CN101912445B - Method for extracting general flavonoids from toona sinensis leaves under assistance of surfactant - Google Patents
Method for extracting general flavonoids from toona sinensis leaves under assistance of surfactant Download PDFInfo
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- CN101912445B CN101912445B CN2010102635951A CN201010263595A CN101912445B CN 101912445 B CN101912445 B CN 101912445B CN 2010102635951 A CN2010102635951 A CN 2010102635951A CN 201010263595 A CN201010263595 A CN 201010263595A CN 101912445 B CN101912445 B CN 101912445B
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Abstract
The invention relates to a method for extracting active substances from tural products, in particular to a method for extracting general flavonoids from toona sinensis leaves under the assistance of a surfactant, namely coconut oil fatty acid diethanloamides. The method comprises the following steps of: taking the toona sinensis leaves dried at room temperature, crushing the leaves into 30-mesh powder, adding distilling water into the powder according to a mass volume ratio of 1:19-21, and obtaining the material solution, wherein the mass volume unit is g/ml; pre-cooking the material solutionat the temperature of 85 to 95 DEG C for 8 to 12 minutes, adding the surfactant, namely the coconut oil fatty acid diethanloamides, of which the concentration is 0.80 percent, into the material solution, and mixing evenly; and performing microwave extraction on the mixed solution, controlling the microwave power to 180W or 360W or 540W, extracting for 8 to 12 minutes at each time for 4 to 6 times, and obtaining the extract, namely the general flavonoids. The method has the characteristics of high extraction efficiency, small using amount of solvent using amount, high speed and stability, and has the advantages of simple step, convenient operation, no pollution, safety and enormous development potential.
Description
Technical field
The present invention relates to a kind of method of extracting the natural product active substance, the method for total flavones in particularly a kind of surfactant assisted extraction Folium toonae sinensis.
Technical background
Tonnae Sinensis (Toona sinensis) is the tall and big deciduous tree of Meliaceae.Tonnae Sinensis is China's endemic tree, and in Central China, the southwest has wildly, cultivation is economized at most in Shandong, Henan, Hebei etc.Studies show that Tonnae Sinensis has numerous pharmacological effects such as antitumor, antioxidation, blood sugar lowering, enhancing people motility of sperm.Wherein, flavonoid substance is a main active.The traditional extracting method of total flavones has decocting cooking method, alcohol reflux, Soxhlet to extract, ooze deer method etc. in the Folium toonae sinensis, and all there is long, problem such as extraction efficiency is low of extraction time in these methods.These years, there is new method to occur again, as ultrasonic extraction, Enzymatic Extraction etc.Supersonic extracting method have save time, energy-saving and environmental protection, extraction efficiency advantages of higher, extraction effect is subject to the influence of factors such as instrument, as extract medium, placement location, the thin and thick of extraction flask wall, by ultrasonic thing granularity etc.Enzyme process mild condition, extract yield are higher, but the time is longer, and extraction efficiency is not high.
The chemical name of the used surfactant of the present invention is a cocoanut fatty acid diethanolamide, by name 6501, the ninol of commodity, and model has 1: 1 type, 1: 1.5 type, 1: 2 type.
Summary of the invention
The method that the purpose of this invention is to provide total flavones in a kind of surfactant assisted extraction Folium toonae sinensis, it by with the aqueous solution that is dissolved with the low quantity of surfactant cocoanut fatty acid diethanolamide as extracting solution, utilize the solubilization of surfactant cocoanut fatty acid diethanolamide, promote extracts active ingredients in conjunction with microwave heating, the present invention has the extraction efficiency height, solvent load is few, quick and stable characteristics; Step of the present invention is simple, and is easy to operate, pollution-free, and nonhazardous has very big development potentiality.
Technical scheme of the present invention is achieved in that the method for total flavones in a kind of surfactant assisted extraction Folium toonae sinensis, and it is characterized in that: it comprises the steps:
1), the air dried Folium toonae sinensis of the room temperature of learning from else's experience, be crushed to 30 orders, Folium toonae sinensis is 1 by mass volume ratio after crushed: 19-21 adds distilled water and obtains feed liquid, and the unit of mass volume ratio is g/ml;
2), be to precook under 85 ℃-95 ℃ behind the 8-12min the feed liquid of step 1) in temperature, add concentration and be 0.80% surfactant cocoanut fatty acid diethanolamide aqueous solution, mixing obtains mixed solution,
3), with step 2) mixed solution carry out microwave extraction, controlled microwave power is 180 W or 360W or 540W, extracts 4-6 time, each 8-12min obtains extractive total flavone.
