CN101285021A - Process for simultaneously abstracting essential oil, chromocor and triterpenes components from agastache - Google Patents
Process for simultaneously abstracting essential oil, chromocor and triterpenes components from agastache Download PDFInfo
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- CN101285021A CN101285021A CNA2008101238365A CN200810123836A CN101285021A CN 101285021 A CN101285021 A CN 101285021A CN A2008101238365 A CNA2008101238365 A CN A2008101238365A CN 200810123836 A CN200810123836 A CN 200810123836A CN 101285021 A CN101285021 A CN 101285021A
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Abstract
The invention belongs to natural products separating and extracting technical field, particularly relating to a process for simultaneously extracting essential oil, flavone and triterpene out of wrinkled giant hyssop. The invention provides a novel separating and extracting process, which can simultaneously separate and extract essential oil, flavone and triterpene by taking wrinkled giant hyssop as raw materials; the used raw materials can be wrinkled giant hyssop as well as cablin pacholi, fresh or dried herbs as well as fresh or dried leaves, stems or other parts. When fresh wrinkled giant hyssop leaves are used as the raw materials, the essential oil thereof comprises more than 40 volatile components such as cis form - isomenthone, anti form - isomenthone piperitone, hexenoic aldehyde, delta-cadinene, cadinol, alpha-muurolene, limonene and pulegone, wherein main volatile components are the cis form - isomenthone and the anti form- isomenthone, contents of which are 34.11 percent and 15.42 percent respectively; the total flavone comprises flavonoids such as acacia substance, tilianin, linarin, agastachoside, isoagastachoside, agastachin, apigenin, apigenin-7- glucoside, 6-methoxyl group apigenin, luteolin and luteolin-7- glucoside, etc., wherein main flavone components are the agastachoside and the isoagastachoside , contents of which are 25.8 percent and 8.21 percent respectively; the triterpene materials comprises triterpene compounds such as cralaegolic acid, oleanolic acid, 3-acetyl oleanolic aldehvde, 3- acetyl oleanolic acid, alpha-amyrin, beta- amyrin, campesterol, campestanol, ursolic acid, erythrodiol, erythrodiol-3-acetic ester, wherein the main triterpene component is the cralaegolic acid , the content of which is 34.6 percent. The components have wide biological activities and a plurality of effects such as liver protection, anti-tumor, anti-HIV-1, anti-proteinase activity of HIV-1, anti-herpes zoster virus and immunity improvement, etc.
Description
Technical field
The present invention relates to a kind of technology of from wrinkled giant hyssop, extracting essential oil, flavones and triterpenes components simultaneously, belong to the process and utilization technology field of Chinese herbal medicine resource.
Background technology
Wrinkled Gianthyssop Herb (Herba Pogostemosis claims patchouli, patchouli again) is a kind of annual herb plant, also is simultaneously the very famous herbal medicine material a kind of commonly used of South East Asia one band, generally is used as medicine with over-ground part or the stem stalk that dries in the shade.Originate in subtropical zones such as Asia Philippines, China's main product in Guangdong, Hainan; Cultivation is arranged.Wrinkled Gianthyssop Herb is an aromatic damp resolving drug commonly used clinically, its suffering of distinguish the flavor of, and slightly warm in nature is returned spleen, stomach, lung channel, has eliminating dampness with aromatics, the preventing or arresting vomiting that whets the appetite, delivers the function of relieving summer-heat.The treatment of be mainly used in turbid damp obstructing in middle-JIAO, the vomiting of gastral cavity naevus, summer-heat and damp burnout clinically, uncomfortable in chestly do not relax, cold-dampness being closed diseases such as heat, abdominal pain diarrhea, nasosinusitis headache
[1]
Wrinkled giant hyssop (Herba Agastaches claims native ageratum, Lysimachia capillipes Hemsl, Da Ye peppermint again) is a kind of per nnial herb, also is the distinctive a kind of Chinese medicinal herbs commonly used of China simultaneously, generally is used as medicine with over-ground part or the stem stalk that dries in the shade.Main product Sichuan, Jiangsu, Zhejiang, Hunan; Cultivation is arranged.Slightly warm in nature, flavor is hot.Dispelling summer-heat from superficies of the body, removing dampness to restore normal function of the stomach.Be used for summer-heat damp cold, uncomfortable in chest, stomachache vomiting and diarrhoea
