CN104974211A - Method for extracting beta-sitosterol from waste kaolin and detection method by thin-layer chromatography - Google Patents
Method for extracting beta-sitosterol from waste kaolin and detection method by thin-layer chromatography Download PDFInfo
- Publication number
- CN104974211A CN104974211A CN201510438711.1A CN201510438711A CN104974211A CN 104974211 A CN104974211 A CN 104974211A CN 201510438711 A CN201510438711 A CN 201510438711A CN 104974211 A CN104974211 A CN 104974211A
- Authority
- CN
- China
- Prior art keywords
- sitosterol
- extract
- thin
- liquid
- add
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Abstract
The invention discloses a method for extracting beta-sitosterol from waste kaolin, which comprises the following steps: (1) extracting waste kaolin, which is used after a grease processing technique, with acetone, filtering, and evaporating to remove the acetone, thereby obtaining grease; and (2) heating the grease in a water bath by using a 5% concentrated sulfuric acid-ethanol solution, extracting under extraction, evaporating to remove the solvent, adding an 80% ethanol solution and sodium hydroxide, heating under reflux for saponification, adding deionized water and petroleum ether into the saponified liquid, oscillating for extraction, stratifying, taking the petroleum ether layer, reextracting, merging the extracts, washing with deionized water to a neutral state, and evaporating to remove the petroleum ether, thereby obtaining the beta-sitosterol extract. The invention also discloses a method for detecting beta-sitosterol by thin-layer chromatography scanning. The method extracts the beta-sitosterol from waste kaolin generated in the grease working process for the first time, is simple in extraction process, can implement waste reutilization, and has higher economical and environmental benefits.
Description
Technical field
The present invention relates to a kind of from fats and oils processing gives up white bole, extract β-sitosterol method and thin-layer chromatography detection method.
Background technology
Sterol is a kind of steroide, comprises plant sterol, zoosterol and mushroom sterol three major types.Wherein plant sterol is a kind of natural active matter, is extensively present in natural plant.Natural plant sterol mainly comprises β-sitosterol, Stigmasterol, brassicasterol and campesterol four kinds, wherein maximum with β-sitosterol content in Semen Maydis oil.
Many experimental results shows, the plant sterols such as β-sitosterol have important physiologically active: 1. effectively can reduce cholesterol in serum (no matter being sequestered or ester type) level, play the effect of the cardiovascular disordeies such as prevention and therapy hypertension, coronary heart disease; 2. can promote to produce profibr(in)olysin incitant, can be used as fibrin and dissolve triggering element, play the effect of prevention thrombosis; 3. there is anti-inflammatory action; 4. there is the effect of bringing down a fever of similar acetylsalicylic acid (Asprin); 5. have the function blocking Induced by Carcinogen cancer cells and formed, anticancer effect is remarkable; 6. molecular structure makes it have stronger percutaneous permeability, promotes sebum secretion and gentle keeps moisture, remaining wetting, soft physiologically active and surfactivity.
The plant sterols such as β-sitosterol are widely used in field of medicaments, cosmetic industry, fodder industry, food.In Japan, occur containing the β-sitosterol of 60% and the medicine of tocopherol mixing, as the commodity selling reducing serum cholesterol.The compound Sitosterol sheet that other drug composition makes is mixed by Sitosterol, there are good serum cholesterol-lowering and reducing blood lipid, can the development of atherosclerosis, all there is therapeutic action to hyperlipidemia, coronary atherosclerotic heart disease, uncomfortable in chest, palpitaition etc.In addition, Sitosterol ointment demonstrates certain superiority in treatment cervical cancer, skin carcinoma.
Useless white bole is as a kind of tankage produced in course of oil processing, less for its research at present, how directly to abandon as waste.If therefrom can go out β-sitosterol by extraction and isolation, and develop it, its economic benefit, social benefit can be very remarkable, have wide DEVELOPMENT PROSPECT.
