CN103655802B - The extracting method of anti-oxidation active substance in a kind of rose leaf - Google Patents
The extracting method of anti-oxidation active substance in a kind of rose leaf Download PDFInfo
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Abstract
The extracting method of anti-oxidation active substance in a kind of rose leaf of disclosure. The method comprises the steps: that (1) fresh rose leaf obtains rose leaf granule through pulverizing and sieving after drying; (2) extract described rose leaf granule with Extraction solvent, obtain extracting solution; (3) the centrifuged supernatant of described extracting solution; Described supernatant is concentrated obtains concentrated solution; (4) described concentrated solution is extracted with ether, ethyl acetate and water saturated butanol solution successively, respectively obtain ether extraction liquid, acetic acid ethyl acetate extract, butanol extraction liquid and water extract, concentrated respectively again obtain ethereal extract, acetic acid ethyl ester extract, n-butyl alcohol extract and water extract, it is respectively labeled as Fa, Fb, Fc and Fd, namely extracts the antioxidant obtaining in rose leaf. Anti-oxidation active substance screening technique provided by the invention employing free-atom aqueous solution separates afterproduct with liquid-phase chromatographic column and reacts online, and separation screening continuously performs, and can quickly detect have oxidation-resistant active ingredient.
Description
Technical field
The present invention relates to the extracting method of anti-oxidation active substance in a kind of rose leaf.
Background technology
Human homergy or can produce free radical under various stressed conditions, excessive free radical can cause a series of diseases such as cancer, aging, diabetes, is at this moment accomplished by supplemented with exogenous antioxidant to maintain interior free yl balance. Suppressing the generation of free radical so that it is quickly quencher, repair its oxidative damage that human body is caused health is significant, the mensuration of searching natural anti-oxidation active component and antioxidant activity has become current focus.
Rose leaf is the leaf of Rosaceae Rosa machaka Flos Rosae Rugosae, and rose leaf contains substantial amounts of flavone compound. This compounds can not only remove the free radical of chain initiating stage in Antioxidation reaction, and can free radical in Direct Acquisition radical reaction chain, block free chain reaction, play the dual function of prevention and chain rupture. At present, the existing extractive technique extracting flavone compound from plant, but the report for extracting flavone compound from rose leaf is few both at home and abroad, only find that Jia Changhong etc. adopts microwave extraction rose leaf flavone, but instrument and equipment is required height by the method, operating cost is high, and range of application is narrower, can not promote on a large scale, therefore occur but without standardized product in the market.
In the mensuration of antioxidant activity, can adopt extract that ABTS free radical and DPPH radical scavenging activity are quickly measured its antioxidant activity at present, but, what these methods measured is the gross activity of extract, but not one-component, and the method adopts colorimetry to be measured, it is easy to be subject to the interference of substrate.
Summary of the invention
It is an object of the invention to provide the extracting method of anti-oxidation active substance in a kind of rose leaf.
In a kind of rose leaf provided by the present invention, the extracting method of anti-oxidation active substance, comprises the steps:
(1) fresh rose leaf obtains rose leaf granule through pulverizing and sieving after drying;
(2) extract described rose leaf granule with Extraction solvent, obtain extracting solution; Described Extraction solvent is water or ethanol water;
(3) the centrifuged supernatant of described extracting solution; Described supernatant is concentrated obtains concentrated solution;
(4) described concentrated solution is extracted with ether, ethyl acetate and water saturated butanol solution successively, respectively obtain ether extraction liquid, acetic acid ethyl acetate extract, butanol extraction liquid and water extract, concentrated respectively again obtain ethereal extract, acetic acid ethyl ester extract, n-butyl alcohol extract and water extract, it is respectively labeled as Fa, Fb, Fc and Fd, namely extracts the antioxidant obtaining in rose leaf.
Described method also includes the step that the antioxidant in described Fa, Fb, Fc and Fd is extracted:
Described Fa, Fb, Fc and Fd are carried out respectively liquid chromatograph separation, is detecting the liquid chromatogram I being extracted thing when wavelength is 270nm and 350nm successively; Each component after separated and free-atom aqueous solution react, and detect subsequently into detector, obtain each extract and the reacted chemical composition collection of illustrative plates II of described free-atom aqueous solution detecting when wavelength is 270nm, 350nm and 747nm; Contrast the absworption peak under 270nm, 350nm and 747nm condition in described chemical composition collection of illustrative plates II, under identical retention time, if the absworption peak under 270nm and 350nm condition is negative absorption peak when 747nm, the component that then this retention time is corresponding is anti-oxidation active substance, and the component collected under this retention time is anti-oxidation active substance.