[1]
The research report shows that Herba Agastaches Rugosae volatile oil can stimulate stomach mucous membrane, promotes gastric secretion, improves digestion ability, and gi tract are had spasmolysis
[2]And have significant anti-microbial effect, can suppress to cause the pathogenic growth breeding of upper respiratory tract infection, effect with treatment flu.In addition, not only contain abundant volatile oil in Wrinkled Gianthyssop Herb and the wrinkled giant hyssop, and contain gold with joyous plain, tilianin, linarin, agastachoside, different agastachoside, agastachin, apigenin, apigenin-7-glucoside, 6-methoxyl group apigenin, luteolin, luteolin-flavonoid compound and Crategolic acids such as 7-glucoside, Oleanolic Acid, 3-acetyl oleanolic aldehyde, the 3-acetyloleanolic acid, α-aromadendrin, β-aromadendrin, campesterol, campestanol, ursolic acid, Erythrodiol, Erythrodiol-triterpene compounds such as 3-acetic ester, have physiologically active widely, protect the liver, antitumor, anti-HIV-1 and HIV-1 protease activity, anti-herpes zoster virus, increase many effects such as immunizing power
[3]
About the separation and extraction technology of the pharmacological component in the wrinkled giant hyssop, focus mostly at present aspect the separation and Extraction of volatile oil.The technology of extracting essential oil, flavones and triterpenes components simultaneously from wrinkled giant hyssop is not appeared in the newspapers both at home and abroad as yet.
1 old intellectual circle, " herbal medicine grand ceremony " [OL], in August, 2006 version.Military science press.http://tieba.baidu.com/f？kz＝130621079
2Patwardhan?S?A，gopra?A?S.An?octamethoxyflavone?from?Agastache?rugosa.Phytochemistry，1981，20(6)1485～1459
3 envelope tin will, Xu Suixu, " progress of wrinkled giant hyssop platymiscium chemistry and pharmacologically active " [J] 1998,15 (2), 144-148
Summary of the invention
The present invention has invented a kind of technology of extracting essential oil, flavones and triterpenes components from wrinkled giant hyssop simultaneously.Comparatively unique is that it has taken into full account the characteristic of contained effective constituent in the wrinkled giant hyssop medicinal material, has carried out dividing other to extract to wherein contained various effective constituents, has realized the separation of each active component in the wrinkled giant hyssop medicinal material.Operate according to the present invention, can obtain the volatile essential oil, flavones ingredient and the triterpenes components that are contained in the wrinkled giant hyssop, and can not cause losing or destroying of activeconstituents with high extraction yield.This is vital for the comprehensive utilization of wrinkled giant hyssop herb resource.
Wrinkled giant hyssop essential oil, wrinkled giant hyssop flavones and wrinkled giant hyssop triterpene according to processing of the present invention will be widely used in fields such as medicine, healthcare products as new type natural medicine material and functional health beverage materials.
Specifically, at first, flavonoid and triterpenes components that we find in the wrinkled giant hyssop and are contained are highly stable, under the steam distillation processing condition that we taked, can be intact be retained in the residue behind the steam distillation, neither can or not in the high temperature hygrothermal environment of steam distillation, not be degraded along with essential oil is steamed by water vapour yet.Established the basis of from wrinkled giant hyssop, extracting essential oil, flavones and triterpenes components simultaneously thus.
Secondly, we find to adopt the steam distillation technology can effectively avoid the wrinkled giant hyssop medicinal material is placed on long-time decoction the in the water and the decocting liquid ingredient too complicated and the flavones wherein and the content problem on the low side of triterpenes components that cause.Under the steam distillation processing condition that we taked, resulting medicinal material distillation residue after drying, wherein contained flavones and triterpenes activeconstituents can effectively be remained.
We find that in steam distillation, condensing temperature is of paramount importance for the yield of essential oil.Condensing temperature should be in 0～25 ℃ of scope.In the separation and Extraction of flavonoid and triterpenes components, the drying mode of steam distillation residue and dried moisture content are vital.Drying should be carried out under the condition of 0.001～0.5MPa at 0～120 ℃, and the steam distillation residue should be dried to moisture content below 15%.Other parameters, the wrinkled giant hyssop raw material is wrinkled giant hyssop (Herba Agastaches, claim native ageratum, Lysimachia capillipes Hemsl, Da Ye peppermint again) or Wrinkled Gianthyssop Herb (HerbaPogostemosis, claim patchouli, patchouli again), can be fresh or the exsiccant herb, also can be fresh or exsiccant leaf, stem stalk or other any local parts.The distillate collecting amount of steam distillation is 2～10 times of amount of wrinkled giant hyssop medicinal material.Rectifying is carried out under normal pressure, the collecting amount of essential oil be distillate amount 1%～20%.The extraction using alcohol of flavones and triterpenes components carries out under the condition of 50 ℃～backflow, and used concentration of ethanol is 80～100%v/v, and solid-liquid ratio is 1: 5～1: 10, and extraction time is 0.5～2h, and extraction time is 1～3 time.Alcohol solvent be recovered in 0～50 ℃, carry out under 0.001～0.5MPa condition, be recycled to ethanol content in the paste and be lower than 3% and stop.The acetone extraction of flavonoid and triterpenes components is separated under the 30 ℃～condition that refluxes and carries out, and used acetone is anhydrous propanone, and solid-liquid ratio is 1: 2～1: 5, and extraction time is 0.5～2h, and extraction time is 1～3 time.The recovery of acetone solvent and removing at 0～50 ℃ is carried out under 0.001～0.5MPa condition, is recycled to acetone content in the pressed powder and is lower than 0.3% and stops.
Embodiment
Following example will specify working method of the present invention, but can not be as limitation of the invention.
Example one
Get Wrinkled Gianthyssop Herb stem 100g, place on the steam distillation device, connect steam-generating installation, carry out steam distillation,, collect distillate, be distilled to distillate and reach the 300ml termination with 20 ℃ tap water condensation.Residue is placed and is at room temperature dried; Distillate rectifying obtains essential oil 2.5g.After residue dries in the air and is lower than 15% to moisture content, be that the ethanol of 95%v/v extracts 3 times down at reflux temperature (78.5 ℃) according to 1: 4 solid-liquid ratio concentration, each 30min obtains ethanol extract.Ethanol extract reclaims solvent, obtains pale brown look to tan paste 13.05g.Paste extracts 3 times down at reflux temperature (56.5 ℃) with acetone according to 1: 4 solid-liquid ratio, and each 30min is divided into acetone extract and two parts of pressed powder that are insoluble to acetone with paste.The acetone extract reclaims acetone and dry, obtains pressed powder 6.7g, is the wrinkled giant hyssop flavones.Be insoluble to the residue of acetone, remove acetone solvent and drying after, obtain pressed powder 0.73g, be the wrinkled giant hyssop triterpene.
Example two
Get the fresh Radix agastaches of 20kg, in the 1000L still kettle of packing into after the rinsing, feed steam and carry out steam distillation,, collect distillate, be distilled to distillate and reach the 100kg termination with 4 ℃ water condensation.Collect the residue in the still kettle, put to dry under 60 ℃ in the vacuum drying oven to moisture content and be lower than 10%, distillate is put fractionation in the fractionation still, collects preceding 0.5% cut, obtains the 0.5kg essential oil.After moisture content reaches requirement, extract 3 times with ethanol immersion under 75 ℃ of 95%v/v according to 1: 4 solid-liquid ratio, each 30min obtains ethanol extract.Extracting solution is put and is reclaimed ethanol on the evaporation concentration device, obtains pale brown look to tan paste 2.5kg.Paste adds acetone according to 1: 4 solid-liquid ratio, extracts 3 times down at reflux temperature (56.5 ℃), obtains acetone extract.Reclaim solvent acetone, and formed semisolid is put oven dry under 60 ℃ in the vacuum drying oven, obtain wrinkled giant hyssop flavones pressed powder 1300g; Be insoluble to the residue of acetone, after removing acetone solvent and drying, obtain wrinkled giant hyssop triterpenes pressed powder 140g.
Example three
The essential oil sample that the fresh Radix agastaches steam distillation of portion is obtained has carried out the mensuration of forming, and measurement result sees Table 1.Measurement result shows, the main component of the essential oil that obtains from fresh Radix agastaches is mainly cis-isomenthone and trans-isomenthone, and its content is respectively 34.11% and 15.42%.All the other are 40 kinds of compositions such as piperitone, hexenoic aldehyde, δ～cadinene, cadinol, α～muurolene, limonene, pulegone; piperitone wherein has antiasthmatic effect; the cavy anaphylactic shock there is provide protection; and increase with dosage; a certain amount of effect relationship is arranged, can be used for treatment of asthma.Pulegone has antihistamine effect, and hexenoic aldehyde has effective anti-microbial activity, and the D-limonene has antitumor efficacy, and bacteriostatic activity eliminates the phlegm, the cough-relieving effect, and the effect of dissolving gallbladdergallstonecholetithiasis shows that the essential oil that this processes obtains has good drug action.
The chemical constitution of the fresh Radix agastaches water distillation of table 1 overhead product
Example four
The flavones that a Wrinkled Gianthyssop Herb medicinal material is obtained and the sample of triterpenes components have carried out the mensuration of forming.Measurement result shows, contain gold and joyous element, tilianin, linarin, agastachoside, different agastachoside, agastachin, apigenin, apigenin-7-glucoside, 6-methoxyl group apigenin, luteolin, luteolin-flavonoid compounds such as 7-glucoside in the resulting wrinkled giant hyssop total flavones, main flavones ingredient wherein is agastachoside and different agastachoside, and its content is respectively 25.8% and 8.21%.Contain Crategolic acid in the resulting triterpene substance, Oleanolic Acid, 3-acetyl oleanolic aldehyde, the 3-acetyloleanolic acid, α-aromadendrin, β-aromadendrin, campesterol, campestanol, ursolic acid, Erythrodiol, Erythrodiol-triterpene compounds such as 3-acetic ester, main triterpenes components wherein is a Crategolic acid, and its content is 34.6%.These compositions have physiologically active widely, protect the liver, antitumor, anti-HIV-1 and HIV-1 protease activity, anti-herpes zoster virus, the many effects such as immunizing power that increase, have producing refreshing effect to the mind, physiological action such as the heatstroke prevention of being good for the stomach, effect is remarkable, has no side effect.
Example five
With healthy Kunming kind small white mouse (male and female half and half, in 4 ages in week, body weight 18-22g provides [approval number: SCXK (Soviet Union) 2002-0006] by laboratory animal field, the south of the River, curry favour mountain, Wuxi) be laboratory animal, resulting essential oil is carried out acute toxicity test, and gained the results are shown in Table 2 and table 3.
Table 2 is for the influence of test agent to the mouse body weight
Table 3 acute toxicity test result
By observing, the interior mouse activity of 1h all reduces after the administration, recovers normal activity behind the 4h gradually.Food-intake reduces to some extent in the test group 2d, and mouse appetite in the later 5d, spirit, hair color are all normal; Behind the 7d, take off neck and put to death, gross necropsy is not seen main organs pathology and intoxicating phenomenons such as the heart, liver, spleen, lung, kidney.Weigh every day in the observation period 7d, and the body weight of test group mouse descends in the 2d after administration, illustrates that the food-intake of this 2d mouse reduces, and in the later 5d, body weight is recovered gradually and constantly increased.Result of study shows, under the situation for the heavy dose of filling of test agent stomach, dead mouse do not occur, and the overt toxicity reaction is not arranged yet.Its toxicity is described, its maximum safe dose is more than 25g/Kg.
Claims (10)
1. technology of from wrinkled giant hyssop, extracting essential oil, flavones and triterpenes components simultaneously.This technology is made up of the following step:
1) the wrinkled giant hyssop raw material is carried out steam distillation or distilling above water, obtain water white distillate and material slag;
2) resulting distillate is carried out rectifying, obtain water white essential oil;
3) resulting material slag is carried out drying and extraction using alcohol, reclaim alcohol solvent then, obtain pale brown look to tan paste;
4) resulting paste is carried out acetone extraction, paste is divided into two parts that dissolve in acetone and be insoluble to acetone;
5) acetone-insoluble part after recovery acetone solvent and the drying, obtains pressed powder, is the wrinkled giant hyssop flavones;
6) be insoluble to the part of acetone, remove acetone solvent and drying after, obtain pressed powder, be the wrinkled giant hyssop triterpenes components.
2. the technology of extracting essential oil, flavones and triterpenes components simultaneously as claimed in claim 1, it is characterized in that the wrinkled giant hyssop raw material is wrinkled giant hyssop (HerbaAgastaches, claim native ageratum, Lysimachia capillipes Hemsl, Da Ye peppermint again) or Wrinkled Gianthyssop Herb (Herba Pogostemosis, claim patchouli, patchouli again), can be fresh or the exsiccant herb, also can be fresh or exsiccant leaf, stem stalk or other any local parts.
