CN104974211B - 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
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- CN104974211B CN104974211B CN201510438711.1A CN201510438711A CN104974211B CN 104974211 B CN104974211 B CN 104974211B CN 201510438711 A CN201510438711 A CN 201510438711A CN 104974211 B CN104974211 B CN 104974211B
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- cupreol
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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
Method and thin-layer chromatography detection side the present invention relates to extract cupreol in a kind of useless white bole from fats and oils processing
Method.
Background technology
Sterol is a kind of steroid, including phytosterol, zoosterol and mushroom sterol three major types.Wherein plant steroid
Alcohol is a kind of natural active matter, is widely present in the plant of nature.Natural phytosterol mainly include cupreol,
Four kinds of stigmasterol, brassicasterol and campesterol, it is maximum with cupreol content wherein in corn oil.
Many experimental results show that the phytosterol such as cupreol has important physiologically active：1. blood can effectively be reduced
Cholesterine (either sequestered or ester type) level in clear, plays the angiocardiopathies such as prevention and treatment hypertension, coronary heart disease
Effect；2. can promote to produce plasminogen activity factor, prevention blood can be played as fibrin dissolving triggering element
The effect of bolt disease；3. there is antiinflammatory action；4. there is the effect of bringing down a fever of similar acetylsalicylic acid (aspirin)；5. there is blocking
The function that Induced by Carcinogen cancer cell is formed, anticancer effect is notable；6. molecular structure makes it have stronger percutaneous permeability, promotees
Enter sebum secretion and gentle holding moisture, maintain wetting, soft physiologically active and surface-active.
The phytosterols such as cupreol are widely used in field of medicaments, cosmetics industry, feed industry, food.In day
, has there is the medicine containing 60% cupreol and tocopherol mixing, as the commodity selling of reduce serum cholesterol in this.By paddy
Sterol mixes the compound sitosterol piece that other drugs composition is made, and has good serum cholesterol-lowering and effect for reducing blood fat, can prevent
The development of stop pulse atherosclerosis, has therapeutic action to hyperlipemia, coronary arteriosclerotic cardiopathy, uncomfortable in chest, palpitaition etc..
In addition, sitosterol ointment shows certain superiority in terms for the treatment of cervical carcinoma, cutaneum carcinoma.
Useless white bole is used as a kind of leftover bits and pieces produced in course of oil processing, less for its research at present, many conducts
Discarded object is directly abandoned.If can therefrom extract and isolate cupreol, and it is developed, its economic benefit, society's effect
Benefit can very significantly, with wide DEVELOPMENT PROSPECT.
The content of the invention
For above-mentioned prior art, β-paddy steroid is extracted from the useless white bole of fats and oils processing it is an object of the invention to provide one kind
The method and thin-layer chromatography detection method of alcohol.
To achieve the above object, the present invention uses following technical proposals：
A kind of method that cupreol is extracted from useless white bole, step is as follows：
(1) by use in grease processing technique after useless white bole extracted using acetone, filter, acetone is evaporated off, obtain
Grease；
(2) grease of step (1) is carried out into heating water bath with the concentrated sulfuric acid-ethanol solution of 5% (percentage by volume), is returned
Stream is extracted, and solvent is evaporated off, and adds ethanol solution, the NaOH of 80% (percentage by volume), saponification is heated to reflux, to saponification
Deionized water, petroleum ether are added in liquid afterwards, concussion extraction takes petroleum ether layer, repeats to extract, combining extraction liquid after layering,
And be washed with deionized to neutrality, petroleum ether is evaporated off, obtain final product cupreol extract.
In step (1), the addition of acetone is the 2-4 times of quality volume (addition in i.e. every gram useless white bole of useless white bole
The amount of acetone is 2-4mL)；Preferably, the addition of acetone is 3 times of quality volumes of useless white bole.
In step (1), the number of times for adding acetone to be extracted is 3 times.
In step (2), the addition of the concentrated sulfuric acid-ethanol solution and the ratio of grease are (8-12) mL:1g, preferably
10mL:1g；The addition of ethanol solution and the ratio of grease are (3-8) mL:1g, preferably 5mL:1g；The addition of NaOH
Amount is 5 with the mass ratio of grease：(16-17).
In step (2), the temperature that adding the concentrated sulfuric acid-ethanol solution carries out heating water bath is 80 DEG C, the time of refluxing extraction
It is 6 hours.
In step (2), it is 80 DEG C to be heated to reflux the temperature of saponification, and the time is 2 hours.Be heated to reflux saponification temperature and when
Between influence can be all produced on the effect of saponification, saponification temperature is too high to decompose target substance, and saponification temperature is too low, can extend soap
The time of change, using saponification temperature of the invention and saponification time, saponification effect is ideal.
In step (2), during concussion extraction, the addition of deionized water and petroleum ether with saponification after liquid volume phase
Together.