In above-mentioned method, in step (1), through described in dry after the moisture content of rose leaf can be 4%��8%;
The granularity of described rose leaf granule can be 20��80 orders.
In above-mentioned method, in step (2), in described ethanol water, the volume content of ethanol can be 10%��90%;
The temperature of described extraction can be 40��80 DEG C, and the time of described extraction can be 60��80min;
The mass ratio of described Extraction solvent and described rose leaf granule can be 5��30:1;
The number of times of described extraction can be 1��3 time.
In above-mentioned method, in step (3), described centrifugal rotating speed can be 3000��4800r/min, and the described centrifugal time can be 5��30min;
The temperature of described concentration can be 40��80 DEG C;
The concentration of described concentrated solution can be 5��8 �� of Brix.
In above-mentioned method, in step (4), the volume ratio of described concentrated solution and described ether can be 1:2��3;
The volume ratio of ether raffinate and described ethyl acetate can be 1:2��3;
The volume ratio of ethyl acetate raffinate and described water-saturated n-butanol can be 1:2��3;
The number of times of described extraction can be 1��2 time;
The temperature of described concentration can be 40��70 DEG C.
In above-mentioned method, described free-atom aqueous solution can be the aqueous solution of 2,2-azino-two (3-ethyl-benzothiazole-6-sulfonic acid) di-ammonium salts (ABTS);
The described free-atom aqueous solution absorbance at 747nm place can be 0.65��0.75;
Negative peak in described liquid chromatogram II is that described free-atom aqueous solution reacts generation with the oxidation-resistant active ingredient in extract and fades, and absorbance reduces and causes.
In above-mentioned method, the temperature of described reaction can be 25��35 DEG C.
In above-mentioned method, the condition that described liquid chromatograph separates is as follows: chromatographic column is AgilentZorbaxAQ post; Mobile phase A is water (formic acid containing mass concentration 2%) mutually, and Mobile phase B is acetonitrile mutually; Gradient elution program: 0��15min, 0%��10%B; 15��20min, 10%B; 20��30min, 10%��15%B; 30��40min, 15%B; 40��50min, 15%��20%B; 50��60min, 20%B; 60��65min, 20%��30%B.
In above-mentioned method, LC-MS can be passed through and detect the described anti-oxidation active substance filtered out. Then can pass through the standard substance antioxidant content to identifying and carry out quantitatively, the standard curve of the Scavenging ability that reference standard polyphenoils is set up, the Scavenging ability of different antioxidant contents is carried out Quantitative Comparison.
There is advantages that
1, in method provided by the invention, rose leaf wide material sources, production technology is simple, and technological parameter is reasonable, and equipment investment cost is low, has higher economic results in society and wide industrial prospect.
2, anti-oxidation active substance screening technique provided by the invention, it is possible to resolve common method can only measure the oxidation resistance of total extract, it is impossible to measure the deficiency of the oxidation resistance of monomer.
3, anti-oxidation active substance screening technique provided by the invention adopts free-atom aqueous solution to separate afterproduct with liquid-phase chromatographic column and react online, and separation screening continuously performs, and can quickly detect have oxidation-resistant active ingredient.
Accompanying drawing explanation
Fig. 1 is the process chart of the method for the present invention.
Fig. 2 is the flow chart of the method screening antioxidant content (step (6)) in the inventive method online.
Fig. 3 is the comparison diagram of the liquid chromatograph of ether extraction liquid in embodiment 1.
Fig. 4 is the comparison diagram of liquid chromatograph in acetic acid ethyl acetate extract in embodiment 1.
Fig. 5 is the comparison diagram of liquid chromatograph in butanol extraction liquid in embodiment 1.
Fig. 6 is the comparison diagram of liquid chromatograph in water extract in embodiment 1.
Detailed description of the invention
The experimental technique used in following embodiment if no special instructions, is conventional method.
Material used in following embodiment, reagent etc., if no special instructions, all commercially obtain.