Summary of the invention
For above-mentioned prior art, the object of this invention is to provide a kind of from fats and oils processing gives up white bole, extract β-sitosterol method and thin-layer chromatography detection method.
For achieving the above object, the present invention adopts following technical proposals:
From useless white bole, extract a method for β-sitosterol, step is as follows:
(1) adopt acetone to extract the useless white bole after use in grease processing technique, filter, steam except acetone, obtain oily matter;
(2) oily matter of step (1) vitriol oil-ethanolic soln of 5% (percent by volume) is carried out heating in water bath, refluxing extraction, steaming desolventizes, add ethanolic soln, the sodium hydroxide of 80% (percent by volume) again, reflux saponification, deionized water, sherwood oil is added in the liquid after saponification, concussion extraction, petroleum ether layer is got after layering, re-extract, combining extraction liquid, and with deionized water wash to neutral, steam except sherwood oil, obtain β-sitosterol extract.
In step (1), the add-on of acetone is useless kaolinic 2-4 times of quality volume (amount namely adding acetone in every gram of useless white bole is 2-4mL); Preferably, the add-on of acetone is useless kaolinic 3 times of quality volumes.
In step (1), adding the number of times that acetone carries out extracting is 3 times.
In step (2), the add-on of the vitriol oil-ethanolic soln and the ratio of oily matter are (8-12) mL:1g, are preferably 10mL:1g; The add-on of ethanolic soln and the ratio of oily matter are (3-8) mL:1g, are preferably 5mL:1g; The add-on of sodium hydroxide and the mass ratio of oily matter are 5:(16-17).
In step (2), adding the temperature that the vitriol oil-ethanolic soln carries out heating in water bath is 80 DEG C, and the time of refluxing extraction is 6 hours.
In step (2), the temperature of reflux saponification is 80 DEG C, and the time is 2 hours.The temperature and time of reflux saponification all can have an impact to the effect of saponification, and the too high meeting of saponification temperature makes target substance decompose, and saponification temperature is too low, can extend the time of saponification, adopts saponification temperature of the present invention and saponification time, and saponification effect is ideal.
In step (2), during concussion extraction, deionized water is all identical with the liquid volume after saponification with the add-on of sherwood oil.
Present invention also offers a kind of thin-layer chromatography scanning detection method of β-sitosterol, step is as follows:
(1) by β-sitosterol extract anhydrous alcohol solution, make sample liquid, by β-sitosterol standard substance anhydrous alcohol solution, make reference liquid;
(2) the β-sitosterol reference liquid of different mass and sample liquid are put respectively in same High Performance Thin silica-gel plate GF
254on, add developping agent, pre-equilibration, after silica-gel plate is put into expansion cylinder, ascending development, exhibition is dried apart from taking out when reaching 8 ㎝, and staining fluid rinses dyeing subsequently, dries colour developing;
(3) thin layer chromatography scanner carries out thin layer scanning, obtains β-sitosterol R
f(Rf value) and integrating peak areas value; Draw β-sitosterol reference liquid quality and integrating peak areas value relation by thin layer chromatograph management software winCATS 1.4.1, the integrating peak areas value of liquid calculates the quality of sample liquid β-sitosterol per sample.
In step (2), the β-sitosterol reference liquid of different mass is 6 kinds of mass gradient, is respectively 50ng, 100ng, 150ng, 300ng, 350ng, 400ng.
In step (2), developping agent is normal hexane: ether: chloroform: acetic acid: toluene, and volume ratio is (3 ~ 5): (0.5 ~ 1.5): (2 ~ 4): (0.1 ~ 0.3): (1 ~ 2).Developping agent is the key factor affecting thin layer detected result, and the present invention carries out screening repeatedly and optimization to the composition of developping agent and proportioning, adopts developping agent of the present invention, can the separation of effective realize target material, the R of target substance
fvalue is suitable.
