in gained chromatogram, main chromatographic peak information sees the following form and Fig. 1～3:
Table 4 three batch sample main peaks retention times (min)
As can be seen from the table, repeat to extract the main component of 3 times and there is no large difference.
Table 5 three batch sample main peaks peak areas account for total peak area percentage ratio (%)
From above-mentioned experiment content, in the chromatogram of different batches volatile oil intermediate, there are 18 total principal character peaks.
In sum, the present invention is by the integrated survey to supercritical extraction process many kinds of parameters, finally obtained effectively extracting the optimised process of Herba Menthae and Herba Schizonepetae volatile oil simultaneously, under the special parameter of this technique, volatile oil yield is significantly better than other process conditions, and meanwhile, this process energy consumption is lower, comparatively save production cost, for antipyretic common cold tablet, produce new intermediate extracting method is provided.
Claims (10)
1. the extracting method of antipyretic common cold tablet crude drug volatile oil, is characterized in that: it is extracted by carbon dioxide supercritical fluid extraction method, and concrete operation step is as follows:
(1) get the crude drug of following weight proportion: Herba Schizonepetae: Herba Menthae=(40-60): (65-85);
(2) crude drug is pulverized, be placed in carbon dioxide supercritical fluid extraction still, at extracting pressure 20～35MPa, 40～50 ℃ of extraction temperature, 34 hertz of delivery pump frequency modulation, extraction 1～4h, after having extracted, again through resolving 1～3 time, resolve pressure 5.2MPa, 45 ℃ of resolution temperatures, drying under reduced pressure, obtains volatile oil.
2. extracting method according to claim 1, is characterized in that: in step (1), and Herba Schizonepetae: Herba Menthae=50:75.
3. extracting method according to claim 1, is characterized in that: in step (2), and extracting pressure 30～32MPa, 45～47 ℃ of extraction temperature, extraction 3～3.5h; Resolve 1 time.
4. extracting method according to claim 3, is characterized in that: in step (2), and extracting pressure 30MPa, 45 ℃ of extraction temperature, extraction 3h.
5. the volatile oil that described in claim 1～4 any one prepared by extracting method, is characterized in that: described volatile oil detects through gas chromatography mass spectrometry technology, contains 18 principal character peaks in its chromatogram, is respectively:
No. 1 peak, retention time is 3.07 ± 0.05min; No. 2 peaks, retention time is 3.18 ± 0.05min; No. 3 peaks, retention time is 3.5 ± 0.1min; No. 4 peaks, retention time is 5.6 ± 0.1min; No. 5 peaks, retention time is 8.9 ± 0.1min; No. 6 peaks, retention time is 9.2 ± 0.1min; No. 7 peaks, retention time is 11.3 ± 0.1min; No. 8 peaks, retention time is 12.4 ± 0.1min; No. 9 peaks, retention time is 12.7 ± 0.1min; No. 10 peaks, retention time is 13.2 ± 0.1min; No. 11 peaks, retention time is 15.5 ± 0.1min; No. 12 peaks, retention time is 15.5 ± 0.1min; No. 13 peaks, retention time is 19.6 ± 0.1min; No. 14 peaks, retention time is 24.1 ± 0.1min; No. 15 peaks, retention time is 27.2 ± 0.1min; No. 16 peaks, retention time is 29.3 ± 0.1min; No. 17 peaks, retention time is 29.7 ± 0.1min; No. 18 peaks, retention time is 31.1 ± 0.1min;
Wherein, detection method concrete operations are as follows:
(1) get volatile oil, prepare need testing solution;
(2) by need testing solution inject gas chromatograph, detect, chromatographic condition is as follows:
Chromatographic column: quartz capillary column;
Injector temperature: 270 ℃;
Heating schedule: 80 ℃ of maintenance 3min of initial column temperature, are warming up to 105 ℃ with 10 ℃/min and keep 20min, then be warming up to 230 ℃ with 15 ℃/min;
Helium flow velocity: 1ml/min;
Split ratio: 20:1;
Mass Spectrometer Method: electron bombardment ionization source, ionizing energy is 70eV, sweep limits 35-400amu.