ABTS free-atom aqueous solution is prepared: take the ABTS(Sigma company of 7mmol/L, Shanghai) aqueous solution mixes with the potassium persulfate solution of 2.45mmol/L, lucifuge reaction more than 12h, testing front methanol, ABTS storing solution is diluted to 747nm place absorbance is 0.65��0.75.
Embodiment 1,
After fresh rose leaf is dried (its water content is 5%), pulverized 20 mesh sieves and obtained rose leaf granule. After weighing 50g rose leaf granule addition triangular flask, add 500g deionized water, extract 3 times at 70 DEG C, extract 60min every time, merge the extracting solution obtained. Extracting solution after merging is obtained 1.5 �� of Brix supernatant after the centrifugal 15min of 4500r/min, 60 DEG C of concentrating under reduced pressure, obtain 6 �� of Brix concentrated solutions. This concentrated solution is sequentially added into ether, ethyl acetate and water-saturated n-butanol solution with 1:2 volume ratio, all extracts and obtain ether extraction liquid, acetic acid ethyl acetate extract, butanol extraction liquid and water extract successively 2 times. Above-mentioned each extract is evaporated to dry respectively at 50 DEG C, obtain ethereal extract (Fa) 2.36g, acetic acid ethyl ester extract (Fb) 3.85g, n-butyl alcohol extract (Fc) 3.94g, and water extract (Fd) 2.97g, dissolve respectively with methanol solution and be settled to 200mL, cross 0.45 ��m of film respectively, separating through high performance liquid chromatography, separation condition is: AgilentZorbaxAQ post (250mm �� 4.6mmi.d., 5 ��m);Mobile phase A is water (containing concentration 2% formic acid) mutually, and Mobile phase B is acetonitrile mutually; Gradient elution program: 0��15min, 0%��10%B; 15��20min, 10%B; 20��30min, 10%��15%B; 30��40min, 15%B; 40��50min, 15%��20%B; 50��60min, 20%B; 60��65min, 20%��30%B. Sample size 10 �� L; Flow velocity is 0.8ml/min; Column temperature 25 DEG C; Detection wavelength 270nm and 356nm. Device detection, obtains the liquid chromatogram of four kinds of extracts after testing, is denoted as composition collection of illustrative plates, and collects each component that separation obtains.
With 0.5mL/min flow velocity, the ABTS free-atom aqueous solution prepared is pumped into past column reaction system, and thermostat temperature is 30 DEG C, and ABTS solution enters detector after flowing through response system, and after 747nm place absorbance balances, baseline returns to zero. By above-mentioned condition by four kinds of extract solutions sample introduction respectively, liquid chromatograph separates each component obtained and enters detector after past column reaction system response with ABTS free-atom aqueous solution, retention time under record 270nm, 356nm and 747nm, respectively obtains corresponding collection of illustrative plates, is denoted as collection of illustrative plates after reaction; Absworption peak under 270nm, 350nm and 747nm condition in collection of illustrative plates after contrast reaction, under identical retention time, if the absworption peak under 270nm and 350nm condition is negative absorption peak when 747nm, the component that then this retention time is corresponding is anti-oxidation active substance, collects the component under this retention time and namely obtains anti-oxidation active substance.
Wherein, the comparison diagram of ethereal extract (Fa) is as shown in Figure 3, the comparison diagram of acetic acid ethyl ester extract (Fb) is as shown in Figure 4, the comparison diagram of n-butyl alcohol extract (Fc) is as shown in Figure 5, the comparison diagram of water extract (Fd) as shown in Figure 6, filters out the component with negative peak and is anti-oxidation active substance.
LC-MS technology is adopted to carry out qualitative analysis the anti-oxidation active substance filtered out in each extract.
Standard diagram in conjunction with each antioxidant, it is possible to learn, detects 10 kinds of antioxidant such as Quercetin, Quercetin 3-��-D-Glucose glycoside, apigenin-8-C-glucoside altogether in ethereal extract; Acetic acid ethyl ester extract detects 14 kinds of antioxidant such as catechin, rutin; N-butyl alcohol extract detects 15 kinds of antioxidant such as chlorogenic acid; Water extract detects 11 kinds of antioxidant such as middle quininic acid.
