CN103705554A - Method for extracting total flavone from acer serrulatum leaves based on ultrasonic assistance - Google Patents

Abstract

The invention discloses a method for extracting total flavone from acer serrulatum leaves based on ultrasonic assistance. The method comprises the following steps: baking and crushing acer serrulatum leaves to serve as extracting raw materials; extracting the extracting raw materials in an ultrasonic extraction kettle with ethanol serving as a solvent, performing extraction once in every 2 minutes, 3 minutes each time, in an air-lift agitating condition and an independent ultrasonic generation mode to obtain an extract after 30 minutes of ultrasonic extract; concentrating and drying the aqueous phase to obtain the total flavone extract from the acer serrulatum leaves. According to the extraction method, few impurities are prepared, the extraction rate can be over 97 percent, the extraction time is short and shortened by over 10 times than that of a traditional extraction method, the operation is simple and practical, effective components in medicinal materials can be protected, physiological activity of thermosensitive medicines cannot be destroyed, and energy consumption can be greatly reduced.

Description

A kind of method based on total flavones in the blue or green Folium Alangii of ultrasound wave assisted extraction

Technical field

The present invention relates to the extractive technique of flavone, be specifically related to a kind of method based on total flavones in the blue or green Folium Alangii of ultrasound wave assisted extraction.

Background technology

Blue or green maple belongs to Aceraceae, Acer plant, produces China, Japan and Korea; Distribution in China is in each province, the Yangtze river basin, and Shandong, Henan, Zhejiang also have.Be born in the border or sparse woods on the following mountain region of height above sea level 1200m, hills more.Flavone compound (Flavonoids) is the low molecule Plant Secondary Metabolites of a class, is distributed widely in vegetable, fruit and medicinal plants.This compounds has common parent nucleus C ₆-C ₃-C ₆structure, from vegetable material, separation has obtained hundreds of kind flavone compound at present, and new compound is also constantly being found.Wherein Flavanones (flavonoids) compound is different according to substituent group and position thereof, and can be divided into I aglycon-apigenin (Apigenin) is that main body, II aglycon-luteolin (Luteolin) are that main body, III aglycon-kaempferol (Kaempferol) are that main body, IV aglycon-Quercetin (Quercetin) are that main body, V naringenin (Naringin) are the totally 5 large classes of main body.The effect of flavone compound is many-sided, and it is a kind of very strong antioxidant, can effectively remove the oxygen-derived free radicals in body, can improve blood circulation, can reduce cholesterol, improves the symptom of cardiovascular and cerebrovascular disease etc.In blue or green maple, also contain flavanone compounds.

Summary of the invention

Technical problem to be solved by this invention is to provide a kind of method based on total flavones in the blue or green Folium Alangii of ultrasound wave assisted extraction that impurity is few, simple to operate, extraction ratio is high, extraction time is short.

The present invention solves the problems of the technologies described above adopted technical scheme: a kind of method based on total flavones in the blue or green Folium Alangii of ultrasound wave assisted extraction, and its step is as follows:

A, by fresh blue or green Folium Alangii sheet, under 60 ℃ of conditions, dry 24h, then pulverize, cross 0.45 μ m sieve for extracting raw material, after extraction raw material is weighed, pack in ultrasonic extraction still;

B, in ultrasonic extraction still, to add mass percentage concentration be the ethanol of 30-50 ℃, the mass volume ratio of described extraction raw material and ethanol is 1g:14-16ml, under gas-lifting type stirring condition, at 30-45 ℃, supersound extraction 30min obtains extracting solution, extracting solution concentrating under reduced pressure goes alcohol phase, and water concentrate drying obtains extractive of general flavone; Wherein ultrasonic occurring mode is: the ultrasonic sounding of independent-excited, and radial vibration column transducer, ultrasonic power is 300W, and supersonic frequency is 22-55kHz, and extracting mode is that interval 2min is once ultrasonic, each 3min.