6. volatile oil according to claim 5, is characterized in that: in described chromatogram, the peak area at each principal character peak accounts for total peak area percentage ratio and is:
No. 1 peak is 5.0-7.0%; No. 2 peaks are 15.0-18.5%, and No. 3 peaks are 4.5-6.0; No. 4 peaks are 0.3-1.2%; No. 5 peaks are 17.0-23.0%, and No. 6 peaks are 0.5-0.9%; No. 7 peaks are 0.5-0.7%; No. 8 peaks are 16.0-19.5; No. 9 peaks are 8.0-11.5%; No. 10 peaks are 1.3-1.7%; No. 11 peaks are 1.7-2.7%; No. 12 peaks are 0.5-0.7%; No. 13 peaks are 1.2-1.5%; No. 14 peaks are 0.5-1.0%; No. 15 peaks are 3.0-4.2%; No. 16 peaks are 2.2-3.3%; No. 17 peaks are 2.5-3.3%; No. 18 peaks are 2.3-3.1%.
7. volatile oil according to claim 5, is characterized in that: chromatograph and mass spectrometer interface temperature: 250 ℃; Ion source temperature: 250 ℃.
8. volatile oil according to claim 5, is characterized in that: in Mass Spectrometer Method, and solvent delay 3min.
9. volatile oil according to claim 5, is characterized in that: described quartz capillary column packing is 5% phenyl/95% methyl polysiloxane.
10. volatile oil according to claim 5, is characterized in that: in step (1), need testing solution solvent for use is ethyl acetate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310746444.5A CN103705577A (en) | 2013-12-30 | 2013-12-30 | Antipyretic cold tablet crude drug volatile oil and extraction method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310746444.5A CN103705577A (en) | 2013-12-30 | 2013-12-30 | Antipyretic cold tablet crude drug volatile oil and extraction method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103705577A true CN103705577A (en) | 2014-04-09 |
Family
ID=50399164
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310746444.5A Pending CN103705577A (en) | 2013-12-30 | 2013-12-30 | Antipyretic cold tablet crude drug volatile oil and extraction method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103705577A (en) |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102988479A (en) * | 2012-10-08 | 2013-03-27 | 卞毓平 | Preparation method and application of anti-dazzling tablet |
-
2013
- 2013-12-30 CN CN201310746444.5A patent/CN103705577A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102988479A (en) * | 2012-10-08 | 2013-03-27 | 卞毓平 | Preparation method and application of anti-dazzling tablet |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102973667B (en) | Preparation method and application of cold-fever tablet | |
| Deng et al. | Recent developments in sample preparation techniques for chromatography analysis of traditional Chinese medicines | |
| CN102988667B (en) | Preparation method and application of tablet for regulating menstruation and activating blood | |
| CN103789094A (en) | Method for extracting agilawood essential oil from agilawood chips | |
| CN103207255B (en) | A kind of detection method of content of NAOXINTONG JIAONANG | |
| CN104997840A (en) | Dracocephalum heterophyllum Benth pentacyclic triterpene component sample pretreatment method and use of Dracocephalum heterophyllum Benth pentacyclic triterpene component | |
| CN101709028B (en) | Method for extracting and separating curdione from oil of zedoary turmeric | |
| CN102988489B (en) | Preparation method and application of nose comforting tablet | |
| CN108120779B (en) | Analysis method for rapidly identifying chemical components in curcuma kwangsiensis | |
| CN108409808A (en) | A kind of method of the broken extraction Gastrodin in Gastrodia eleta Bl. of continuous low-temperature high pressure | |
| CN103705577A (en) | Antipyretic cold tablet crude drug volatile oil and extraction method thereof | |
| CN102836256A (en) | Preparation method for baipuhuang tablet (traditional Chinese medicine tablet) | |
| US20100303974A1 (en) | Method of preparing an extract from multiple botanic herbs by an ultrasonic way under a low temperature | |
| CN102988479B (en) | Preparation method and application of anti-dazzling tablet | |
| CN104447778A (en) | Preparation method of vomicine | |
| CN101973861A (en) | Method for preparing germacrone | |
| CN104922513A (en) | Preparation method and application of Ganmaoqingre granules | |
| CN109423358A (en) | A kind of extracting method of Chinese small iris volatile oil | |
| CN104804011A (en) | Method for separating and purifying isoimperatorin and imperatorin from angelica dahurica | |
| Shen et al. | Solid-liquid extraction of chlorogenic acid from Eucommia ulmoides Oliver leaves: Kinetic and mass transfer studies | |
| CN102988691B (en) | Preparation method and application of liver-strengthening tablet | |
| CN103698461A (en) | Detection method of volatile oil intermediate of antipyretic cold tablet | |
| CN102274310A (en) | Preparation method of cinquefoil total triterpenoids | |
| Liu et al. | Extraction of paeonol from Jisheng Shenqi Wan using supercritical fluid extraction | |
| CN110551005A (en) | Preparation method of magnolol |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into 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: 20140409 |