Embodiment 2,
After fresh rose leaf is dried (its water content is 6%), pulverized 20 mesh sieves and obtained rose leaf granule. After weighing 50g rose leaf granule addition triangular flask, add the ethanol water of 1000g ethanol volumn concentration 50%, extract 2 times at 70 DEG C, extract 60min every time, merge the extracting solution obtaining 1.2 �� of Brix. This extracting solution is obtained supernatant after the centrifugal 15min of 4500r/min, concentrating under reduced pressure at 55 DEG C, obtain the concentrated solution of 6 �� of Brix. This concentrated solution is sequentially added into ether, ethyl acetate and water-saturated n-butanol solution with 1:3 volume ratio, extracts and obtain ether extraction liquid, acetic acid ethyl acetate extract, butanol extraction liquid and water extract successively 1 time. Each extract is evaporated to respectively at 45 DEG C dry, obtain ethereal extract (Fa) 2.12g, acetic acid ethyl ester extract (Fb) 3.89g, n-butyl alcohol extract (Fc) 3.57g, and water extract (Fd) 2.84g, dissolve respectively with methanol solution and be settled to 200mL, cross 0.45 ��m of film respectively, separating through high performance liquid chromatography, separation condition is: AgilentZorbaxAQ post (250mm �� 4.6mmi.d., 5 ��m);Mobile phase A is water (containing concentration 2% formic acid) mutually, and Mobile phase B is acetonitrile mutually; Gradient elution program: 0��15min, 0%��10%B; 15��20min, 10%B; 20��30min, 10%��15%B; 30��40min, 15%B; 40��50min, 15%��20%B; 50��60min, 20%B; 60��65min, 20%��30%B. Sample size 10 �� L; Flow velocity is 0.8ml/min; Column temperature 25 DEG C; Detection wavelength 270nm, 356nm. Device detection, obtains the liquid chromatogram of four kinds of extracts after testing, is denoted as composition collection of illustrative plates, and collects each component that separation obtains.
With 0.7mL/min flow velocity, the ABTS free-atom aqueous solution prepared is pumped into past column reaction system, and thermostat temperature is 35 DEG C, and ABTS solution enters detector after flowing through response system, and after 747nm place absorbance balances, baseline returns to zero. By above-mentioned condition by four kinds of extract solutions sample introduction respectively, liquid chromatograph separates each component obtained and enters detector after past column reaction system response with ABTS free-atom aqueous solution, retention time under record 270nm, 356nm and 747nm, respectively obtains corresponding collection of illustrative plates, is denoted as collection of illustrative plates after reaction; Absworption peak under 270nm, 350nm and 747nm condition in collection of illustrative plates after contrast reaction, under identical retention time, if the absworption peak under 270nm and 350nm condition is negative absorption peak when 747nm, the component that then this retention time is corresponding is anti-oxidation active substance, collects the component under this retention time and namely obtains anti-oxidation active substance.
LC-MS technology is adopted to carry out qualitative analysis the anti-oxidation active substance filtered out in each extract.
Standard diagram in conjunction with each antioxidant, it is possible to learn, detects 10 kinds of antioxidant such as Quercetin, Quercetin 3-��-D-Glucose glycoside, apigenin-8-C-glucoside altogether in ethereal extract; Acetic acid ethyl ester extract detects 14 kinds of antioxidant such as catechin, rutin; N-butyl alcohol extract detects 15 kinds of antioxidant such as chlorogenic acid; Water extract detects 11 kinds of antioxidant such as middle quininic acid.
Claims (8)
1. an extracting method for anti-oxidation active substance in rose leaf, comprises the steps:
(1) fresh rose leaf obtains rose leaf granule through pulverizing and sieving after drying;
(2) extract described rose leaf granule with Extraction solvent, obtain extracting solution; Described Extraction solvent is water or ethanol water;
The temperature of described extraction is 40��80 DEG C, and the time of described extraction is 60��80min;
The mass ratio of described Extraction solvent and described rose leaf granule is 5��30:1;
(3) the centrifuged supernatant of described extracting solution; Described supernatant is concentrated obtains concentrated solution;
(4) described concentrated solution is extracted with ether, ethyl acetate and water saturated butanol solution successively, respectively obtain ether extraction liquid, acetic acid ethyl acetate extract, butanol extraction liquid and water extract, concentrated respectively again obtain ethereal extract, acetic acid ethyl ester extract, n-butyl alcohol extract and water extract, be respectively labeled as Fa, Fb, Fc and Fd;
Described method also includes the step that the antioxidant in described Fa, Fb, Fc and Fd is extracted:
Described Fa, Fb, Fc and Fd are carried out respectively liquid chromatograph separation, is detecting the liquid chromatogram I being extracted thing when wavelength is 270nm and 350nm successively; Each component after separated and free-atom aqueous solution react, and detect subsequently into detector, obtain each extract and the reacted chemical composition collection of illustrative plates II of described free-atom aqueous solution detecting when wavelength is 270nm, 350nm and 747nm;Contrast the absworption peak under 270nm, 350nm and 747nm condition in described chemical composition collection of illustrative plates II, under identical retention time, if the absworption peak under 270nm and 350nm condition is negative absorption peak when 747nm, the component that then this retention time is corresponding is anti-oxidation active substance, and the component collected under this retention time is anti-oxidation active substance.
