CN103936811A - Tea seed meal superfine grinding and ultrasonic-assisted water-alcohol method for extraction of tea saponin - Google Patents
Tea seed meal superfine grinding and ultrasonic-assisted water-alcohol method for extraction of tea saponin Download PDFInfo
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- CN103936811A CN103936811A CN201310023109.2A CN201310023109A CN103936811A CN 103936811 A CN103936811 A CN 103936811A CN 201310023109 A CN201310023109 A CN 201310023109A CN 103936811 A CN103936811 A CN 103936811A
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Abstract
The invention relates to a method using tea seed meal as a raw material for extraction of high purity tea saponin. The method is as follows: using a superfine grinding machine to grind the tea seed meal into tea seed meal powder with a particle size less than 500 mesh, then adding hot water, leaching in certain ultrasonic treatment conditions, then using ethyl alcohol to extract the tea saponin therein, then concentrating, bleaching, and drying to obtain the high purity tea saponin. Compared with the method for extraction of the tea saponin in the prior art, the method has the advantages of simple technical operation, low production cost, short period and high efficiency, the produced tea saponin purity reaches above 95%, and the method is suitable for large-scale popularization and application, can make full use of tea seed resources, and promotes the development of tea industry.
Description
Technical field
The present invention relates to a kind of technology of utilizing the tea dregs of rice to extract high-purity tea saponin, belong to natural product extraction separation field.
Background technology
Tea saponin claims again theasaponin, is a kind of pentacyclic triterpenoid that contains structure sugar and structure acid by extracting in the tea-cake dregs after all kinds of tea-seed, tea seed liquefaction.It is a kind of natural nonionic surface active agent of excellent property, can be widely used in daily use chemicals, building materials, weaving, pesticide field, has higher economic worth.China abounds with tea oil, produces approximately 150,000 tons of tea oil per year, approximately 500,000 tons of tea seed cakes.Be the tea dregs of rice with the residue that organic solvent is further carried tea seed cake after oil.Due to tea dregs of rice bitter, poisonous, substantially go out of use at present, cause the very large wasting of resources.Therefore, from the discarded tea dregs of rice, extract tea saponin and not only can improve the comprehensive utilization ratio of the tea dregs of rice, can also extend camellia oleiferaindustry chain, promote the industrialized development of oil tea, have broad prospects.
At present, extracting tea saponin and conventionally adopt water seaoning, solvent-extraction process from the tea dregs of rice, there is many defects such as extraction time is long, yield is low, poor product quality, energy consumption height in these two kinds of methods, has limited the suitability for industrialized production of tea saponin.Along with the development of Technology, ultrasonic extraction, the New Environment Protection Technologies such as microwave-assisted extraction method start to cause concern, but about utilizing the tea dregs of rice for raw material, the research of extracting tea saponin by tea dregs of rice micronizing and the auxiliary water alcohol method of ultrasonic wave has no report.
Summary of the invention
The present invention, taking the shortcoming that solves above-mentioned technology as object, provides a kind of method of utilizing the tea dregs of rice to extract high-purity tea saponin as raw material, and the method preparation technology is simple, cycle is short, and efficiency is high, and gained tea saponin purity is high, and can reclaim ethanol, be conducive to reduce production costs.
Technical scheme of the present invention is that the auxiliary water alcohol method of tea dregs of rice micronizing and ultrasonic wave extracts tea saponin, and its step is as follows:
(1) adopt supper micron mill to pulverize and be less than 500 object tea dregs of rice powder for particle diameter carrying the tea dregs of rice after oil.
(2) use the aqueous solution 60 DEG C of constant temperature in tea dregs of rice powder, ultrasonic frequency 20kHz～40kHz, lixiviate 20～60min under the condition of ultrasonic power 400w～800w, obtains tea saponin vat liquor after centrifugation.Again by residue as stated above lixiviate once, the centrifugal vat liquor that obtains, merges twice vat liquor.
(3) in the vat liquor of collecting, add flocculation agent to flocculate, centrifugal, remove precipitation, obtain clarified liq.
(4) in clarified liq, add 95% ethanol as extraction solvent, under the condition of 50 DEG C of constant temperature, extract 1.5～3h, after centrifugation, obtain tea saponin extraction liquid.