In step (2), described staining fluid is mixed by 1g:20mL by phospho-molybdic acid and acetic acid.
Beneficial effect of the present invention:
(1) extract in the useless white bole that system of the present invention produces first from course of oil processing and obtain β-sitosterol, extracting method is simple, can realize the recycling of refuse, have higher economy and environmental benefit; Present invention also offers a kind of detection method of β-sitosterol, there is the advantages such as simple, quick, accurate, stable, can be used for the detection of any one containing β-sitosterol content in the starting material of β-sitosterol, product and byproduct, in β-sitosterol exploitation, there is extensive, important using value.
(2) the useless white bole after adopting method of the present invention to extract β-sitosterol, can be reused for the machining process of grease.
Embodiment
Below by specific examples, the present invention will be further elaborated, should be noted that following explanation is only to explain the present invention, not limiting its content.
Embodiment 1: the isolation and determination of β-sitosterol in useless white bole
(1) extraction of β-sitosterol
Take the useless white bole 50g produced in Semen Maydis oil decoloration process, add 150ml acetone, extract 3 times, stratification, steam after united extraction liquid except acetone obtains oily matter 16.575g.180ml 5% (percent by volume) vitriol oil-ethanolic soln is added, 80 DEG C of heating in water bath, back flow reaction 6 hours in oily matter; Steaming desolventizes, and adds 50ml 80% (percent by volume) ethanol and 5g NaOH, 80 DEG C of reflux saponification 2h.Add respectively and the deionized water of saponification liquor same volume, sherwood oil, concussion extraction, gets petroleum ether layer after layering, three times so repeatedly.Combining extraction liquid, adds deionized water and is washed till neutrality, and petroleum ether layer rotary evaporation removes sherwood oil, obtains β-sitosterol extract, adds dehydrated alcohol constant volume and obtain sample liquid 9.6ml.
(2) detection of β-sitosterol
Precision takes β-sitosterol standard substance (Sigma company) 0.2mg, adds dehydrated alcohol and is settled to 2ml, makes the reference liquid that concentration is 0.1mg/ml.Accurate absorption 0.5,1,1.5,3,3.5,4ul β-sitosterol reference liquid and 2.5ul sample liquid point are in same High Performance Thin silica-gel plate GF
254on (10cm × 10cm), add 10ml developping agent, developping agent is normal hexane: ether: chloroform: acetic acid: toluene=4:1:3:0.2:1.5 (V/V/V/V/V), pre-equilibration 20 minutes, plate is put into expansion cylinder (12cm × 15cm × 10cm), ascending development, exhibition is apart from 8 ㎝, taking-up is dried, dyeing is rinsed with 10ml staining fluid, prescription of its dyeing liquor is: phospho-molybdic acid: acetic acid=5g:100ml, dry colour developing 5min for 105 DEG C, visual standard product and sample two points in same level align and are all dyed to blueness, Camag 3 type thin layer chromatography scanner is utilized to carry out thin-layer chromatography scanning under 650nm absorbing wavelength, sweep velocity is 20mm/s, data resolution is 50um/step, obtain R
f=0.38, irradiation light is tungsten lamp, carry out detection computations, with the quality of β-sitosterol standard substance (ng) for X-coordinate (X), integrating peak areas value (AU) is ordinate zou (Y), is directly obtained the regression equation of standard substance and integrating peak areas value relation by thin layer chromatograph management software winCATS 1.4.1:
Y＝6959.4165+53.9858X，r＝0.99938，RSD＝1.60％。
Result shows, sample liquid is good in 50 ~ 400ng scope internal linear, and in 2.5ul sample liquid, the content of β-sitosterol is 247ng, as calculated in 9.6ml extracting solution containing β-sitosterol 948.48ug, namely the 50g content of β-sitosterol in white bole that gives up is 948.48ug.
