CN1478578A - Microwave Assisted Extraction of Active Components of Glycyrrhizae - Google Patents
Microwave Assisted Extraction of Active Components of Glycyrrhizae Download PDFInfo
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- CN1478578A CN1478578A CNA03130365XA CN03130365A CN1478578A CN 1478578 A CN1478578 A CN 1478578A CN A03130365X A CNA03130365X A CN A03130365XA CN 03130365 A CN03130365 A CN 03130365A CN 1478578 A CN1478578 A CN 1478578A
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- microwave
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- radix glycyrrhizae
- licorice
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- 238000000874 microwave-assisted extraction Methods 0.000 title abstract description 5
- 238000000034 method Methods 0.000 claims abstract description 50
- 230000008569 process Effects 0.000 claims abstract description 30
- 238000000605 extraction Methods 0.000 claims abstract description 22
- LPLVUJXQOOQHMX-QWBHMCJMSA-N glycyrrhizinic acid Chemical compound O([C@@H]1[C@@H](O)[C@H](O)[C@H](O[C@@H]1O[C@@H]1C([C@H]2[C@]([C@@H]3[C@@]([C@@]4(CC[C@@]5(C)CC[C@@](C)(C[C@H]5C4=CC3=O)C(O)=O)C)(C)CC2)(C)CC1)(C)C)C(O)=O)[C@@H]1O[C@H](C(O)=O)[C@@H](O)[C@H](O)[C@H]1O LPLVUJXQOOQHMX-QWBHMCJMSA-N 0.000 claims abstract description 19
- 235000006200 Glycyrrhiza glabra Nutrition 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000002791 soaking Methods 0.000 claims abstract description 5
- 238000009835 boiling Methods 0.000 claims abstract description 4
- 244000303040 Glycyrrhiza glabra Species 0.000 claims description 12
- 235000011477 liquorice Nutrition 0.000 claims description 10
- 239000012567 medical material Substances 0.000 claims description 8
- 238000002386 leaching Methods 0.000 claims description 6
- 230000010354 integration Effects 0.000 claims description 4
- 238000007654 immersion Methods 0.000 claims description 2
- 238000010298 pulverizing process Methods 0.000 claims 1
- 239000002904 solvent Substances 0.000 abstract description 10
- LPLVUJXQOOQHMX-UHFFFAOYSA-N glycyrrhetinic acid glycoside Natural products C1CC(C2C(C3(CCC4(C)CCC(C)(CC4C3=CC2=O)C(O)=O)C)(C)CC2)(C)C2C(C)(C)C1OC1OC(C(O)=O)C(O)C(O)C1OC1OC(C(O)=O)C(O)C(O)C1O LPLVUJXQOOQHMX-UHFFFAOYSA-N 0.000 abstract description 9
- 229960004949 glycyrrhizic acid Drugs 0.000 abstract description 9
- UYRUBYNTXSDKQT-UHFFFAOYSA-N glycyrrhizic acid Natural products CC1(C)C(CCC2(C)C1CCC3(C)C2C(=O)C=C4C5CC(C)(CCC5(C)CCC34C)C(=O)O)OC6OC(C(O)C(O)C6OC7OC(O)C(O)C(O)C7C(=O)O)C(=O)O UYRUBYNTXSDKQT-UHFFFAOYSA-N 0.000 abstract description 9
- 235000019410 glycyrrhizin Nutrition 0.000 abstract description 9
- VTAJIXDZFCRWBR-UHFFFAOYSA-N Licoricesaponin B2 Natural products C1C(C2C(C3(CCC4(C)CCC(C)(CC4C3=CC2)C(O)=O)C)(C)CC2)(C)C2C(C)(C)CC1OC1OC(C(O)=O)C(O)C(O)C1OC1OC(C(O)=O)C(O)C(O)C1O VTAJIXDZFCRWBR-UHFFFAOYSA-N 0.000 abstract description 8
- 239000001685 glycyrrhizic acid Substances 0.000 abstract description 8
- 238000000944 Soxhlet extraction Methods 0.000 abstract description 7
- 235000001453 Glycyrrhiza echinata Nutrition 0.000 abstract description 5
- 235000017382 Glycyrrhiza lepidota Nutrition 0.000 abstract description 5
- 229940010454 licorice Drugs 0.000 abstract description 5
- 239000000463 material Substances 0.000 abstract description 4
- 230000008901 benefit Effects 0.000 abstract description 3
- 238000009776 industrial production Methods 0.000 abstract description 2
- 239000003960 organic solvent Substances 0.000 abstract description 2
- 241000202807 Glycyrrhiza Species 0.000 abstract 4
- 230000000052 comparative effect Effects 0.000 description 15
- 239000000284 extract Substances 0.000 description 12
- 230000000694 effects Effects 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 5
- 239000003814 drug Substances 0.000 description 4