Present invention also offers a kind of thin-layer chromatography scanning detection method of cupreol, step is as follows：
(1) by cupreol extract anhydrous alcohol solution, sample liquid is made, by the anhydrous second of cupreol standard items
Alcohol dissolves, and is made titer；
(2) the cupreol titer and sample liquid of different quality are put in same High Performance Thin silica gel plate GF respectively254
On, add solvent, pre-equilibration, after silica gel plate is put into expansion cylinder, ascending development, exhibition is dried away from being taken out when reaching 8 ㎝, then
Dyeing liquor rinses dyeing, drying colour developing；
(3) thin-layer chromatogram scanner carries out thin layer scanning, obtains cupreol Rf(Rf value) and integrating peak areas value；By thin layer
Chromatograph management software winCATS 1.4.1 draw cupreol titer quality and integrating peak areas value relation, according to sample
The integrating peak areas value of liquid calculates the quality of sample liquid cupreol.
In step (2), the cupreol titer of different quality is 6 kinds of mass gradients, respectively 50ng, 100ng,
150ng, 300ng, 350ng, 400ng.
In step (2), solvent is n-hexane：Ether：Chloroform：Acetic acid：Toluene, volume ratio is (3~5):(0.5~
1.5)：(2~4)：(0.1~0.3)：(1~2).Solvent is the key factor for influenceing thin layer testing result, and the present invention is to launching
The composition and proportioning of agent have carried out multiple screening and optimization, using solvent of the invention, can effectively realize object
The separation of matter, the R of target substancefValue is suitable.
In step (2), the dyeing liquor is by 1g by phosphomolybdic acid and acetic acid:20mL is mixed.
Beneficial effects of the present invention：
(1) extracted in the useless white bole that present invention system produces from course of oil processing first and obtain cupreol, extracted
Method is simple, the recycling of waste is capable of achieving, with economical and environmentally friendly benefit higher；Present invention also offers a kind of β-paddy steroid
The detection method of alcohol, have the advantages that it is simple, quick, accurate, stable, can be used for any raw material containing cupreol,
The detection of cupreol content in product and byproduct, has extensive, important application value in cupreol exploitation.
(2) the useless white bole after cupreol is extracted using the method for the present invention, the processing work of grease can be reused for
Skill process.
Specific embodiment
Below by instantiation, the present invention will be further elaborated, it should explanation, the description below be only for
The present invention is explained, its content is not defined.
Embodiment 1：The extraction and detection of cupreol in useless white bole
(1) extraction of cupreol
The useless white bole 50g produced in corn oil decoloration process, plus 150ml acetone are weighed, is extracted 3 times, stratification, closed
And acetone is evaporated off after extract solution obtains grease 16.575g.To in grease add 180ml 5% (percentage by volume) concentrated sulfuric acid-
Ethanol solution, 80 DEG C of heating water baths, back flow reaction 6 hours；Solvent is evaporated off, 50ml 80% (percentage by volume) ethanol is added
With 5g NaOH, 80 DEG C are heated to reflux saponification 2h.Deionized water, petroleum ether respectively plus with saponification liquor same volume, concussion extraction
Take, petroleum ether layer is taken after layering, so repeatedly for three times.Combining extraction liquid, plus deionized water is washed till neutrality, and petroleum ether layer rotation is steamed
Hair removal petroleum ether, obtains cupreol extract, plus absolute ethyl alcohol constant volume obtains sample liquid 9.6ml.
(2) detection of cupreol
Precision weighs cupreol standard items (Sigma companies) 0.2mg, adds absolute ethyl alcohol to be settled to 2ml, is made concentration
It is the titer of 0.1mg/ml.Precision draw 0.5,1,1.5,3,3.5,4ul cupreol titer and 2.5ul sample liquids point in
Same High Performance Thin silica gel plate GF254On (10cm × 10cm), 10ml solvents are added, solvent is n-hexane：Ether：Chlorine
It is imitative：Acetic acid：Toluene=4:1:3:0.2:1.5 (V/V/V/V/V), pre-equilibration 20 minutes, expansion cylinder (12cm × 15cm is put into by plate
× 10cm), ascending development is opened up away from 8 ㎝, and taking-up is dried, and is rinsed with 10ml dyeing liquors and dyeed, and prescription of its dyeing liquor is：Phosphomolybdic acid：Second
Acid=5g：100ml, 105 DEG C of drying colour developing 5min, it is seen that standard items and sample two points in same level align and contaminated
Au bleu, thin-layer chromatography scanning is carried out using the type thin-layer chromatogram scanners of Camag 3 under 650nm absorbing wavelengths, and sweep speed is
20mm/s, data resolution is 50um/step, obtains Rf=0.38, irradiation light is tungsten lamp, detection calculating is carried out, with cupreol
The quality (ng) of standard items is abscissa (X), and integrating peak areas value (AU) is ordinate (Y), by thin layer chromatograph management software
WinCATS 1.4.1 directly obtain the regression equation of standard items and integrating peak areas value relation：
Y=6959.4165+53.9858X, r=0.99938, RSD=1.60%.