Embodiment 2:
The extracting method of β-sitosterol is with embodiment 1; The difference of detection method and embodiment 1 is: developping agent is 15ml, developping agent is normal hexane: ether: chloroform: acetic acid: toluene=3:0.5:2:0.1:1 (V/V/V/V/V), staining agent 8ml, obtains 9.6ml sample liquid (i.e. 50g give up white bole) containing β-sitosterol average out to 927.06ug according to the equation of linear regression of embodiment 1.
Embodiment 3:
The extracting method of β-sitosterol is with embodiment 1; The difference of detection method and embodiment 1 is: developping agent is 12ml, developping agent is normal hexane: ether: chloroform: acetic acid: toluene=5:1.5:4:0.3:2 (V/V/V/V/V), staining agent 12ml, obtains 9.6ml sample liquid (i.e. 50g give up white bole) containing β-sitosterol average out to 931.21ug according to the equation of linear regression of embodiment 1.
Embodiment 4:
Take the useless white bole 50g produced in Semen Maydis oil decoloration process, add 100ml acetone, extract 3 times, stratification, steam except acetone after united extraction liquid, obtain oily matter 16.146g.130ml 5% (percent by volume) vitriol oil-ethanolic soln is added, 80 DEG C of heating in water bath, back flow reaction 6 hours in oily matter; Steaming desolventizes, and adds 100ml 80% (percent by volume) ethanol and 5g NaOH, 80 DEG C of reflux saponification 2h.Add respectively and the deionized water of saponification liquor same volume, sherwood oil, concussion extraction, gets petroleum ether layer after layering, three times so repeatedly.Combining extraction liquid, adds deionized water and is washed till neutrality, and petroleum ether layer rotary evaporation removes sherwood oil, obtains β-sitosterol extract, adds dehydrated alcohol constant volume and obtain sample liquid 9.6ml.
Calculate according to the detection method of embodiment 1, obtain 9.6ml sample liquid (i.e. 50g give up white bole) containing β-sitosterol average out to 934.13ug.
Embodiment 5:
Take the useless white bole 50g produced in Semen Maydis oil decoloration process, add 200ml acetone, extract 3 times, stratification, steam except acetone after united extraction liquid, obtain oily matter 16.684g.200ml 5% (percent by volume) vitriol oil-ethanolic soln is added, 80 DEG C of heating in water bath, back flow reaction 6 hours in oily matter; Steaming desolventizes, and adds 50ml 80% (percent by volume) ethanol and 5gNaOH, 80 DEG C of reflux saponification 2h.Add respectively and the deionized water of saponification liquor same volume, sherwood oil, concussion extraction, gets petroleum ether layer after layering, three times so repeatedly.Combining extraction liquid, adds deionized water and is washed till neutrality, and petroleum ether layer rotary evaporation removes sherwood oil, obtains β-sitosterol extract, adds dehydrated alcohol constant volume and obtain sample liquid 9.6ml.
Calculate according to the detection method of embodiment 1, obtain 9.6ml sample liquid (i.e. 50g give up white bole) containing β-sitosterol average out to 942.26ug.
Embodiment 6:
Take the useless white bole 50g produced in soybean oil decoloration process, add 150ml acetone, extract 3 times, stratification, steam except acetone after united extraction liquid, obtain oily matter 16.410g.180ml 5% (percent by volume) vitriol oil-ethanolic soln is added, 80 DEG C of heating in water bath, back flow reaction 6 hours in oily matter; Steaming desolventizes, and adds 80ml 80% (percent by volume) ethanol and 5gNaOH, 80 DEG C of reflux saponification 2h.Add respectively and the deionized water of saponification liquor same volume, sherwood oil, concussion extraction, gets petroleum ether layer after layering, three times so repeatedly.Combining extraction liquid, adds deionized water and is washed till neutrality, and petroleum ether layer rotary evaporation removes sherwood oil, obtains β-sitosterol extract, adds dehydrated alcohol constant volume and obtain sample liquid 9.6ml.