(5) tea saponin extraction liquid is carried out reclaiming ethanol after concentrating under reduced pressure.After solution after to be concentrated is cooling, add flocculation agent flocculation, after centrifugation, obtain clarified liq.
(6) by extremely white or faint yellow of activated carbon decolorizing for gained clarified liq, obtain destainer.Then by the dry destainer tea saponin finished product that obtains.
Advantage of the present invention is: by the tea dregs of rice are carried out to micronizing pre-treatment, can reduce greatly the powder particle diameter of tea dregs of rice raw material, increase its solvability; In flooding process, adopt ultrasonic wave to carry out auxiliary treatment, ul-trasonic irradiation can produce cavitation effect in liquid, powerful pressure causes the destruction of biological cell wall, and whole shattering process completed in moment, release, diffusion and the dissolving of intracellular matter strengthened in the vibration that ultrasonic wave produces simultaneously, the material being leached biological activity in the time being broken remains unchanged, and can greatly improve extraction rate and yield simultaneously.Tea saponin after water extraction in using 95% ethanol as solvent extraction water extract, not only can significantly improve the purity of tea saponin, has also greatly reduced solvent load and solvent recoverable, is conducive to reduce production costs.
Embodiment
Embodiment 1
Adopt supper micron mill that the tea dregs of rice of carrying after oil are carried out to micronizing and cross 500 mesh sieves, take 100g tea dregs of rice powder, then add 800ml distilled water, under the condition of 60 DEG C of constant temperature, ultrasonic Assisted Extraction 20min.
Adjusting ultrasonic frequency is 20kHz, and ultrasonic power is 400w.After lixiviate completes, centrifugation, residue adds water 300ml lixiviate once more as stated above, merges twice vat liquor.Add flocculation agent by 5% of vat liquor, leave standstill clarification, disgorging, obtains tea saponin extracting solution.Then the ratio of 1: 0.5 by volume, to the ethanol that adds 95% in tea saponin extracting solution, stirs, and leaves standstill 2h under the condition of 50 DEG C of constant temperature, and centrifugation obtains tea saponin extraction liquid.Utilize Rotary Evaporators to carry out concentration to tea saponin extraction liquid, reclaim ethanol reagent, by the concentrated solution rear decoloring that flocculates, and then carry out drying treatment, obtain off-white powder shape tea saponin 9.81g, purity is 95.46%.The rate of recovery of gained tea saponin is 93.4%.
Embodiment 2
Adopt supper micron mill that the tea dregs of rice of carrying after oil are carried out to micronizing and cross 500 mesh sieves, take 250g tea dregs of rice powder, then add 2000ml distilled water, under the condition of 60 DEG C of constant temperature, ultrasonic Assisted Extraction 20min.Adjusting ultrasonic frequency is 40kHz, and ultrasonic power is 800w.After lixiviate completes, centrifugation, residue adds water 500ml lixiviate once more as stated above, merges twice vat liquor.All the other implementation steps are with identical described in embodiment 1.Finally obtain tea saponin finished product 24.57g, purity is 96.79%.The rate of recovery of gained tea saponin is 94.1%.
Claims (4)
1. the auxiliary water alcohol method of tea dregs of rice micronizing and ultrasonic wave extracts a method for tea saponin, it is characterized in that step is as follows:
(1) adopt supper micron mill to pulverize and be less than 500 object tea dregs of rice powder for particle diameter carrying the tea dregs of rice after oil.
(2) use the aqueous solution 60 DEG C of constant temperature in tea dregs of rice powder, ultrasonic frequency 20kHz～40kHz, lixiviate 20～60min under the condition of ultrasonic power 400w～800w, obtains tea saponin vat liquor after centrifugation.Precipitate water with equally carrying out secondary lixiviate above, the centrifugal vat liquor that obtains, merges twice vat liquor again.
(3) in the vat liquor of collecting, add the flocculation of 5～10% flocculation agent, centrifugal, remove precipitation, obtain clarified liq.
(4) in clarified liq, add 95% ethanol as extraction solvent, under the condition of 50 DEG C of constant temperature, extract 1.5～3h, after centrifugation, obtain tea saponin extraction liquid.
(5) tea saponin extraction liquid is carried out reclaiming ethanol after concentrating under reduced pressure.After solution after to be concentrated is cooling, add 5～10% flocculation agent flocculation, after centrifugation, obtain clarified liq.