Result shows that sample liquid is linear good in the range of 50~400ng, the content of cupreol in 2.5ul sample liquids
It is 247ng, the content for being computed cupreol in the useless white bole of 948.48ug containing cupreol in 9.6ml extract solutions, i.e. 50g is
948.48ug。
Embodiment 2：
The extracting method of cupreol is with embodiment 1；Detection method is with the difference of embodiment 1：Solvent is 15ml,
Solvent is n-hexane：Ether：Chloroform：Acetic acid：Toluene=3:0.5:2:0.1:1 (V/V/V/V/V), coloring agent 8ml, according to reality
The equation of linear regression for applying example 1 obtains 9.6ml sample liquids (i.e. 50g give up white bole) 927.06ug of average out to containing cupreol.
Embodiment 3：
The extracting method of cupreol is with embodiment 1；Detection method is with the difference of embodiment 1：Solvent is 12ml,
Solvent is n-hexane：Ether：Chloroform：Acetic acid：Toluene=5:1.5:4:0.3:2 (V/V/V/V/V), coloring agent 12ml, according to
The equation of linear regression of embodiment 1 obtains 9.6ml sample liquids (i.e. 50g give up white bole) 931.21ug of average out to containing cupreol.
Embodiment 4：
The useless white bole 50g produced in corn oil decoloration process, plus 100ml acetone are weighed, is extracted 3 times, stratification, closed
And acetone is evaporated off after extract solution, obtain grease 16.146g.To in grease add 130ml 5% (percentage by volume) concentrated sulfuric acid-
Ethanol solution, 80 DEG C of heating water baths, back flow reaction 6 hours；Solvent is evaporated off, 100ml 80% (percentage by volume) ethanol is added
With 5g NaOH, 80 DEG C are heated to reflux saponification 2h.Deionized water, petroleum ether respectively plus with saponification liquor same volume, concussion extraction
Take, petroleum ether layer is taken after layering, so repeatedly for three times.Combining extraction liquid, plus deionized water is washed till neutrality, and petroleum ether layer rotation is steamed
Hair removal petroleum ether, obtains cupreol extract, plus absolute ethyl alcohol constant volume obtains sample liquid 9.6ml.
Detection method according to embodiment 1 is calculated, and obtains 9.6ml sample liquids (i.e. 50g give up white bole) containing cupreol
Average out to 934.13ug.
Embodiment 5：
The useless white bole 50g produced in corn oil decoloration process, plus 200ml acetone are weighed, is extracted 3 times, stratification, closed
And acetone is evaporated off after extract solution, obtain grease 16.684g.To in grease add 200ml 5% (percentage by volume) concentrated sulfuric acid-
Ethanol solution, 80 DEG C of heating water baths, back flow reaction 6 hours；Solvent is evaporated off, 50ml 80% (percentage by volume) ethanol is added
With 5g NaOH, 80 DEG C are heated to reflux saponification 2h.Deionized water, petroleum ether respectively plus with saponification liquor same volume, concussion extraction
Take, petroleum ether layer is taken after layering, so repeatedly for three times.Combining extraction liquid, plus deionized water is washed till neutrality, and petroleum ether layer rotation is steamed
Hair removal petroleum ether, obtains cupreol extract, plus absolute ethyl alcohol constant volume obtains sample liquid 9.6ml.
Detection method according to embodiment 1 is calculated, and obtains 9.6ml sample liquids (i.e. 50g give up white bole) containing cupreol
Average out to 942.26ug.
Embodiment 6：
The useless white bole 50g produced in soybean oil decoloration process, plus 150ml acetone are weighed, is extracted 3 times, stratification, closed
And acetone is evaporated off after extract solution, obtain grease 16.410g.To in grease add 180ml 5% (percentage by volume) concentrated sulfuric acid-
Ethanol solution, 80 DEG C of heating water baths, back flow reaction 6 hours；Solvent is evaporated off, 80ml 80% (percentage by volume) ethanol is added
With 5g NaOH, 80 DEG C are heated to reflux saponification 2h.Deionized water, petroleum ether respectively plus with saponification liquor same volume, concussion extraction
Take, petroleum ether layer is taken after layering, so repeatedly for three times.Combining extraction liquid, plus deionized water is washed till neutrality, and petroleum ether layer rotation is steamed
Hair removal petroleum ether, obtains cupreol extract, plus absolute ethyl alcohol constant volume obtains sample liquid 9.6ml.