Calculate according to the detection method of embodiment 1, obtain 9.6ml sample liquid (i.e. 50g give up white bole) containing β-sitosterol average out to 952.22ug.
Embodiment 7:
Take the useless white bole 50g produced in soybean oil decoloration process, add 100ml acetone, extract 3 times, stratification, steam except acetone after united extraction liquid, obtain oily matter 16.231g.130ml 5% (percent by volume) vitriol oil-ethanolic soln is added, 80 DEG C of heating in water bath, back flow reaction 6 hours in oily matter; Steaming desolventizes, and adds 50ml 80% (percent by volume) ethanol and 5gNaOH, 80 DEG C of reflux saponification 2h.Add respectively and the deionized water of saponification liquor same volume, sherwood oil, concussion extraction, gets petroleum ether layer after layering, three times so repeatedly.Combining extraction liquid, adds deionized water and is washed till neutrality, and petroleum ether layer rotary evaporation removes sherwood oil, obtains β-sitosterol extract, adds dehydrated alcohol constant volume and obtain sample liquid 9.6ml.
Calculate according to the detection method of embodiment 1, obtain 9.6ml sample liquid (i.e. 50g give up white bole) containing β-sitosterol average out to 947.34ug.
Claims (10)
1. from useless white bole, extract a method for β-sitosterol, it is characterized in that, step is as follows:
(1) adopt acetone to extract the useless white bole after use in grease processing technique, filter, steam except acetone, obtain oily matter;
(2) the oily matter vitriol oil-ethanolic soln of step (1) is carried out heating in water bath, refluxing extraction, steaming desolventizes, add ethanolic soln, sodium hydroxide again, reflux saponification, adds deionized water, sherwood oil in the liquid after saponification, extraction, petroleum ether layer is got after layering, re-extract, combining extraction liquid, and with deionized water wash to neutral, steam except sherwood oil, obtain β-sitosterol extract.
2. from useless white bole, extract the method for β-sitosterol as claimed in claim 1, it is characterized in that, in step (1), the add-on of acetone is useless kaolinic 2-4 times of quality volume.
3. from useless white bole, extract as claimed in claim 1 the method for β-sitosterol, it is characterized in that, in step (1), adding the number of times that acetone carries out extracting is 3 times.
4. from useless white bole, extract the method for β-sitosterol as claimed in claim 1, it is characterized in that, in step (2), the add-on of the vitriol oil-ethanolic soln and the ratio of oily matter are (8-12) mL:1g; The add-on of ethanolic soln and the ratio of oily matter are (3-8) mL:1g; The add-on of sodium hydroxide and the mass ratio of oily matter are 5:(16-17).
5. from useless white bole, extract as claimed in claim 1 the method for β-sitosterol, it is characterized in that, in step (2), adding the temperature that the vitriol oil-ethanolic soln carries out heating in water bath is 80 DEG C, and the time of refluxing extraction is 6 hours;
The temperature of reflux saponification is 80 DEG C, and the time is 2 hours.
6. from useless white bole, extract the method for β-sitosterol as claimed in claim 1, it is characterized in that, in step (2), deionized water is all identical with the liquid volume after saponification with the add-on of sherwood oil.
7. a thin-layer chromatography scanning detection method for β-sitosterol, it is characterized in that, step is as follows:
(1) the β-sitosterol extract anhydrous alcohol solution obtained by the extracting method according to any one of claim 1-6, makes sample liquid, by β-sitosterol standard substance anhydrous alcohol solution, makes reference liquid;
(2) the β-sitosterol reference liquid of different mass and sample liquid are put respectively on same thin-layer silicon offset plate, add developping agent, pre-equilibration, after silica-gel plate is put into expansion cylinder, ascending development, dry, staining fluid rinse dyeing, dry colour developing;
(3) thin layer chromatography scanner carries out thin layer scanning, obtains β-sitosterol R
fwith integrating peak areas value; Draw β-sitosterol reference liquid quality and integrating peak areas value relation, the integrating peak areas value of liquid calculates the quality of sample liquid β-sitosterol per sample.