The best approach of total flavones in a kind of surfactant assisted extraction Folium toonae sinensis, it is characterized in that: it comprises the steps:
1), the air dried Folium toonae sinensis of the room temperature of learning from else's experience, be crushed to 30 orders, Folium toonae sinensis is to add distilled water at 1: 20 to obtain feed liquid by mass volume ratio after crushed;
2), be to precook under 90 ℃ behind the 10min the feed liquid of step 1) in temperature, add concentration and be 0.80% surfactant cocoanut fatty acid diethanolamide aqueous solution, mixing obtains mixed solution;
3), with step 2) mixed solution carry out microwave extraction, controlled microwave power is 180W, extracts 5 times, each 10min obtains extractive total flavone.
Described surfactant cocoanut fatty acid diethanolamide is 1: 1.5 type.
Its principle is that the surfactant cocoanut fatty acid diethanolamide has specific parents' molecular structure, can reduce the interfacial tension between Folium toonae sinensis cell membrane and aqueous solution, can strengthen wettability and the permeability of solvent to material, and flavone in the Folium toonae sinensis is had solubilization, leach usefulness and extraction ratio thereby can increase.In addition, the microwave radiation process is that frequency electromagnetic waves penetrates spe medium, arrives the vascular bundle and the glandular cell system of material inside.Because absorb microwave energy, the cell interior temperature rises rapidly, make its cell interior pressure surpass the expansion ability to bear of cell wall, cause cell rupture, effective ingredient freely flows out in the born of the same parents.
Main feature of the present invention is: the surfactant auxiliary extraction technology that the present invention adopts extracts the method for Tonnae Sinensis total flavones and compares with existing extractive technique from Folium toonae sinensis, has the following advantages and distinguished effect:
1. the collaborative microwave method of surfactant cocoanut fatty acid diethanolamide is extracted and has greatly been improved Tonnae Sinensis total flavones extraction effect, and save time, efficient, energy-conservation, extraction ratio is higher than simple microwave method extraction ratio 53.60%;
With the distilled water solution that is dissolved with the low quantity of surfactant cocoanut fatty acid diethanolamide as extracting solution, pollution-free, nonhazardous can be widely used in industries such as food, cosmetics and health product, has market prospect preferably, is worthy of popularization;
3. operation is simple, and equipment maintenance is convenient.The large-scale industrial production process is less to surfactant cocoanut fatty acid diethanolamide-microwave-assisted extraction process reforming equipment investment from traditional extraction technique.
The specific embodiment
The method of total flavones in a kind of surfactant assisted extraction Folium toonae sinensis of the present invention, it comprises the steps:
1), the air dried Folium toonae sinensis of the room temperature of learning from else's experience, be crushed to 30 orders, Folium toonae sinensis is 1 by mass volume ratio after crushed: 19-21 adds distilled water and obtains feed liquid, and the unit of mass volume ratio is g/ml;
2), be to precook under 85 ℃-95 ℃ behind the 8-12min the feed liquid of step 1) in temperature, add concentration and be 0.80% surfactant cocoanut fatty acid diethanolamide aqueous solution, mixing obtains mixed solution;
3), with step 2) mixed solution carry out microwave extraction, controlled microwave power is 180 W or 360W or 540W, extracts 4-6 time, each 8-12min obtains extractive total flavone.
Below in conjunction with specific embodiment the present invention is described in further detail, but not as a limitation of the invention.
Embodiment 1
The best approach of total flavones in a kind of surfactant assisted extraction Folium toonae sinensis, it comprises the steps:
1), the air dried Folium toonae sinensis of the room temperature of learning from else's experience 3 grams, be crushed to 30 orders, Folium toonae sinensis is to add distilled water 60 mls at 1: 20 to obtain feed liquid by mass volume ratio after crushed;
2) be to precook under 90 ℃ behind the 10min in temperature, with the feed liquid of step 1), adding concentration is 0.80% surfactant cocoanut fatty acid diethanolamide aqueous solution 90ml, mixing obtains mixed solution, and described surfactant cocoanut fatty acid diethanolamide is 1: 1.5 type;
3), with step 2) mixed solution carry out microwave extraction, controlled microwave power is 180W, extracts 5 times, each 10min obtains extractive total flavone.
