CN105949815A - Ultrasonic-Soxhlet combined extraction device and traditional Chinese medicine dreg pigment extraction method based on same - Google Patents
Ultrasonic-Soxhlet combined extraction device and traditional Chinese medicine dreg pigment extraction method based on same Download PDFInfo
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- CN105949815A CN105949815A CN201610302214.3A CN201610302214A CN105949815A CN 105949815 A CN105949815 A CN 105949815A CN 201610302214 A CN201610302214 A CN 201610302214A CN 105949815 A CN105949815 A CN 105949815A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B61/00—Dyes of natural origin prepared from natural sources, e.g. vegetable sources
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Abstract
The invention discloses an ultrasonic-Soxhlet combined extraction device and a traditional Chinese medicine dreg pigment extraction method based on the same. Based on the device, the extraction method comprises four steps as follows: step one, drying and grinding of dregs; step two, extraction of pigments; step three, purification of the pigments; step four, drying of the pigments. According to the method, cellulase is added on the basis of an ultrasonic-Soxhlet combined extraction method, so that the pigment extraction rate of the traditional Chinese medicine dregs is increased. The extraction process is simple, the production efficiency is high, pollution is prevented, the pigment extraction rate and the product quality are remarkably improved, and accordingly, the traditional Chinese medicine dregs as waste resources are utilized to the greatest extent.
Description
Technical field
The present invention relates to a kind of ultrasound wave-cable-styled combined extracting device and the extracting method of Chinese medicine dreg pigment thereof,
Especially extract in the case of enzymatic, a kind of make Chinese medicine dreg pigment extraction ratio increase
Extracting method.
Background technology
Chinese medicine dreg annual emissions reaches 30,000,000 tons at present according to statistics.Natural resources of Chinese medicinal materials is developed in a large number,
While bringing great economic benefit, the medicinal residues problem that Chinese crude drug produces is the most following.Traditional Chinese medicine
Medicinal residues generally to be regarded as refuse and abandon, and processing method is mainly burned, landfill disposal, the most not only pollutes ring
Border, waste soil, and the huge wasting of resources can be caused, underuse the resource of medicinal residues self.Thing
In reality, Chinese medicine dreg still retains many compositions.Chinese crude drug complicated component, pharmaceutical factory extracting after its effective ingredient,
Remaining medicinal residues still contain other active component a large amount of.Wherein, the pigment in Chinese medicine dreg is that pole has exploitation
Value meaning.Making full use of resource, the shortage that can reduce resource can reduce again Chinese medicine dreg to ring
The pollution in border, it can be seen that, carry out the extraction work of Chinese medicine dreg pigment and be necessary.Carry out Chinese medicine
The extraction of medicinal residues pigment, on the one hand can reduce the pollution of the waste of resource, environment；On the other hand can also
Pigment extraction obtained replaces synthetic dyestuff, and this is one is significantly to work.
The research of pigment both at home and abroad is directed generally to the extracting method of pigment and the purposes of pigment.Such as the side extracted
Method has: reflux extraction, extraction, supercritical CO2Extraction, enzyme process abstraction technique, microwave extracting skill
Art, ultrasonic enhanced extraction technology etc..From the point of view of current extraction process technology, have no ultrasound wave-cable-styled
Close the method extracting Chinese medicine dreg pigment, then carry out the work of ultrasound wave-cable-styled combined extracting Chinese medicine dreg pigment
It is the pole work that has new meaning.The innovative point of the present invention has 4 points: (1) raw material is Chinese medicine dreg；(2) ultrasonic
Ripple-cable-styled combined extracting device, has no commercially available；(3) cellulase is added, it is therefore an objective to assisted extraction,
Improve the yield of effective ingredient；(4) ultrasonic assistant soxhlet extraction method.The invention enables the extraction ratio of pigment
Increase compared with traditional method, be that a pole has the significant work of innovation.
Pigment have synthetic dyestuff and natural pigment point, synthetic dyestuff belongs to coal tar based dye compound, has
The carcinogen such as beta-naphthylamine etc can be formed in human body, there is safety issue.Natural pigment is mainly
From plant, animal material and microbial cell obtain, because of animals and plants Material growth breeding by season, weather,
The impact of the factors such as the place of production, insufficient raw material, the pigment therefrom extracted is the most expensive, and application is limited to.
The pigment extracting gained in medicinal residues belongs to natural pigment, and natural pigment has the natural colour that nature is the same,
Can apply in the sweets of multiple-layer polychromatic so that it is seem more tempting；The pigment extracted in Chinese medicine dreg can
As a kind of coloring agent, can be used for the coloring of foods and cosmetics.Useless medicinal residues are used to extract natural plant color
Element has become as one of effective way.The present invention uses microwave-cable-styled-ultrasonic combined method to extract Chinese medicine dreg
In pigment, the pigment quality obtained and color valency are all preferable, have good repeatability, are suitable for scale
Produce, decrease the waste of resource, and there is wide development prospect.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of ultrasound wave-cable-styled combined extracting device and Chinese medicines thereof
The extracting method of slag pigment.
Solve above-mentioned technical problem and be the technical scheme is that a kind of ultrasound wave-cable-styled combined extracting device,
Including controllable lift platform, glass container, thermostat water bath, round-bottomed flask, adapter, Soxhlet extractor, ball
Shape condensing tube and the sonochemical process system being made up of ultrasonic horn and ultrasonic generator；Described round-bottomed flask,
Adapter, Soxhlet extractor, spherical condensation tube are sequentially connected with from top to bottom, and wherein, round-bottomed flask is fixed on perseverance
In warm water bath, glass container is placed on controllable lift platform, and Soxhlet extractor is positioned at glass container.Institute
Stating ultrasonic horn to be inserted in glass container, ultrasonic horn is connected with ultrasonic generator.
The method of the extracting method of a kind of Chinese medicine dreg pigment, is carried out as follows:
(1) Chinese medicine dreg is ground, cross 30-60 mesh sieve, be dried at 20-30 DEG C.
(2) surname extraction: medicinal residues 5g, 1.0g cellulase filter paper after step 1 being processed is wrapped, and puts
In Soxhlet extractor, 300mL mixed solvent is drained in round-bottomed flask by Glass rod, extracts 3-4h,
In extractive process, the temperature of thermostat water bath is set as 65 DEG C, and the power of ultrasonic generator is 400-500w.
After end to be extracted, the extract in round-bottomed flask is carried out at 50 DEG C rotary evaporation, when mixed liquor is in viscous
Evaporation is stopped during thick shape.
(3) with pigment viscous solution obtained in S-8 macroporous resin adsorption step 2, the most again with 5% (body
Long-pending solubility) ethanol water carries out eluting desorption to the S-8 macroporous resin after absorption, obtains pigment eluent.
(4) the pigment eluent in step 3 is placed in microwave vacuum dryer dry 1-2h and obtains Chinese medicines
Slag pigment.Microwave Power Density is 10w/g, and vacuum is 0.02-0.04Mpa.
Further, mixed solvent is by acetone: petroleum ether (volume ratio 1:1-1:6) forms.
The invention has the beneficial effects as follows that the extraction ratio of the Chinese medicine dreg pigment extracted by this method is increased,
Also indicate that with the presence of the extraction that can be of value to pigment under conditions of cellulase simultaneously.And at natural pigment
Extraction purification aspect, macroporous resin adsorption separates the most whole process less energy consumption, low cost, and technique is simple, and
The extraction process that the natural pigment product of gained is more traditional is soaked, filters, is concentrated, and quality significantly improves, color
Element product impurities is few, and color valency is high.
Accompanying drawing explanation
Fig. 1 is the ultrasound wave-cable-styled combined extracting installation drawing of the medlar residue pigment of the present invention；
Fig. 2 is the medlar residue pigment extractive technique route map of the present invention；
Fig. 3 is the infared spectrum of the wolfberry pigment ethanol solution obtained；
Fig. 4 is the ultraviolet-visible spectrogram of wolfberry pigment ethanol solution；
In figure, controllable lift platform 1, glass container 2, thermostat water bath 3, round-bottomed flask 4, mixed solution 5,
Adapter 6, filter paper bag 7, Soxhlet extractor 8, spherical condensation tube 9, ultrasonic horn 10, ultrasonic generator 11.
Detailed description of the invention
The present invention below in conjunction with embodiment and is further elaborated referring to the drawings:
As it is shown in figure 1, a kind of ultrasound wave-cable-styled combined extracting device, hold including controllable lift platform 1, glass
Device 2, thermostat water bath 3, round-bottomed flask 4, adapter 6, Soxhlet extractor 8, spherical condensation tube 9 and by
Ultrasonic horn 10 and the sonochemical process system of ultrasonic generator 11 composition；Described round-bottomed flask 4, adapter 6,
Soxhlet extractor 8, spherical condensation tube 9 are sequentially connected with from top to bottom, and described lixiviating solution 5 can pass through glass
Rod drains in round-bottomed flask 4；Described filter paper bag 7 is placed in Soxhlet extractor 8 by tweezers；Its
In, round-bottomed flask 4 is fixed in thermostat water bath 3, and glass container 2 is placed on controllable lift platform 1, and
Soxhlet extractor 8 is positioned at glass container 2.Described ultrasonic horn 10 is inserted in glass container 2, ultrasonic horn
10 are connected with ultrasonic generator 11.One end of described adapter 6 is connected with round-bottomed flask 4, and the other end is from glass
Hole bottom container 2 enters；The bottom of described Soxhlet extractor 8 is connected, simultaneously with the other end of adapter 6
Soxhlet extraction takes the top of 8 and passes from the hole at glass container 2 top；Whole device can during operation
Position is controlled by controllable lift platform 1.
First buy following raw material: Chinese medicine medlar residue, cellulase, acetone, petroleum ether, ethanol.
The preparation side extracting pigment from the Chinese medicine medlar residue present invention provided below by specific embodiment
Method is further detailed.
(1) Chinese medicine medlar residue is pulverized, cross 30-60 mesh sieve, be dried at 20-30 DEG C.
(2) respectively weigh the medicinal residues 5g after processing in step 1 and a certain amount of cellulase is respectively placed in four
In Soxhlet extractor, numbering 1～4 respectively.Addition 300mL mixed solvent acetone in four round-bottomed flasks:
Petroleum ether (volume ratio 1:1-1:6), the amount adding cellulase is as shown in table 1.At 40-60 DEG C the most next time
Stream extracts 3-4h, and the mixed solution after extracting is spin-dried at 50 DEG C, obtains the wolfberry pigment of 4 sticky shapes.
(3) with the wolfberry pigment of sticky shape in S-8 macroporous resin respectively adsorption step 2, the most again by 5%
(volume ratio) ethanol water carries out eluting desorption to the S-8 macroporous resin after absorption, obtains medicinal residues Fructus Lycii
Pigment eluent, is labeled as 1～No. 4.
(4) wolfberry pigment 1 in step 3～No. 4 are placed in microwave vacuum dryer dry 1-2h.Weigh,
Calculate thick extraction ratio.
(5) weigh dried Chinese medicine dreg wolfberry pigment 0.1g to be dissolved in 50mL ethanol solution, use ethanol
Solution compares, and surveys its infrared spectrum and uv-vis spectra, the most as shown in Figure 3, Figure 4.Can by Fig. 4
See: the ethanol solution of Chinese medicine dreg wolfberry pigment has maximum absorption band at wavelength 450nm, therefore with 450
Characteristic absorption wavelength as Chinese medicine dreg wolfberry pigment.
The thick extraction ratio of embodiment Chinese medicine slag wolfberry pigment is shown in Table 1.
The thick extraction ratio of table 1 medicinal residues wolfberry pigment
| Embodiment sequence number | 1 | 2 | 3 | 4 |
| Cellulase quality | 0g | 0.5g | 1.0g | 1.5g |
| Wolfberry pigment extraction ratio | 8.64% | 9.62% | 9.71% | 9.54% |
Conclusion: can be drawn by embodiment, the quality adding cellulase when extracting pigment is 0-1.0g,
The extraction ratio of rear wolfberry pigment is gradually increased, during until the cellulase quality added is 1.0g, it is seen that extract
Rate reduces.It can thus be appreciated that extraction effect is optimal when the quality of the cellulase added is 1.0g.
Claims (3)
1. ultrasound wave-cable-styled combined extracting device, it is characterised in that include that controllable lift platform (1), glass hold
Device (2), thermostat water bath (3), round-bottomed flask (4), adapter (6), Soxhlet extractor (8), spherical
Condensing tube (9) and the sonochemical process system being made up of ultrasonic horn (10) and ultrasonic generator (11)；
Described round-bottomed flask (4), adapter (6), Soxhlet extractor (8), spherical condensation tube (9) depend on from top to bottom
Secondary connection, wherein, round-bottomed flask (4) is fixed in thermostat water bath (3), and glass container (2) is placed in
On controllable lift platform (1), and Soxhlet extractor (8) is positioned at glass container (2).Described ultrasonic horn (10)
Being inserted in glass container (2), ultrasonic horn (10) is connected with ultrasonic generator (11).
2. a method for the extraction of Chinese medicine dreg pigment based on device described in claim 1, is characterized in that, by such as
Lower step is carried out:
(1) Chinese medicine dreg is ground, cross 30-60 mesh sieve, be dried at 20-30 DEG C.
(2) surname extraction: medicinal residues 5g, 1.0g cellulase filter paper after step 1 being processed is wrapped, and puts
In Soxhlet extractor (8), 300mL mixed solvent is drained in round-bottomed flask (4) by Glass rod,
Extracting 3-4h, in extractive process, the temperature of thermostat water bath (3) is set as 65 DEG C, ultrasonic generator (11)
Power be 400-500w.After end to be extracted, the extract in round-bottomed flask is rotated at 50 DEG C
Evaporation, stops evaporation when mixed liquor is thick.
(3) with pigment viscous solution obtained in S-8 macroporous resin adsorption step 2, the most again with 5% (body
Long-pending solubility) ethanol water carries out eluting desorption to the S-8 macroporous resin after absorption, obtains pigment eluent.
(4) the pigment eluent in step 3 is placed in microwave vacuum dryer dry 1-2h and obtains Chinese medicines
Slag pigment.Microwave Power Density is 10w/g, and vacuum is 0.02-0.04Mpa.
3. in the extracting method according to the medicinal residues pigment described in claims 1, it is characterised in that: mixed solvent is by third
Ketone: petroleum ether (volume ratio 1:1-1:6) forms.
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| CN201610302214.3A CN105949815B (en) | 2016-05-07 | 2016-05-07 | The extracting method of the cable-styled combined extracting device of ultrasonic wave and its Chinese medicine dreg pigment |
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| CN201610302214.3A CN105949815B (en) | 2016-05-07 | 2016-05-07 | The extracting method of the cable-styled combined extracting device of ultrasonic wave and its Chinese medicine dreg pigment |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108384276A (en) * | 2018-05-07 | 2018-08-10 | 湖南农业大学 | A kind of Ipomoea batatas(L.)Lam and its production method |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101176745A (en) * | 2006-11-03 | 2008-05-14 | 中国科学院长春应用化学研究所 | Method for making chinese medicine radix astragali |
| CN102911791A (en) * | 2012-09-25 | 2013-02-06 | 常州亚环环保科技有限公司 | Method for extracting gardenia essential oil |
| CN103142684A (en) * | 2013-03-27 | 2013-06-12 | 吉首大学 | Tripterospermum cordatum extractive and preparation method thereof |
| CN204073487U (en) * | 2014-04-30 | 2015-01-07 | 五邑大学 | A kind of ultrasonic wave Soxhlet extractor |
| CN105175465A (en) * | 2015-08-12 | 2015-12-23 | 河北工业大学 | Method for extracting Ginkgo biloba leaf flavonoid |
| CN205182248U (en) * | 2015-12-02 | 2016-04-27 | 上海矩源自动化科技有限公司 | Ultrasonic wave cable formula dynamic extraction concentrator |
-
2016
- 2016-05-07 CN CN201610302214.3A patent/CN105949815B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101176745A (en) * | 2006-11-03 | 2008-05-14 | 中国科学院长春应用化学研究所 | Method for making chinese medicine radix astragali |
| CN102911791A (en) * | 2012-09-25 | 2013-02-06 | 常州亚环环保科技有限公司 | Method for extracting gardenia essential oil |
| CN103142684A (en) * | 2013-03-27 | 2013-06-12 | 吉首大学 | Tripterospermum cordatum extractive and preparation method thereof |
| CN204073487U (en) * | 2014-04-30 | 2015-01-07 | 五邑大学 | A kind of ultrasonic wave Soxhlet extractor |
| CN105175465A (en) * | 2015-08-12 | 2015-12-23 | 河北工业大学 | Method for extracting Ginkgo biloba leaf flavonoid |
| CN205182248U (en) * | 2015-12-02 | 2016-04-27 | 上海矩源自动化科技有限公司 | Ultrasonic wave cable formula dynamic extraction concentrator |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108384276A (en) * | 2018-05-07 | 2018-08-10 | 湖南农业大学 | A kind of Ipomoea batatas(L.)Lam and its production method |
| CN108384276B (en) * | 2018-05-07 | 2020-02-07 | 湖南农业大学 | Purple sweet potato pigment and production method thereof |
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| CN105949815B (en) | 2017-06-30 |
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