8. the thin-layer chromatography scanning detection method of β-sitosterol as claimed in claim 7, it is characterized in that, in step (2), the β-sitosterol reference liquid of different mass is 6 kinds of mass gradient, be respectively 50ng, 100ng, 150ng, 300ng, 350ng, 400ng.
9. the thin-layer chromatography scanning detection method of β-sitosterol as claimed in claim 7, it is characterized in that, in step (2), developping agent is normal hexane: ether: chloroform: acetic acid: toluene, and volume ratio is (3 ~ 5): (0.5 ~ 1.5): (2 ~ 4): (0.1 ~ 0.3): (1 ~ 2).
10. the thin-layer chromatography scanning detection method of β-sitosterol as claimed in claim 7, it is characterized in that, in step (2), described staining fluid is mixed by 1g:20mL by phospho-molybdic acid and acetic acid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510438711.1A CN104974211B (en) | 2015-07-23 | 2015-07-23 | Method for extracting beta-sitosterol from waste kaolin and detection method by thin-layer chromatography |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510438711.1A CN104974211B (en) | 2015-07-23 | 2015-07-23 | Method for extracting beta-sitosterol from waste kaolin and detection method by thin-layer chromatography |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104974211A true CN104974211A (en) | 2015-10-14 |
| CN104974211B CN104974211B (en) | 2017-05-24 |
Family
ID=54271215
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510438711.1A Expired - Fee Related CN104974211B (en) | 2015-07-23 | 2015-07-23 | Method for extracting beta-sitosterol from waste kaolin and detection method by thin-layer chromatography |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104974211B (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110530835A (en) * | 2019-09-27 | 2019-12-03 | 山西省农业科学院农产品加工研究所 | The Fluorometric assay method of phthalic ester plasticizer in oily substance |
| CN110632237A (en) * | 2019-09-26 | 2019-12-31 | 吕梁学院 | Method for evaluating oxidation resistance of phytosterol in red dates by applying TLC-CMS (thin layer chromatography-sodium carboxymethyl cellulose) technology |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3332969A (en) * | 1965-09-13 | 1967-07-25 | Owens Illinois Inc | Process for the recovery of beta-sitosterol from vegetable matter |
| CN1400298A (en) * | 2002-04-16 | 2003-03-05 | 李大鹏 | Fruit kernel oil extracted from plant fruit kernel, its extraction method, medicinal composite and application |
| CN101367860A (en) * | 2008-09-27 | 2009-02-18 | 南京工业大学 | Method for separating and extracting beta-sitosterol from mixed phytosterin |
| CN103940654A (en) * | 2014-05-06 | 2014-07-23 | 山东师范大学 | Method for extracting vitamin E from waste kaolin and thin layer chromatography detection method |
-
2015
- 2015-07-23 CN CN201510438711.1A patent/CN104974211B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3332969A (en) * | 1965-09-13 | 1967-07-25 | Owens Illinois Inc | Process for the recovery of beta-sitosterol from vegetable matter |
| CN1400298A (en) * | 2002-04-16 | 2003-03-05 | 李大鹏 | Fruit kernel oil extracted from plant fruit kernel, its extraction method, medicinal composite and application |
| CN101367860A (en) * | 2008-09-27 | 2009-02-18 | 南京工业大学 | Method for separating and extracting beta-sitosterol from mixed phytosterin |
| CN103940654A (en) * | 2014-05-06 | 2014-07-23 | 山东师范大学 | Method for extracting vitamin E from waste kaolin and thin layer chromatography detection method |
Non-Patent Citations (4)
| Title |
|---|
| 彭莹 等: "天然植物甾醇的应用与提取工艺", 《化工进展》 * |
| 曹莹 等: "植物甾醇提取方法研究进展", 《粮油食品科技》 * |
| 杨振强等: "植物甾醇的开发与应用研究进展", 《粮油加工与食品机械》 * |