2. method according to claim 1, it is characterised in that: in step (1), through described in dry after the moisture content of rose leaf be 4%��8%;
The granularity of described rose leaf granule is 20��80 orders.
3. method according to claim 1 and 2, it is characterised in that: in step (2), in described ethanol water, the volume content of ethanol is 10%��90%;
The number of times of described extraction is 1��3 time.
4. method according to claim 1 and 2, it is characterised in that: in step (3), described centrifugal rotating speed is 3000��4800r/min, and the described centrifugal time is 5��30min;
The temperature of described concentration is 40��80 DEG C;
The concentration of described concentrated solution is 5��8 �� of Brix.
5. method according to claim 1 and 2, it is characterised in that: in step (4), the volume ratio of described concentrated solution and described ether is 1:2��3;
The volume ratio of ether raffinate and described ethyl acetate is 1:2��3;
The volume ratio of ethyl acetate raffinate and described water-saturated n-butanol is 1:2��3;
The number of times of described extraction is 1��2 time;
The temperature of described concentration is 40��70 DEG C.
6. method according to claim 1, it is characterised in that: described free-atom aqueous solution is the aqueous solution of 2,2-azino-two (3-ethyl-benzothiazole-6-sulfonic acid) di-ammonium salts;
The described free-atom aqueous solution absorbance at 747nm place is 0.65��0.75.
7. method according to claim 1, it is characterised in that: the temperature of described reaction is 25��35 DEG C.
8. method according to claim 1 and 2, it is characterised in that: the described anti-oxidation active substance gone out by LC-MS evaluation and screening.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2240131C1 (en) * | 2003-04-04 | 2004-11-20 | Аладьев Сергей Иванович | Agent "artrovit" for prophylaxis and treatment of arthritis and arthrosis |
| CN102507772A (en) * | 2011-10-26 | 2012-06-20 | 西北农林科技大学 | Method for detecting antioxidative activity compound in mixture |
| CN102614276A (en) * | 2012-04-22 | 2012-08-01 | 吉林化工学院 | Dahurian rose fruit leaf general flavone extract, and extracting method and medical application thereof |
| CN103417679A (en) * | 2013-09-11 | 2013-12-04 | 河南中医学院 | Method for extracting anti-cerebral-ischemia material from roses and application of anti-cerebral ischemia material |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2240131C1 (en) * | 2003-04-04 | 2004-11-20 | Аладьев Сергей Иванович | Agent "artrovit" for prophylaxis and treatment of arthritis and arthrosis |
| CN102507772A (en) * | 2011-10-26 | 2012-06-20 | 西北农林科技大学 | Method for detecting antioxidative activity compound in mixture |
| CN102614276A (en) * | 2012-04-22 | 2012-08-01 | 吉林化工学院 | Dahurian rose fruit leaf general flavone extract, and extracting method and medical application thereof |
| CN103417679A (en) * | 2013-09-11 | 2013-12-04 | 河南中医学院 | Method for extracting anti-cerebral-ischemia material from roses and application of anti-cerebral ischemia material |
Non-Patent Citations (2)
| Title |
|---|
| 丁香叶、月季叶和玫瑰叶黄酮对自由基和亚硝酸盐的清除作用比较研究;贾长虹等;《食品科技》;20111231;第36卷(第2期);第212-215页，尤其是第212页第3段 * |
| 花卉抗氧化筛选与玫瑰花抗氧化活性研究;第3期;《中国优秀博硕士学位论文全文数据库（硕士）基础科学辑》;20040915(第3期);第42页4.2.7节，第34页4.1.2.7 * |
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