CN104312729A - Extracting method of elsholtia containing 0.5% to 1.5% of thymol - Google Patents
Extracting method of elsholtia containing 0.5% to 1.5% of thymol Download PDFInfo
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- CN104312729A CN104312729A CN201410569943.6A CN201410569943A CN104312729A CN 104312729 A CN104312729 A CN 104312729A CN 201410569943 A CN201410569943 A CN 201410569943A CN 104312729 A CN104312729 A CN 104312729A
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- thymol
- elscholtiza
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- extracting solution
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/025—Recovery by solvent extraction
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- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
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- Organic Chemistry (AREA)
- Medicines Containing Plant Substances (AREA)
- Acyclic And Carbocyclic Compounds In Medicinal Compositions (AREA)
Abstract
The invention relates to an extracting method of elsholtia containing 0.5% to 1.5% of thymol. The method is characterized by comprising the following steps: by using dried mosla chinensis maxim as a raw material and carrying out microwave extraction, cutting the dried mosla chinensis maxim firstly and crushing to 60-100-mesh powder; putting mosla chinensis maxim powder in a microwave extraction tank and adding 1-2 times of 70wt% of edible alcohol for soaking for 1-5 hours; then adding 10-15% sodium hydroxide aqueous solution which is 6-8 times of mosla chinensis maxim and starting microwave to extract for 5-20 minutes at 50-80 DEG C to obtain elsholtzia dregs and an extracting liquid; and further carrying out membrane separation, concentration and drying on the elsholtzia extracting liquid to obtain an elsholtzia extract. The elsholtzia extract which is low in cost and is not extracted by ethyl acetate and petroleum ether is obtained, wherein the thymol content is from 0.5% to 1.5%.
Description
Technical field
The present invention relates to technical field of plant extraction, especially a kind of elscholtiza extracting method.
background technology
Elscholtiza, belongs to Labiatae per nnial herb, medicine-food two-purpose.Herb can be used as medicine, and taste is pungent, slightly warm in nature, has the function in wind dispelling sweating, loose wet, the warm stomach tune of row water; Also has the effect of sanitas.Containing the volatile oil of 1-2% in elscholtiza herb, volatilization main body of oil be thymol, isothymol, to P-cymene.Thymol, has another name called thymol, molecular weight 150, and colourless transparent crystal, has off-odor, volatilizees, can distill with water vapour 100 DEG C time.Fusing point 51.5 DEG C, boiling point about 233 DEG C; Solvability 1g is dissolved in about 1000ml water, 1ml ethanol, and germicidal action is stronger than phenol, and toxicity is low.Also containing flavonoid compounds such as 7-methyl scutellarin, apigenin, luteolin, coffic acid and Quercetins in elscholtiza herb.These Flavonoid substances have anti-oxidant, anti-ageing, anti-bacteria, the function such as anticancer.Chinese invention patent publication number is CN1679707, name is called a kind of preparation, quality controlling means of Herba Moslae extract, a kind of pharmaceutical preparation containing the Herba Moslae volatile oil of 1%-99% and the vehicle (comprising the medicine of other adapted) of 99%-1% is disclosed, there is antiviral, antibacterium, anti-inflammatory, antidiarrheal, pain relieving, the effect of bringing down a fever, and gastrointestinal function can be suppressed hyperfunction.Chinese invention patent publication number is CN103695181A, the preparation method of a kind of Herba Moslae extract of title, and adopt the method for water extraction simultaneous extraction Herba Moslae volatile oil and Flavonoid substances, in Herba Moslae extract, the content of thymol can reach more than 0.40%.
summary of the inventionthe elscholtiza extracting method that technical problem to be solved by this invention is to provide a kind of low cost, thymol content is 0.5-1.5%.
In order to solve this technical problem, technical scheme of the present invention is: with drystone elscholtiza for raw material, adds ethanol, sodium hydroxide and pure water, adopts microwave extraction device to extract.
Concrete extraction step is:
1, by first for drystone elscholtiza segment, 60-100 object powder is ground into;
2, Mosla chinensis Maxim. powder is placed in microwave extraction tank, adds the edible ethanol of 70% of 1-2 times of its weight, soak 1-5 hour;
The content adding 6-8 times of Mosla chinensis Maxim. weight is the aqueous sodium hydroxide solution of 10-15%, and open microwave and extract, the microwave extraction time is 5-20 minute, and temperature is 50-80 DEG C; After extraction terminates, obtain elscholtiza slag and extracting solution; In extracting solution, the thymol content of soluble solid can reach 0.5-1.5%;
?the further membrane sepn of elscholtiza extracting solution, concentrated, drying obtain Herba Moslae extract.In extract, thymol content can reach 0.5-1.5%;
Described segment, pulverizing, microwave extraction, membrane sepn, concentrated, drying is all known technology.