| 管伟举 等: "植物甾醇研究进展", 《粮食与油脂》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110632237A (en) * | 2019-09-26 | 2019-12-31 | 吕梁学院 | Method for evaluating oxidation resistance of phytosterol in red dates by applying TLC-CMS (thin layer chromatography-sodium carboxymethyl cellulose) technology |
| CN110632237B (en) * | 2019-09-26 | 2021-10-08 | 吕梁学院 | Method for evaluating oxidation resistance of phytosterol in red dates by applying TLC-CMS (thin layer chromatography-sodium carboxymethyl cellulose) technology |
| CN110530835A (en) * | 2019-09-27 | 2019-12-03 | 山西省农业科学院农产品加工研究所 | The Fluorometric assay method of phthalic ester plasticizer in oily substance |
| CN110530835B (en) * | 2019-09-27 | 2022-03-04 | 山西省农业科学院农产品加工研究所 | Fluorescence method detection method for phthalate plasticizer in oil substances |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104974211B (en) | 2017-05-24 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Lin et al. | Macroporous resin purification behavior of phenolics and rosmarinic acid from Rabdosia serra (MAXIM.) HARA leaf | |
| CN105175465B (en) | A method of extracting ginko leaves flavone | |
| CN103520233B (en) | The Preparation method and use of a kind of Folium Apocyni Veneti total polyphenols | |
| CN103211732A (en) | Preparation method and application of mixture with tyrosinase inhibitory activity | |
| CN101239962B (en) | Method for extracting proanthocyanidins from cranberry | |
| CN1994997B (en) | Method for separating and purifying 6-gingerol | |
| CN103725420B (en) | A kind of extract the method for Nigella damascena L. platymiscium Volatile Oil from Seed, device and application | |
| US20020038020A1 (en) | Process for extracting glycoside using an aqueous two-phase system | |
| CN104974211A (en) | Method for extracting beta-sitosterol from waste kaolin and detection method by thin-layer chromatography | |
| Fan et al. | Ionic liquid-based microwave-assisted extraction of verbascoside from Rehmannia root | |
| CN104569192B (en) | A kind of quality determining method of Flemingia macrophylla | |
| CN103349637A (en) | Compound traditional Chinese medicine extract with effects of whitening and moisturizing, preparation method and application thereof | |
| CN101955479A (en) | Method for extracting orientin from bamboo leaf | |
| Zhang et al. | Extraction of isoflavones from Puerariae lobata using subcritical water | |
| CN104370992B (en) | A kind of from Glossy Privet Fruit, extract ursolic acid and the method for Oleanolic Acid mixture | |
| CN103102255A (en) | Method for separating and purifying four phloroglucinol compounds from dryopteris fragrans | |
| CN101407536B (en) | Process for preparing high-purity asiaticoside by solvent crystallization | |
| CN104398557A (en) | Method for preparing general flavones by using complexing method | |
| JPH01175978A (en) | Production of crude catechin compound | |
| CN104807944A (en) | Preparing method of scorzonera general flavone and finger-print map thereof | |
| CN103467539A (en) | Method for extracting rosavin from Rhodiola rosea | |
| CN108947944A (en) | A kind of application of tyrosinase inhibitor ginger florigen A in face cream, facial cleanser or whitening emulsion | |
| CN101648936A (en) | Chemical composition separation method of traditional Chinese medicine smilax composition and clinical application thereof | |
| CN101863957B (en) | Method for synchronously extracting tanshinone IIA and salvianolic acid B from danshen root efficiently | |
| CN107510629A (en) | Extraction process, belamcanda chinensis extract and its application of belamcanda chinensis extract and moisturizing cream |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20170524 Termination date: 20180723 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |