CN101177448A - Method for extracting mersosin by ultrasonic field assisted with mixed solvent - Google Patents
Method for extracting mersosin by ultrasonic field assisted with mixed solvent Download PDFInfo
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- CN101177448A CN101177448A CNA2007101906263A CN200710190626A CN101177448A CN 101177448 A CN101177448 A CN 101177448A CN A2007101906263 A CNA2007101906263 A CN A2007101906263A CN 200710190626 A CN200710190626 A CN 200710190626A CN 101177448 A CN101177448 A CN 101177448A
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Abstract
The invention relates to an ultrasonic field-assistant Toosendanin extraction method for compound solvent, which is characterized in that: the chopped Melia azedarach barks and seeds are directly used as the extraction object and are put into the extraction solvent; the extraction solvent with the extraction object is put into an ultrasonic field to obtain the powder with Toosendanin after distillation and concentration, extraction and separation and evaporation drying orderly; the extraction solvent is a compound solvent with solvents of two or more polarities. The invention has the advantages that: the cavitation effect, the thermal effect and the mechanical effect of ultrasonic wave are adopted in the process; the cell walls of the Melia azedarach barks or the seeds are effectively broken; the compound solvent regulates the polarity of the extract, enabling the effective components flow out of the cells into the solution body, and efficiently reducing the solvent consumption and the extraction cost.
Description
Technical field
The impressed field that the present invention relates to natural product is assisted extraction process, particularly the combined extraction method of the lixiviate Kuliansu under ultrasonic field is assisted.
Background technology
Kuliansu (toosendanin) is the tetracyclic triterpenes material that extracts from natural phant China tree or melia toosendan, has certain medical treatment effect, and good broad spectrum disinfestation anti-microbial property arranged, harmless to human body, be easy to degraded, can be used for preventing and treating diseases and pests of agronomic crop, be a kind of botanical pesticide that has a high potential.The extracting method of Meliaceae effective ingredients in plant mainly comprises conventional solvent extraction method, supercritical fluid extraction, microwave assistant extraction and ultrasonic field assistance extraction.Because Kuliansu polarity is medium, and impurity is a lot of in the bark of Melia azedarach L. or the seeds of trees, be difficult to its whole propositions with conventional solvent extraction method, and extraction rate to be slow, extraction efficiency is low, solvent consumption is excessive.
The supercritical carbon dioxide extraction method selectivity is good, service temperature is low, be suitable for extracting the thermo-sensitivity composition that must propose at normal temperatures, but extraction cost height, equipment complexity, the material that active component content is lower in, the plant not high for purity requirements such as Kuliansus is also incorrect.Microwave has very strong penetration power. can to the extractive substance internal and external parts simultaneously evenly, heating promptly, so the microwave assistant extraction efficiency is higher, but be not suitable for the extraction of thermo-sensitivity composition, and Microwave Extraction Equipment manufacture difficulty height, be difficult to realize serialization production.
The existing both at home and abroad report that utilizes ultrasonic wave from another Meliaceae plant seal chinaberry, to assist lixiviate nimbin (Azadirachtin), in CN03117359.4, mentioned the comprehensive leach extraction method that solvent method is combined with ultrasonic wave as Chen Yuming, neem kernel fragmentation after the oil expression is joined in the extraction solvent, strengthening leaching with ultrasonic wave handles, the result proves, in lixiviate in the time of 20 minutes, the nimbin leaching yield has been brought up to more than 85% from 65～75% of single-solvent process, but this invention has only been carried out comprehensive extraction at neem kernel, active constituent content is higher relatively in the kind benevolence, and lixiviate is easy; And serve as to extract the workload that object can reduce raw materials pretreatment on the one hand with the bark or the seeds of trees, on the one hand then because of wherein impurity is various, the difficult extracting effect well that reaches.Do not see as yet so far about ultrasonic assistance method and mixed solvent method associating lixiviate Meliaceae effective ingredients in plant, the especially report of lixiviate Kuliansu.
Summary of the invention
Problem to be solved by this invention provides the Kuliansu extracting method that a kind of ultrasonic field is assisted mixed solvent, it is the extraction of from bark of Melia azedarach L. or China tree seed, carrying out Kuliansu, utilize hyperacoustic cavitation effect, heat effect and mechanical effect, effectively fracturing cell walls; The mixing preparation that utilizes solvent to be to regulate extraction agent polarity rightly, makes effective constituent emigrated cell and stripping quickly in the solution main body, reduces solvent consumption and extraction cost.
Technical solution problem of the present invention adopts following scheme:
Ultrasonic field of the present invention assists the characteristics of the Kuliansu extracting method of mixed solvent to be:
Directly carried thing, will be carried thing and join in the extraction solvent with bark of Melia azedarach L. or the China tree seed pulverized; Again adding there is the extraction solvent of being carried thing to place ultrasonic field, carries out the lixiviate in the ultrasonic field; Vat liquor successively through distillation concentrate, extracting and separating, evaporation drying, obtain containing the powder of Kuliansu;
Described extraction solvent is the mixed solvent of two or more polar solvent, and described polar solvent comprises methyl alcohol, ethanol, acetone, methylene dichloride, trichloromethane and water.
The characteristics of extracting method of the present invention also are:
Described extraction solvent is that volumetric concentration is 5～95% mixed solvent.
The ultrasonic frequency of described ultrasonic field is 28kHz, 40kHz, 45kHz or 100kHz, Ultrasonographic power density 5～20W/L.
Described extraction temperature is 40～100 ℃ a constant temperature.
The described thing of being carried is crushed to 10～60 orders, and the single extraction time is 10～60 minutes under the temperature constant state, the mass volume ratio of being carried thing and extraction solvent is 1: 5～15 grams per milliliters, and filter residue lixiviate 1～5 time repeatedly merges vat liquor.
Compared with the prior art, beneficial effect of the present invention is embodied in:
1, the present invention adopts the collaborative lixiviate mode that ultrasonic field and mixed solvent lixiviate combine, hyperacoustic mechanical effect, cavitation effect and internal heating effect have been utilized, can make cell wall rupture effectively, and the solubleness of increase Kuliansu in solvent, improve the concentration gradient in its velocity of diffusion and the leaching process, quicken the stripping of effective constituent, realize the high-level efficiency extraction; Utilize the polarity allotment effect of mixed solvent, the polarity parameter of extraction solvent is freely allocated between strong polarity (as the polarity parameter 10.2 of water) at low-pole (as the polarity parameter 3.4 of methylene dichloride), with mix similar better to Kuliansu, thereby raising extraction rate, shorten extraction time, improve the throughput of equipment.
2, the present invention compares with the conventional solvent extraction method of the same terms, and in lixiviate 40 minutes, the present invention can extract more than Kuliansu 1.5 grams from per 100 gram bark of Melia azedarach L., and the single solvent water extract method only can be extracted 0.7～0.8 gram from the equivalent bark of Melia azedarach L..As seen, combined extraction method has improved more than 2 times lixiviate speed, and effect is remarkable.
Description of drawings
Fig. 1 extracts the high-efficient liquid phase chromatogram of Kuliansu crude product for the inventive method.
Fig. 2 extracts the infrared spectrogram of Kuliansu crude product for the inventive method.
Below by embodiment, the invention will be further described in conjunction with the accompanying drawings.
Embodiment
Embodiment 1:
Dried bark of Melia azedarach L. is crushed to 60 orders, get 10 grams and place the 250mL flask, add mixed solvent 100mL uniform mixing according to 1: 10 ratio, wherein mixed solvent is by distilled water and alcoholic acid analytical reagent mixed preparing and get, and the alcoholic acid volumetric concentration is 70% in the mixed solvent, therefore, the polarity parameter of mixed solvent is 6.07, that is: ethanol 4.3 * 0.7+ water 10.2 * 0.3, at ultrasonic frequency 40kHz, ultrasonic body power density 10W/L, 70 ℃ of following lixiviates of extraction temperature 40 minutes; After filtration, filter residue is put into the 250mL flask, adds above-mentioned mixed solvent 100mL once more, and ultrasonic frequency 40kHz, ultrasonic body power density 10W/L, 70 ℃ of following lixiviates 40 minutes.After the filtration, merging filtrate, underpressure distillation adds the 50mL n-butanol extraction then and gets extraction liquid after 24 hours, and 3 times repeatedly, combining extraction liquid, the reduction vaporization drying obtains the pale yellow powder product.Adopt high performance liquid chromatograph, Fourier infrared spectrograph to product qualitative detection (spectrogram respectively as shown in Figure 1 and Figure 2), adopting the extraction yield of paradimethy laminobenzaldehyde-sulfuric acid determination of color Kuliansu is 1.5%.
Embodiment 2:
Dried bark of Melia azedarach L. is crushed to 40 orders, get 10 grams and place the 250mL flask, add mixed solvent 150mL uniform mixing according to 1: 15 ratio, wherein mixed solvent is to be got by the analytical reagent mixed preparing of distilled water and methyl alcohol, and the volumetric concentration of methyl alcohol is 70% in the mixed solvent, therefore, the polarity parameter of mixed solvent is 7.68, that is: methyl alcohol 6.6 * 0.7+ water 10.2 * 0.3, at ultrasonic frequency 45kHz, ultrasonic body power density 5W/L, 80 ℃ of following lixiviates of extraction temperature 30 minutes; After filtration, filter residue is put into the 250mL flask, adds above-mentioned mixed solvent 150mL, once more ultrasonic frequency 45kHz, ultrasonic body power density 5W/L, 80 ℃ of following lixiviates 30 minutes.After the filtration, filtrate is merged, underpressure distillation adds the 50mL ethyl acetate extraction then and gets extraction liquid after 24 hours, extract repeatedly 3 times, and combining extraction liquid, the reduction vaporization drying obtains the pale yellow powder product.Adopt high performance liquid chromatograph, Fourier infrared spectrograph that product is carried out qualitative detection, adopting the extraction yield of paradimethy laminobenzaldehyde-sulfuric acid determination of color Kuliansu is 1.2%.
Embodiment 3:
Dried China tree seed is crushed to 20 orders, get 10 grams and place the 250mL flask, add mixed solvent 50mL uniform mixing according to 1: 5 ratio, mixed solvent is to be that 1: 1 acetone and methylene dichloride analytical reagent mixed preparing gets by volume ratio, and therefore, the polarity parameter of mixed solvent is 4.4, that is: acetone 5.4 * 0.5+ methylene dichloride 3.4 * 0.5, in ultrasonic frequency 100kHz, ultrasonic body power density 20W/L, 70 ℃ of extraction temperatures, lixiviate 40 minutes.After filtration, filter residue is put into the 250mL flask, adds above-mentioned mixed solvent 50mL, once more ultrasonic frequency 100kHz, ultrasonic body power density 20W/L, 70 ℃ of following lixiviates 40 minutes.After filtration, filtrate is merged, underpressure distillation, add then behind the 50mL ethyl acetate extraction 24h extraction liquid, 3 times repeatedly, combining extraction liquid, the reduction vaporization drying obtains the pale yellow powder product.Adopt high performance liquid chromatograph, Fourier infrared spectrograph that product is carried out qualitative detection, adopting the extraction yield of paradimethy laminobenzaldehyde-sulfuric acid determination of color Kuliansu is 1.3%.
In concrete the enforcement, the distillation of follow-up refining process using routine concentrates, repeatedly extraction, reduction vaporization technology, promptly utilizes medium polar solvents extractions such as propyl carbinol, ethyl acetate repeatedly, and extraction liquid merges the back reduction vaporization and obtains Kuliansu powder crude product.
Claims (5)
1. ultrasonic field is assisted the Kuliansu extracting method of mixed solvent, it is characterized in that:
Directly carried thing, will be carried thing and join in the extraction solvent with bark of Melia azedarach L. or the China tree seed pulverized; Again adding there is the extraction solvent of being carried thing to place ultrasonic field, carries out the lixiviate in the ultrasonic field; Vat liquor successively through distillation concentrate, extracting and separating, evaporation drying, obtain containing the powder of Kuliansu;
Described extraction solvent is the mixed solvent of two or more polar solvent, and described polar solvent comprises methyl alcohol, ethanol, acetone, methylene dichloride, trichloromethane and water.
2. ultrasonic field according to claim 1 is assisted the Kuliansu extracting method of mixed solvent, it is characterized in that described extraction solvent is that volumetric concentration is 5～95% mixed solvent.
3. ultrasonic field according to claim 1 is assisted the Kuliansu extracting method of mixed solvent, and the ultrasonic frequency that it is characterized in that described ultrasonic field is 28kHz, 40kHz, 45kHz or 100kHz, Ultrasonographic power density 5～20W/L.
4. ultrasonic field according to claim 1 is assisted the Kuliansu extracting method of mixed solvent, it is characterized in that described extraction temperature is 40～100 ℃ a constant temperature.
5. ultrasonic field according to claim 1 is assisted the Kuliansu extracting method of mixed solvent, it is characterized in that the described thing of being carried is crushed to 10～60 orders, the single extraction time is 10～60 minutes under the temperature constant state, the mass volume ratio of being carried thing and extraction solvent is 1: 5～15 grams per milliliters, filter residue lixiviate 1～5 time repeatedly merges vat liquor.
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| Application Number | Priority Date | Filing Date | Title |
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| CNA2007101906263A CN101177448A (en) | 2007-11-20 | 2007-11-20 | Method for extracting mersosin by ultrasonic field assisted with mixed solvent |
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| CNA2007101906263A CN101177448A (en) | 2007-11-20 | 2007-11-20 | Method for extracting mersosin by ultrasonic field assisted with mixed solvent |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107396656A (en) * | 2017-09-15 | 2017-11-28 | 广西壮族自治区农业科学院经济作物研究所 | One cultivates peanut with shell seed-soaking method |
| CN108271794A (en) * | 2018-02-06 | 2018-07-13 | 浦江县美泽生物科技有限公司 | A kind of margosine method for producing insecticide |
| CN108464313A (en) * | 2018-02-06 | 2018-08-31 | 浦江县美泽生物科技有限公司 | A kind of preparation method of botanical fungicide |
| WO2019080571A1 (en) * | 2017-10-24 | 2019-05-02 | 江苏金太阳纺织科技股份有限公司 | Method for extracting toosendanin |
| CN112322071A (en) * | 2020-11-23 | 2021-02-05 | 江南大学 | Extraction method and application of cortex meliae pigment |
-
2007
- 2007-11-20 CN CNA2007101906263A patent/CN101177448A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107396656A (en) * | 2017-09-15 | 2017-11-28 | 广西壮族自治区农业科学院经济作物研究所 | One cultivates peanut with shell seed-soaking method |
| CN107396656B (en) * | 2017-09-15 | 2022-12-02 | 广西壮族自治区农业科学院经济作物研究所 | Peanut seed soaking method with shell |
| WO2019080571A1 (en) * | 2017-10-24 | 2019-05-02 | 江苏金太阳纺织科技股份有限公司 | Method for extracting toosendanin |
| CN108271794A (en) * | 2018-02-06 | 2018-07-13 | 浦江县美泽生物科技有限公司 | A kind of margosine method for producing insecticide |
| CN108464313A (en) * | 2018-02-06 | 2018-08-31 | 浦江县美泽生物科技有限公司 | A kind of preparation method of botanical fungicide |
| CN112322071A (en) * | 2020-11-23 | 2021-02-05 | 江南大学 | Extraction method and application of cortex meliae pigment |
| CN112322071B (en) * | 2020-11-23 | 2021-09-24 | 江南大学 | Extraction method and application of cortex meliae pigment |
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Open date: 20080514 |