The present invention has following advantages and characteristic:
1, combination technique is novel.
When tradition extracts essential oil, the slag abandoned is too many, and active ingredient loss is large; When tradition extracts medicinal extract, essential oil fundamental loss.Adopt the aqueous sodium hydroxide solution adding 10-15%, 70% edible ethanol, uses pure water microwave extraction, and the microwave extraction time is 5-20 minute, and temperature is 50-80 DEG C; Enhance penetrating power and the solvability of thymol, achieve the fully stripping fast of the volatile components such as thymol, these technical combinations are supported mutually, make the thymol content of soluble solid in extracting solution to reach 0.5-1.5%.In Herba Moslae extract, thymol content can reach 0.5-1.5%.
2, cost is low.
Adopt the aqueous sodium hydroxide solution adding 10-15%, 70% edible ethanol, pure water microwave extraction, the disposable effective constituent being extracted elscholtiza, significantly shortens extraction time, reduces cost.
Embodiment
The following stated example understands the present invention in detail.
Embodiment 1
1, according to 2010 editions " pharmacopeia " quality standards, by the drystone elscholtiza beet slicer segment be up to the standards, then pulverize with Universalpulverizer, the order numerical control of powder is built in 60-80 order;
2, microwave extraction: adopt patent of invention publication number to be CN103695181A, the microwave extraction device of method described in the preparation method of a kind of Herba Moslae extract of title, taking 10kg Mosla chinensis Maxim. powder is placed in microwave extraction tank, adds the edible ethanol of 10kg70%, soaks 2 hours;
3, add the aqueous sodium hydroxide solution of 80kg 10%, open microwave and extract, start timing when temperature reaches 50 DEG C, extraction time is 20 minutes, and temperature controls as 50-80 DEG C; After extraction terminates, obtain elscholtiza slag and extracting solution; Wherein elscholtiza slag weight is 38kg, and extracting solution is 55kg; In extracting solution, soluble solid is detected with Abbe refractometer, result is 1. 5%, with gas chromatograph, detect by 2010 editions " pharmacopeia " quality standards, obtaining thymol concentration in extracting solution is 1450 μ g/ml, and as calculated, in the soluble solid in extracting solution, the content of thymol is 0.97%.
Simultaneous test.
With same equipment and operating method, take 10kg Mosla chinensis Maxim. powder and be placed in microwave extraction tank, add 10kg pure water, soak 2 hours; Add 80kg pure water, open microwave and extract, start timing when temperature reaches 50 DEG C, extraction time is 20 minutes, and temperature controls as 50-80 DEG C; After extraction terminates, obtain elscholtiza slag and extracting solution; Wherein elscholtiza slag weight is 40kg, and extracting solution is 52kg; In extracting solution, soluble solid is detected with Abbe refractometer, result is 0.5%, with gas chromatograph, detect by 2010 editions " pharmacopeia " quality standards, obtaining thymol concentration in extracting solution is 226 μ g/ml, and as calculated, in the soluble solid in extracting solution, the content of thymol is 0.45%.
Embodiment 2
1, according to 2010 editions " pharmacopeia " quality standards, by the drystone elscholtiza beet slicer segment be up to the standards, then pulverize with Universalpulverizer, the order numerical control of powder is built in 60-100 order;
2, microwave extraction: adopt microwave extraction device, take 10kg Mosla chinensis Maxim. powder and be placed in microwave extraction tank, adds the edible ethanol of 20kg 70%, soaks 1 hour;
3, add the aqueous sodium hydroxide solution of 70kg 15%, open microwave and extract, start timing when temperature reaches 50 DEG C, extraction time is 5 minutes, and temperature controls as 50-80 DEG C; After extraction terminates, obtain elscholtiza slag and extracting solution; Wherein elscholtiza slag weight is 36kg, and extracting solution is 58kg; In extracting solution, soluble solid is detected with Abbe refractometer, result is 0.75%, with gas chromatograph, detect by 2010 editions " pharmacopeia " quality standards, obtaining thymol concentration in extracting solution is 1050 μ g/ml, and as calculated, in the soluble solid in extracting solution, the content of thymol is 1.50%.
Simultaneous test is with embodiment 1.