3. the technology of extracting essential oil, flavones and triterpenes components simultaneously as claimed in claim 1, it is characterized in that described steam distillation or distilling above water are meant puts into the encloses container that water and raw material are kept apart with the wrinkled giant hyssop raw material, feed steam or water is added thermogenesis steam, make steam pass the bed of material, condensation and collect formed steam then obtains the process of distillate and material slag.
4. the technology of extracting essential oil, flavones and triterpenes components simultaneously as claimed in claim 3, it is characterized in that described steam distillation or distilling above water are 100～150 ℃ of Heating temperatures, carry out under the condition that condensing temperature is 0～25 ℃, the collecting amount of distillate is 2～10 times of amount of wrinkled giant hyssop raw material.
5. the technology of extracting essential oil, flavones and triterpenes components simultaneously as claimed in claim 1 is characterized in that described rectifying carries out under normal pressure, the collecting amount of essential oil be distillate amount 1%～20%.
6. the technology of extracting essential oil, flavones and triterpenes components simultaneously as claimed in claim 1 is characterized in that described drying at 0～120 ℃, carries out under 0.001～0.5MPa condition, is dried to moisture content in the material slag and is lower than 15% and stops.
7. the technology of extracting essential oil, flavones and triterpenes components simultaneously as claimed in claim 1, it is characterized in that described extraction using alcohol carries out under the condition of 50 ℃～backflow, used concentration of ethanol is 80～100%v/v, solid-liquid ratio is 1: 5～1: 10, extraction time is 0.5～2h, and extraction time is 1～3 time.
8. the technology of extracting essential oil, flavones and triterpenes components simultaneously as claimed in claim 1 is characterized in that be recovered in 0～50 ℃ of described alcohol solvent carrying out under 0.001～0.5MPa condition, is recycled to ethanol content in the paste and is lower than 3% and stops.
9. the technology of extracting essential oil, flavones and triterpenes components simultaneously as claimed in claim 1, it is characterized in that described acetone extraction carries out under the condition of 30 ℃～backflow, used acetone is anhydrous propanone, and solid-liquid ratio is 1: 2～1: 5, extraction time is 0.5～2h, and extraction time is 1～3 time.
10. the technology of extracting essential oil, flavones and triterpenes components simultaneously as claimed in claim 1, it is characterized in that the recovery of described acetone solvent and remove at 0～50 ℃, 0.001 carry out under～0.5MPa the condition, the acetone content that is recycled in the pressed powder is lower than 0.3% termination.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101935591A (en) * | 2010-09-10 | 2011-01-05 | 吉水县金海天然香料油科技有限公司 | Refinement and extraction method of patchouli oil |
| CN102241557A (en) * | 2010-05-10 | 2011-11-16 | 孙志高 | Process for supercritical extraction of limonene from sweet orange peel essential oil |
| CN102357117A (en) * | 2011-10-31 | 2012-02-22 | 天津医科大学 | Pogostemon cablin volatile oil, preparation method thereof and application thereof to prepare anti-tumor medicines |
| CN105795430A (en) * | 2016-03-30 | 2016-07-27 | 吉林工商学院 | Preparation method for agastache rugosus seasoning |
| CN106398870A (en) * | 2016-08-28 | 2017-02-15 | 广西灏源盛世生物科技有限公司 | Extraction method of pogostemon cablin essential oil |
-
2008
- 2008-06-06 CN CNA2008101238365A patent/CN101285021A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102241557A (en) * | 2010-05-10 | 2011-11-16 | 孙志高 | Process for supercritical extraction of limonene from sweet orange peel essential oil |
| CN101935591A (en) * | 2010-09-10 | 2011-01-05 | 吉水县金海天然香料油科技有限公司 | Refinement and extraction method of patchouli oil |
| CN101935591B (en) * | 2010-09-10 | 2012-05-23 | 吉水县金海天然香料油科技有限公司 | Refinement and extraction method of patchouli oil |
| CN102357117A (en) * | 2011-10-31 | 2012-02-22 | 天津医科大学 | Pogostemon cablin volatile oil, preparation method thereof and application thereof to prepare anti-tumor medicines |
| CN105795430A (en) * | 2016-03-30 | 2016-07-27 | 吉林工商学院 | Preparation method for agastache rugosus seasoning |
| CN105795430B (en) * | 2016-03-30 | 2018-10-30 | 吉林工商学院 | A kind of preparation method of wrinkled giant hyssop flavouring |
| CN106398870A (en) * | 2016-08-28 | 2017-02-15 | 广西灏源盛世生物科技有限公司 | Extraction method of pogostemon cablin essential oil |
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