With the rutin is standard control, adopts the aluminum chloride colorimetry, measures general flavone content.The total flavones extraction ratio can reach 98.70% in the Folium toonae sinensis.
Embodiment 2
The method of total flavones in a kind of surfactant assisted extraction Folium toonae sinensis, it comprises the steps:
1), the air dried Folium toonae sinensis of the room temperature of learning from else's experience 2 grams, be crushed to 30 orders, Folium toonae sinensis is that 1:19 adds distilled water 38 ml and obtains feed liquid by mass volume ratio after crushed;
2) be to precook under 85 ℃ behind the 8min in temperature, with the feed liquid of step 1), adding concentration is 0.80% surfactant cocoanut fatty acid diethanolamide aqueous solution 60 ml, mixing obtains mixed solution, and described surfactant cocoanut fatty acid diethanolamide is the 1:1.5 type;
3), with step 2) mixed solution carry out microwave extraction, controlled microwave power is 360W, extracts 4 times, each 8min obtains extractive total flavone.
With the rutin is standard control, adopts the aluminum chloride colorimetry, measures general flavone content.The total flavones extraction ratio can reach 95% in the Folium toonae sinensis.
Embodiment 3
The method of total flavones in a kind of surfactant assisted extraction Folium toonae sinensis, it comprises the steps:
1), the air dried Folium toonae sinensis of the room temperature of learning from else's experience 5 grams, be crushed to 30 orders, Folium toonae sinensis is that 1:21 adds distilled water 105 ml and obtains feed liquid by mass volume ratio after crushed;
2) be to precook under 95 ℃ behind the 12min in temperature, with the feed liquid of step 1), adding concentration is 0.80% surfactant cocoanut fatty acid diethanolamide aqueous solution 150 ml, mixing obtains mixed solution, and described surfactant cocoanut fatty acid diethanolamide is the 1:1.5 type;
3), with step 2) mixed solution carry out microwave extraction, controlled microwave power is 540W, extracts 6 times, each 12min obtains extractive total flavone.
With the rutin is standard control, adopts the aluminum chloride colorimetry, measures general flavone content.The total flavones extraction ratio can reach 96.60% in the Folium toonae sinensis.
Concentration is that 0.80% surfactant cocoanut fatty acid diethanolamide aqueous solution is meant that the water of 1 ml contains the surfactant cocoanut fatty acid diethanolamide of 0.008 g in the foregoing description.The surfactant cocoanut fatty acid diethanolamide is not limited only to 1: 1.5 type among the embodiment, and it can also be 1: 1 type, 1: 2 type.
Contrast test:
Table 1 distinct methods extracts the comparison of test results of Tonnae Sinensis total flavones
Extracting method | Extraction conditions | Extraction ratio (%) |
1. microwave water is carried | Water, microwave power 180w, extraction 5 times, each 10min | 45.10 |
2. microwave, surfactant and water | Water, cocoanut fatty acid diethanolamide, microwave power 180w, extraction 5 times, each 10min | 86.90 |
3. precook, microwave, surfactant and water | Water, 90 ℃ of 10min that precook, cocoanut fatty acid diethanolamide, microwave power 180w, extract 5 times, each 10min | 98.70 |
Specifying of table 1:
Extracting method 1: take by weighing through the air dried 2 gram Folium toonae sinensiss of room temperature, be crushed to 30 orders, Folium toonae sinensis after crushed, 40 milliliters of adding distil waters carry out microwave extraction, controlled microwave power is 180W, extracts 5 times, at every turn 10min;
Extracting method 2: take by weighing through the air dried 2 gram Folium toonae sinensiss of room temperature, be crushed to 30 orders, Folium toonae sinensis after crushed, 40 milliliters of adding distil waters add 60 ml concns and are 0.8% surfactant cocoanut fatty acid diethanolamide again, carry out microwave extraction, microwave power 180w extracts 5 times, each 10min.Described surfactant cocoanut fatty acid diethanolamide is the 1:1.5 type;
Extracting method 3: through the air dried 2 gram Folium toonae sinensiss of room temperature, be crushed to 30 orders, Folium toonae sinensis after crushed, 40 milliliters of adding distil waters, the 10min that precooks under 90 ℃ of temperature adds 60 ml concns and is 0.8% surfactant cocoanut fatty acid diethanolamide again, carry out microwave extraction, microwave power 180w extracts 5 times, each 10min.Described surfactant cocoanut fatty acid diethanolamide is the 1:1.5 type.
With the rutin is standard control, adopts the aluminum chloride colorimetry, measures general flavone content.
The comparison of test results of extracting the Tonnae Sinensis total flavones from the distinct methods of table 1 shows, adopts extracting method of the present invention (extracting method 3) Tonnae Sinensis total flavones extraction ratio the highest.
The present invention adopts and precooks, the mode of microwave extraction, with the aqueous solution that is dissolved with the low quantity of surfactant cocoanut fatty acid diethanolamide as extracting solution, adopt the Orthogonal Experiment and Design scheme, technical parameters such as kind by pretreated mode, microwave power, extraction solvent, action time, extraction time, surfactant in the screening surfactant leaching process and concentration, obtains quick, accurate, efficient, economical from Folium toonae sinensis the method for extraction Tonnae Sinensis total flavones.
Claims (1)
1. the method for total flavones in the surfactant assisted extraction Folium toonae sinensis, it is characterized in that: it comprises the steps:
1), the air dried Folium toonae sinensis of the room temperature of learning from else's experience 3 grams, be crushed to 30 orders, Folium toonae sinensis is to add distilled water 60 mls at 1: 20 to obtain feed liquid by mass volume ratio after crushed;
2) be to precook under 90 ℃ behind the 10min in temperature, with the feed liquid of step 1), adding concentration is 0.80% surfactant cocoanut fatty acid diethanolamide aqueous solution 90ml, mixing obtains mixed solution, and described surfactant cocoanut fatty acid diethanolamide is 1: 1.5 type;
3), with step 2) mixed solution carry out microwave extraction, controlled microwave power is 180W, extracts 5 times, each 10min obtains extractive total flavone;
Or: 1), the air dried Folium toonae sinensis of the room temperature of learning from else's experience 2 grams, be crushed to 30 orders, Folium toonae sinensis is that 1:19 adds distilled water 38 ml and obtains feed liquid by mass volume ratio after crushed;
2) be to precook under 85 ℃ behind the 8min in temperature, with the feed liquid of step 1), adding concentration is 0.80% surfactant cocoanut fatty acid diethanolamide aqueous solution 60 ml, mixing obtains mixed solution, and described surfactant cocoanut fatty acid diethanolamide is the 1:1.5 type;
3), with step 2) mixed solution carry out microwave extraction, controlled microwave power is 360W, extracts 4 times, each 8min obtains extractive total flavone;
Or: 1), the air dried Folium toonae sinensis of the room temperature of learning from else's experience 5 grams, be crushed to 30 orders, Folium toonae sinensis is that 1:21 adds distilled water 105 ml and obtains feed liquid by mass volume ratio after crushed;
2) be to precook under 95 ℃ behind the 12min in temperature, with the feed liquid of step 1), adding concentration is 0.80% surfactant cocoanut fatty acid diethanolamide aqueous solution 150 ml, mixing obtains mixed solution, and described surfactant cocoanut fatty acid diethanolamide is the 1:1.5 type;
3), with step 2) mixed solution carry out microwave extraction, controlled microwave power is 540W, extracts 6 times, each 12min obtains extractive total flavone.
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CN102178739B (en) * | 2011-04-14 | 2013-04-10 | 华东理工大学 | Method for extracting flavone by using surfactant from herb to coordinate with enzymolysis-microwave |
CN103169789A (en) * | 2012-12-18 | 2013-06-26 | 甘肃农业大学 | Method for extracting total flavonoid in silverweed cinquefoil root |
CN105231249A (en) * | 2015-09-17 | 2016-01-13 | 暨南大学 | Bamboo leaf flavone extracting method by synergy of ultrasonic and surface-active agent |
CN105878118A (en) * | 2016-05-21 | 2016-08-24 | 广州丹奇日用化工厂有限公司 | Method for extracting cedrela sinensis extract from cedrela sinensis leaves and application of method |
CN106377453B (en) * | 2016-08-31 | 2020-12-25 | 海南师范大学 | Morinda citrifolia extract emulsion and preparation method and application thereof |
CN112250720A (en) * | 2020-10-26 | 2021-01-22 | 长沙中战茶油集团有限公司 | Method for extracting flavone |
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CN101396432A (en) * | 2008-10-13 | 2009-04-01 | 广西大学 | Method for concentrating and separating flavonoids from toona sinensis leaves |
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