Embodiment 3
1, microwave extraction: adopt microwave extraction device, take the Mosla chinensis Maxim. powder 100kg described in embodiment 1, be placed in 2500L microwave extraction tank, adds the edible ethanol of 150kg 70%, soaks 1 hour;
Add the aqueous sodium hydroxide solution of 750kg 15%, open microwave and extract, start timing when temperature reaches 50 DEG C, extraction time is 50 minutes, and temperature controls as 50-80 DEG C; After extraction terminates, obtain elscholtiza slag and extracting solution; Wherein elscholtiza slag weight is 390kg, and extracting solution is 550kg; In extracting solution, soluble solid is detected with Abbe refractometer, result is 1.75%, with gas chromatograph, detect by 2010 editions " pharmacopeia " quality standards, obtaining thymol concentration in extracting solution is 1350 μ g/ml, and as calculated, in the soluble solid in extracting solution, the content of thymol is 0.77%;
The micro-filtrate membrane filtration of 0.22 μm first used by elscholtiza extracting solution, and filtrate is used nanofiltration membrane separation again, concentrated, and obtains concentrated solution, and concentrated solution is dry with spray-drying tower, obtains Herba Moslae extract.After testing, in extract, thymol content is 0.70%.
Simultaneous test is with embodiment 1.
Claims (1)
1. thymol content is an elscholtiza extracting method of 0: 5 to 1: 5, with drystone elscholtiza for raw material, it is characterized in that, adopts following steps:
By first for drystone elscholtiza segment, be ground into 60-100 object powder;
Mosla chinensis Maxim. powder is placed in microwave extraction tank, adds the edible ethanol of 70% of 1-2 times of its weight, soak 1-5 hour;
The content adding 6-8 times of Mosla chinensis Maxim. weight is again the aqueous sodium hydroxide solution of 10-15%, and open microwave and extract, the microwave extraction time is 5-20 minute, and temperature is 50-80 DEG C; After extraction terminates, obtain elscholtiza slag and extracting solution; In extracting solution, the thymol content of soluble solid is 0.5-1.5%;
The further membrane sepn of elscholtiza extracting solution, concentrated, drying obtain Herba Moslae extract, and in Herba Moslae extract, the mass content of thymol is 0.5-1.5%.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111388381A (en) * | 2020-05-21 | 2020-07-10 | 成都蓓乐康生物科技有限公司 | Cosmetic elsholtzia extract and extraction method thereof |
Citations (5)
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|---|---|---|---|---|
| CN1357229A (en) * | 2000-12-13 | 2002-07-10 | 刘岱 | Application, production and processing of elsholtzia herb as natural plant pest and disease preventing and eliminating agent |
| CN102604743A (en) * | 2012-04-14 | 2012-07-25 | 河南羚锐制药股份有限公司 | Method for extracting volatile substance from plant |
| CN103695181A (en) * | 2013-12-31 | 2014-04-02 | 湖南省百里香天然生物制品开发有限公司 | Preparation method of elsholtziae extract |
| CN103721438A (en) * | 2013-12-31 | 2014-04-16 | 湖南省百里香天然生物制品开发有限公司 | Microwave extracting device and method for extracting herba elsholtziae |
| CN203634854U (en) * | 2013-12-31 | 2014-06-11 | 湖南省百里香天然生物制品开发有限公司 | Microwave extracting device |
-
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- 2014-10-23 CN CN201410569943.6A patent/CN104312729A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1357229A (en) * | 2000-12-13 | 2002-07-10 | 刘岱 | Application, production and processing of elsholtzia herb as natural plant pest and disease preventing and eliminating agent |
| CN102604743A (en) * | 2012-04-14 | 2012-07-25 | 河南羚锐制药股份有限公司 | Method for extracting volatile substance from plant |
| CN103695181A (en) * | 2013-12-31 | 2014-04-02 | 湖南省百里香天然生物制品开发有限公司 | Preparation method of elsholtziae extract |
| CN103721438A (en) * | 2013-12-31 | 2014-04-16 | 湖南省百里香天然生物制品开发有限公司 | Microwave extracting device and method for extracting herba elsholtziae |
| CN203634854U (en) * | 2013-12-31 | 2014-06-11 | 湖南省百里香天然生物制品开发有限公司 | Microwave extracting device |
Non-Patent Citations (1)
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| 仇昆伦 等: "百里香酚的研究进展", 《香料香精化妆品》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111388381A (en) * | 2020-05-21 | 2020-07-10 | 成都蓓乐康生物科技有限公司 | Cosmetic elsholtzia extract and extraction method thereof |
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Application publication date: 20150128 |