- 239000004615 ingredient Substances 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 239000012043 crude product Substances 0.000 description 3
- 229940079593 drug Drugs 0.000 description 3
- 229930194248 Licoflavone Natural products 0.000 description 2
- MEHHCBRCXIDGKZ-UHFFFAOYSA-N Licoflavone C Natural products CC(C)=CCC1=C(O)C=C(O)C(C(C=2)=O)=C1OC=2C1=CC=C(O)C=C1 MEHHCBRCXIDGKZ-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 241000411851 herbal medicine Species 0.000 description 2
- 238000005728 strengthening Methods 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 1
- 239000004378 Glycyrrhizin Substances 0.000 description 1
- 240000002045 Guettarda speciosa Species 0.000 description 1
- 235000001287 Guettarda speciosa Nutrition 0.000 description 1
- 235000017443 Hedysarum boreale Nutrition 0.000 description 1
- 235000007858 Hedysarum occidentale Nutrition 0.000 description 1
- 230000000259 anti-tumor effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000010364 biochemical engineering Methods 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 150000004676 glycans Chemical class 0.000 description 1
- 239000001947 glycyrrhiza glabra rhizome/root Substances 0.000 description 1
- 230000036039 immunity Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000003834 intracellular effect Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000010534 mechanism of action Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000035772 mutation Effects 0.000 description 1
- 229920001282 polysaccharide Polymers 0.000 description 1
- 239000005017 polysaccharide Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 238000002137 ultrasound extraction Methods 0.000 description 1
- 239000005418 vegetable material Substances 0.000 description 1
Landscapes
- Medicines Containing Plant Substances (AREA)
Abstract
一种甘草有效成分的微波辅助提取方法，甘草经粉碎、浸泡后其提取过程采用了微波辐照处理与索氏提取联合工艺。甘草加水浸泡后的微波处理在常压下进行，控制微波辐照功率密度30～70W/g，微波辐照时间10～30秒，水温在沸点以下。甘草浸泡过程中的加水量为药材的1.5～3.5倍，浸泡时间1～10分钟。提取时间0.5～2.5小时。本发明的优点是：综合了微波技术与传统索氏提取工艺的特点，浸提效率显著提高，甘草酸得率增加，同时克服了传统工艺提取时间长、溶剂用量大的问题。以水作为提取剂，无有机溶剂残留，对环境无污染。同时对现有的微波设备没有特殊的要求，对现行工艺改动较少，流程简单可靠，适用于工业生产。The invention discloses a microwave-assisted extraction method of active components of licorice. After the licorice is pulverized and soaked, the extraction process adopts a combined process of microwave irradiation treatment and Soxhlet extraction. The microwave treatment after the licorice is soaked in water is carried out under normal pressure, the microwave irradiation power density is controlled to 30-70W/g, the microwave irradiation time is 10-30 seconds, and the water temperature is below the boiling point. The amount of water added during the licorice soaking process is 1.5 to 3.5 times that of the medicinal materials, and the soaking time is 1 to 10 minutes. The extraction time is 0.5-2.5 hours. The invention has the advantages that the characteristics of the microwave technology and the traditional Soxhlet extraction process are integrated, the extraction efficiency is significantly improved, the yield of glycyrrhizic acid is increased, and the problems of long extraction time and large amount of solvent used in the traditional process are overcome. With water as the extractant, there is no organic solvent residue and no pollution to the environment. At the same time, there is no special requirement on the existing microwave equipment, less changes to the current process, the process is simple and reliable, and it is suitable for industrial production.
Description
Technical field
The present invention relates to a kind of extracting method of Chinese herbal medicine effective ingredients, particularly relate to the method that a kind of employing microwave treatment-Soxhlet is extracted process integration.