Detection method according to embodiment 1 is calculated, and obtains 9.6ml sample liquids (i.e. 50g give up white bole) containing cupreol
Average out to 952.22ug.
Embodiment 7：
The useless white bole 50g produced in soybean oil decoloration process, plus 100ml acetone are weighed, is extracted 3 times, stratification, closed
And acetone is evaporated off after extract solution, obtain grease 16.231g.To in grease add 130ml 5% (percentage by volume) concentrated sulfuric acid-
Ethanol solution, 80 DEG C of heating water baths, back flow reaction 6 hours；Solvent is evaporated off, 50ml 80% (percentage by volume) ethanol is added
With 5g NaOH, 80 DEG C are heated to reflux saponification 2h.Deionized water, petroleum ether respectively plus with saponification liquor same volume, concussion extraction
Take, petroleum ether layer is taken after layering, so repeatedly for three times.Combining extraction liquid, plus deionized water is washed till neutrality, and petroleum ether layer rotation is steamed
Hair removal petroleum ether, obtains cupreol extract, plus absolute ethyl alcohol constant volume obtains sample liquid 9.6ml.
Detection method according to embodiment 1 is calculated, and obtains 9.6ml sample liquids (i.e. 50g give up white bole) containing cupreol
Average out to 947.34ug.
Claims (8)
1. it is a kind of from useless white bole extract cupreol method, it is characterised in that step is as follows：
(1) by use in grease processing technique after useless white bole extracted using acetone, filter, acetone is evaporated off, obtain oily
Thing；
(2) grease of step (1) is carried out into heating water bath with the concentrated sulfuric acid-ethanol solution, refluxing extraction is evaporated off solvent, then add
Ethanol solution, NaOH, are heated to reflux saponification, and to deionized water, petroleum ether is added in the liquid after saponification, extraction is layered
After take petroleum ether layer, repeat to extract, combining extraction liquid, and be washed with deionized to neutrality, petroleum ether is evaporated off, obtain final product β-paddy steroid
Alcohol extracting thing；
In step (2), the addition of the concentrated sulfuric acid-ethanol solution and the ratio of grease are (8-12) mL:1g；The addition of ethanol solution
Amount is (3-8) mL with the ratio of grease:1g；The addition of NaOH is 5 with the mass ratio of grease：(16-17).
2. the method for extracting cupreol from useless white bole as claimed in claim 1, it is characterised in that in step (1), third
The addition of ketone is 2-4 times of quality volume of useless white bole.
3. the method for extracting cupreol from useless white bole as claimed in claim 1, it is characterised in that in step (1), plus
It is 3 times to enter the number of times that acetone extracted.
4. the method for extracting cupreol from useless white bole as claimed in claim 1, it is characterised in that in step (2), plus
Enter the concentrated sulfuric acid-ethanol solution to carry out the temperature of heating water bath is 80 DEG C, and the time of refluxing extraction is 6 hours；
It is 80 DEG C to be heated to reflux the temperature of saponification, and the time is 2 hours.
5. the method for extracting cupreol from useless white bole as claimed in claim 1, it is characterised in that in step (2), go
The addition of ionized water and petroleum ether is identical with the liquid volume after saponification.
6. the thin-layer chromatography scanning detection method of a kind of cupreol, it is characterised in that step is as follows：
(1) the cupreol extract anhydrous alcohol solution for obtaining the extracting method any one of claim 1-5,
Sample liquid is made, by cupreol standard items anhydrous alcohol solution, titer is made；
(2) the cupreol titer and sample liquid of different quality are put on same thin layer silica gel plate respectively, adds and launch
Agent, pre-equilibration, after silica gel plate is put into expansion cylinder, ascending development dries, dyeing liquor rinse dyeing, drying colour developing；
(3) thin-layer chromatogram scanner carries out thin layer scanning, obtains cupreol RfWith integrating peak areas value；Draw cupreol titer
Quality and integrating peak areas value relation, the integrating peak areas value according to sample liquid calculate the quality of sample liquid cupreol；
In step (2), solvent is n-hexane：Ether：Chloroform：Acetic acid：Toluene, volume ratio is (3~5):(0.5~1.5)：
(2~4)：(0.1~0.3)：(1~2).
7. the thin-layer chromatography scanning detection method of cupreol as claimed in claim 6, it is characterised in that in step (2), no
The cupreol titer of homogenous quantities is 6 kinds of mass gradients, respectively 50ng, 100ng, 150ng, 300ng, 350ng, 400ng.
8. the thin-layer chromatography scanning detection method of cupreol as claimed in claim 6, it is characterised in that in step (2), institute
It is by 1g by phosphomolybdic acid and acetic acid to state dyeing liquor:20mL is mixed.
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| 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 |
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| 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 |
| 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 |
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| 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 |
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| 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 |
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2015
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| 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 |
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