(6) by extremely white or faint yellow of activated carbon decolorizing for gained clarified liq, obtain destainer.Then by the dry destainer tea saponin finished product that obtains.
2. require described tea dregs of rice micronizing and the auxiliary water alcohol method of ultrasonic wave to extract the method for tea saponin according to right 1, it is characterized in that: described tea dregs of rice powder and aqueous solution mass ratio are 1: 8.
3. require described tea dregs of rice micronizing and the auxiliary water alcohol method of ultrasonic wave to extract the method for tea saponin according to right 1, it is characterized in that: described flocculation agent is 1% chitosan solution, flocculating conditions is bath temperature 50-65 DEG C, leaves standstill 2h.
4. require described tea dregs of rice micronizing and the auxiliary water alcohol method of ultrasonic wave to extract the method for tea saponin according to right 1, it is characterized in that: the volume ratio of described vat liquor and extraction solvent 95% ethanol is 1: 0.5.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201310023109.2A CN103936811A (en) | 2013-01-18 | 2013-01-18 | Tea seed meal superfine grinding and ultrasonic-assisted water-alcohol method for extraction of tea saponin |
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| CN201310023109.2A CN103936811A (en) | 2013-01-18 | 2013-01-18 | Tea seed meal superfine grinding and ultrasonic-assisted water-alcohol method for extraction of tea saponin |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106967144A (en) * | 2017-03-28 | 2017-07-21 | 钦州市桂耘贸易有限公司 | A kind of method that Tea Saponin is extracted from tea bran |
| CN107056876A (en) * | 2017-05-22 | 2017-08-18 | 江西乔盛茶皂素科技有限公司 | A kind of method that high-purity tea saponin is extracted from camellia seed meal |
| CN107468597A (en) * | 2017-10-09 | 2017-12-15 | 三江县稻香山茶油生态发展有限公司 | One plant tea bran shampoo and preparation method thereof |
| CN108003215A (en) * | 2017-12-25 | 2018-05-08 | 华远医药研究院有限公司 | The cleaning extracting method of Tea Saponin |
| CN109627280A (en) * | 2019-01-18 | 2019-04-16 | 宜春学院 | A kind of extracting method of Tea Saponin |
| CN110724595A (en) * | 2019-10-11 | 2020-01-24 | 浙江久晟油茶科技股份有限公司 | Biological polysaccharide flocculant and preparation method and application thereof |
| CN112194700A (en) * | 2020-10-09 | 2021-01-08 | 张利民 | Preparation method of natural high-purity tea saponin with high decontamination efficiency |
-
2013
- 2013-01-18 CN CN201310023109.2A patent/CN103936811A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106967144A (en) * | 2017-03-28 | 2017-07-21 | 钦州市桂耘贸易有限公司 | A kind of method that Tea Saponin is extracted from tea bran |
| CN107056876A (en) * | 2017-05-22 | 2017-08-18 | 江西乔盛茶皂素科技有限公司 | A kind of method that high-purity tea saponin is extracted from camellia seed meal |
| CN107056876B (en) * | 2017-05-22 | 2019-05-24 | 江西乔盛茶皂素科技有限公司 | A method of extracting high-purity tea saponin from camellia seed meal |
| CN107468597A (en) * | 2017-10-09 | 2017-12-15 | 三江县稻香山茶油生态发展有限公司 | One plant tea bran shampoo and preparation method thereof |
| CN108003215A (en) * | 2017-12-25 | 2018-05-08 | 华远医药研究院有限公司 | The cleaning extracting method of Tea Saponin |
| CN109627280A (en) * | 2019-01-18 | 2019-04-16 | 宜春学院 | A kind of extracting method of Tea Saponin |
| CN109627280B (en) * | 2019-01-18 | 2021-05-11 | 宜春学院 | Extraction method of tea saponin |
| CN110724595A (en) * | 2019-10-11 | 2020-01-24 | 浙江久晟油茶科技股份有限公司 | Biological polysaccharide flocculant and preparation method and application thereof |
| CN112194700A (en) * | 2020-10-09 | 2021-01-08 | 张利民 | Preparation method of natural high-purity tea saponin with high decontamination efficiency |
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Application publication date: 20140723 |