Background technology
Radix Glycyrrhizae is the traditional Chinese crude drug of China, and it is historical remote, of many uses as one of composition of Chinese herbal medicine or some Chinese patent medicines.In recent years Radix Glycyrrhizae extract such as glycyrrhizin, glycyrrhizic acid, Angelica Polysaccharide and licoflavone etc. be studies show that Radix Glycyrrhizae extract has the effect of antitumor, mutation, blood fat reducing, enhance immunity adjusting.Traditional Radix Glycyrrhizae extracting method has extraction, Soxhlet method, circumfluence method etc., all has extraction time length, impurity dissolution rate height, problems such as the solvent for use amount is big, extraction efficiency is low, organic solvent residual; If use water as the extraction solvent, when extraction time than long time easy moldy metamorphism also.The ultrasonic extraction of newly-developed is to utilize cavitation effect of ultrasonic waves to strengthen leaching process, CO
2Supercritical methanol technology is to utilize to extract solvent property change the leaching process of strengthening under supercriticality, and the extraction effect of these two kinds of methods all significantly is better than traditional method, but have all that equipment investment is big, operating cost is than problems such as height.Microwave-assisted extracts by using less solvent and energy to support, is an eco-friendly green production technology, and its mechanism of action is difference and other method fully.The volume heating of microwave and selectivity heating, the microscopic structures of vegetable material is changed, make that target component is easier to be discharged from substrate, therefore, microwave-assisted extracts can improve extraction rate, reaches the purpose of strengthening mass transfer, shortening extraction time.It all is extractions of adopting microwave to replace traditional heat source to carry out that the effective liquorice microwave-assisted of reported in literature extracts, the people's such as Zhang Mengjun that deliver as " Chinese patent medicine " 2002 the 24th the 5th phase of volume article " microwave-assisted extracts the research of licoflavone " utilizes the direct irradiation Radix Glycyrrhizae of microwave energy and extracts solvent; The people's such as Xuejun Pan that deliver as " Biochemicalengineering journal " the 5th phase in 2002 article " Microwave-assistedextraction of glycyrrhizic acid from licorice root ", utilize microwave to carry out the Radix Glycyrrhizae reflux, extract, as thermal source, therefore need special-purpose Microwave Extraction Equipment, change bigger existing technology.The present invention overcomes the deficiencies in the prior art, is starting point to utilize microwave technology to improve traditional handicraft, and extraction process is significantly improved and enhanced.
Summary of the invention
The purpose of this invention is to provide a kind of extracting method that can significantly improve effective liquorice, extract quality improved significantly, and have extraction efficiency height, flow process simple and reliable, be applicable to industrial characteristics.
For reaching this purpose, the method for inventing and used a kind of microwave treatment and Soxhlet to extract process integration is extracted effective liquorice, is different from the simple method with the microwave extraction medicinal liquid of present employing.Major technique of the present invention is characterised in that the leaching process of effective liquorice has adopted microwave exposure to handle with Soxhlet and extracted process integration, microwave treatment after Radix Glycyrrhizae is soaked is carried out under normal pressure, controlled microwave irradiance power density 30～70W/g (Radix Glycyrrhizae), microwave irradiation time 10～30 seconds, water temperature is below boiling point.Amount of water in the Radix Glycyrrhizae immersion process is 1.5～3.5 times of medical material, soak time 1～10 minute.0.5～2.5 hour extraction time.The controlled microwave irradiance power density also can be 45～65W/g (Radix Glycyrrhizae), microwave irradiation time 10～15 seconds.Microwave treatment can be clearance-type or continous way.The present invention utilizes the characteristics of microwave volume heating and selectivity heating, strengthen in the medical material target component from medical material inside to the diffusion of extracting solvent.The effective ingredient of Chinese crude drug is intracellular matter, discharges in cell so the extraction of effective ingredient is actually target component, is diffused into the process in the solvent.The first step of extracting method is to adopt microwave exposure, by microwave heating the microscopic structures of host material inside is changed, and reduces in the leaching process target component in the resistance to mass tranfer of host material inside; Second step extracted for Soxhlet, can keep the higher concentration difference inside and outside host material of licorice ingredient in the leaching process like this, thus the extraction efficiency height, and need not filtration, technology is simple.
Specific embodiment
Below in conjunction with embodiment the present invention is further detailed.
Radix Glycyrrhizae is soaked after the plant pulverizer is ground into 20～80 orders with it, and it is 3.0 times of amounts of medical material that amount of water is soaked in control, soak time 2 minutes.Guarantee the Radix Glycyrrhizae moistening, but do not retain too many moisture, otherwise having relatively high expectations to microwave equipment and splendid attire medical material container.The Radix Glycyrrhizae powder that the first step will be soaked is put into microwave field and is carried out microwave pretreatment.Under normal pressure, carry out, present embodiment controlled microwave power density 52W/g (Radix Glycyrrhizae), exposure time 12 seconds guarantees that water temperature is below boiling point.Second step was that Soxhlet is extracted.The medical material that microwave treatment is crossed is transferred in the apparatus,Soxhlet's, and the extraction solvent is a water, and control extractant consumption is 12 times of medical material, 2.0 hours extraction times.Extracting solution can be produced glycyrrhizic acid inclusion compound and extractum respectively.Extracting solution adds dilute sulfuric acid and transfers Ph=2, leaves standstill 12 hours, and filtration will precipitate oven dry and promptly get glycyrrhizic acid inclusion compound.Extracting solution gets glycyrrhizic acid extractum through concentrated, water bath method to constant weight.Calculating the Radix Glycyrrhizae extractum yield with inventory is 36.55%, and the glycyrrhizic acid inclusion compound yield is 8.19%, and content in crude product is 22.41% in the extractum.
Comparative example 1: technical process and embodiment are basic identical, and not existing together is to soak 1h.
Comparative example 2: technical process and embodiment are basic identical, do not exist together be do not soak, without microwave treatment.
Comparative example 3: technical process and embodiment are basic identical, do not exist together be soak 1h, without microwave treatment.
Comparative example 4: technical process and embodiment are basic identical, do not exist together be soak 1h, without microwave treatment, Soxhlet extraction time is 3.5h.
It is as shown in the table that embodiment and comparative example extract experimental result.
Comparative example 2 is compared with comparative example 3: the effect of soaking traditional Soxhlet extraction process is described.
Embodiment compares with comparative example 1: the effect of soaking new technology is described.
Embodiment compares with comparative example 2: illustrate that new technology is better than traditional Soxhlet extraction process.
Embodiment compares with comparative example 4: illustrate that new technology is better than traditional Soxhlet extraction process.
Table: embodiment and comparative example extract experimental result
| The experiment number | Yield of extract (%) | Crude product yield (%) | Content in crude product in the extractum (%) | Process characteristic/operating time |
| Embodiment | ????36.55 | ????8.19 | ?????22.41 | Do not soak-microwave/2h |
| Comparative example 1 | ????33.00 | ????7.16 | ?????21.70 | Soak 1h-microwave/3h |
| Comparative example 2 | ????28.44 | ????3.17 | ?????11.15 | Do not soak-microwave/2h not |
| Comparative example 3 | ????30.19 | ????5.80 | ?????19.21 | Soak not microwave/3h of 1h- |
| Comparative example 4 | ????34.53 | ????7.48 | ?????21.66 | Soak not microwave/4.5h of 1h- |
Beneficial effect of the present invention and advantage are: combine the advantage of microwave technology and traditional Soxhlet extraction process, extracting efficiency significantly improves, the glycyrrhizic acid yield increases, and has overcome simultaneously the problem that traditional handicraft extraction time is long, solvent load is large. Use water instead as extractant, organic solvent-free is residual, environmentally safe, clean environment firendly. The present invention is take applied microwave technological transformation traditional handicraft as starting point, so existing microwave equipment is not had special requirement, less to the current technology change, flow process is simple and reliable, is applicable to industrial production.
Claims (4)
1, a kind of microwave auxiliary extracting method of effective liquorice, Radix Glycyrrhizae is characterized in that after pulverizing, soaking the leaching process of effective liquorice has adopted microwave exposure to handle with Soxhlet and extracted process integration, microwave treatment after Radix Glycyrrhizae is soaked is carried out under normal pressure, controlled microwave irradiance power density 30～70W/g (Radix Glycyrrhizae), microwave irradiation time 10～30 seconds, water temperature is below boiling point.
2, the microwave auxiliary extracting method of effective liquorice according to claim 1 is characterized in that amount of water in the Radix Glycyrrhizae immersion process is 1.5～3.5 times of medical material, soak time 1～10 minute.
3, the microwave auxiliary extracting method of effective liquorice according to claim 1 and 2 is characterized in that 0.5～2.5 hour extraction time.
4, the microwave auxiliary extracting method of effective liquorice according to claim 1 is characterized in that controlled microwave irradiance power density 45～65W/g (Radix Glycyrrhizae), microwave irradiation time 10～15 seconds.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03130365 CN1218764C (en) | 2003-07-04 | 2003-07-04 | Microwave auxiliary extraction method of licorice effective component |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03130365 CN1218764C (en) | 2003-07-04 | 2003-07-04 | Microwave auxiliary extraction method of licorice effective component |
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| Publication Number | Publication Date |
|---|---|
| CN1478578A true CN1478578A (en) | 2004-03-03 |
| CN1218764C CN1218764C (en) | 2005-09-14 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 03130365 Expired - Fee Related CN1218764C (en) | 2003-07-04 | 2003-07-04 | Microwave auxiliary extraction method of licorice effective component |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100379754C (en) * | 2004-11-22 | 2008-04-09 | 王煊 | Extraction of saponin by non-solvent microwave heat |
| CN102599198A (en) * | 2012-01-13 | 2012-07-25 | 东北林业大学 | Method for extracting ragweed insecticidal active substances by Soxhlet-microwave combination |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100343205C (en) * | 2005-11-15 | 2007-10-17 | 江西汇仁药业有限公司 | Method for separating Chinese medicinal active substances |
-
2003
- 2003-07-04 CN CN 03130365 patent/CN1218764C/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100379754C (en) * | 2004-11-22 | 2008-04-09 | 王煊 | Extraction of saponin by non-solvent microwave heat |
| CN102599198A (en) * | 2012-01-13 | 2012-07-25 | 东北林业大学 | Method for extracting ragweed insecticidal active substances by Soxhlet-microwave combination |
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| Publication number | Publication date |
|---|---|
| CN1218764C (en) | 2005-09-14 |
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