Compared with prior art, the invention has the advantages that a kind of method based on total flavones in the blue or green Folium Alangii of ultrasound wave assisted extraction, blue or green Folium Alangii sheet drying, pulverize as extracting raw material, extract raw material and in ultrasonic extraction still, take ethanol as solvent, under gas-lifting type stirring condition, the ultrasonic tune of independent-excited, extracting mode is that interval 2min is once ultrasonic, each 3min, supersound extraction 30min obtains extracting solution, water concentrate drying just obtains extractive of general flavone from blue or green Folium Alangii, this extracting method impurity is few, extraction ratio Gao Keda is more than 97%, extraction time is short, than traditional extraction process, can shorten 10 times of above times, operation is simple, effective ingredient in medical material is had to protective effect, can not destroy the physiologically active of thermal sensitivity medicine, simultaneously, can greatly reduce energy consumption.

The specific embodiment

Below in conjunction with embodiment, the present invention is described in further detail.

Embodiment 1

By fresh blue or green Folium Alangii sheet, at 60 ℃, dry 24h, pulverize, cross 0.45 μ m sieve, obtain 50g and extract raw material, pack in ultrasonic extraction still, add the ethanol 750mL of mass percentage concentration 40%, mix, under gas-lifting type stirring condition, in 35 ℃ of supersound extraction 30min, obtain extracting solution, extracting solution concentrating under reduced pressure goes alcohol phase, and water concentrate drying obtains extractive of general flavone, and in extract, flavones content is about 72%.Ultrasonic occurring mode wherein: the ultrasonic sounding of independent-excited, radial vibration column transducer, ultrasonic power is 300W, and supersonic frequency is 33kHz, and extracting mode is that interval 2min is once ultrasonic, each 3min.

Embodiment 2

Substantially the same manner as Example 1, it is 30% ethanol 800mL that difference just adds mass percentage concentration, and supersonic frequency is 22kHz, and in extract, flavones content is about 65%.

Embodiment 3

Substantially the same manner as Example 1, it is 50% ethanol 700mL that difference just adds mass percentage concentration, and supersonic frequency is 55kHz, and in extract, flavones content is about 70%.

In above-mentioned flavone extract, the content detection of flavone compound is according to Al ³⁺-rutin binary complex fluorimetry is analyzed, excitation spectrum bandwidth 3nm, and excitation wavelength lambda ex436nm, emission spectra bandwidth 5nm, λ em483nm, rutin standard solution fluorescence intensity is to respective concentration mapping quantitatively.In extracting solution, the mensuration of active constituent content adopts high-efficient liquid phase chromatogram technique analysis in 4, and chromatographic column is Varian, and Microsorb-MV100C18 detects wavelength 360nm, and mobile phase is methanol/water=55: 45, and phosphoric acid is adjusted pH=2.5; Column temperature is 25 ℃, flow velocity is 1.0ml/min, sample size is 10 μ l, standard substance external standard method is quantitative, and in flavone extract, flavonoid content is about 65-75%, and Main Ingredients and Appearance is IV aglycon-Quercetin flavonoid monomer, as Quercetin-3-O-β-D-galactoside, Quercetin-3-O-alpha-L-rhamnoside, Quercetin, rutin etc.

The extractive of general flavone that the present invention makes has the effects such as the microcirculation of improvement, arrhythmia.On microcirculation of the heart, impact can be experimental subject with SD rat in testing, give 4.0g(crude drug) extract gastric infusion every day of/kg, after 7 days with matched group capacity gavages such as (7 days) normal saline venous blood sampling simultaneously, the adenosine diphosphate sodium salt (ADP) of take is derivant, by Born turbidimetry, survey and respectively organize platelet aggregation, and get cardiac blood simultaneously, on T hrombosis inducer, form thrombosis, result shows, administration group and matched group comparison, 1min platelet aggregation rate has obviously and reduces, difference has statistical significance (P<0.05), thrombosis length also has obvious shortening (P<0.05).In ARR impact experiment, can be experimental subject with rat, give the extract saturated solution gastric infusion of 1.0ml/kg every day, after 8 days with matched group capacity gavages such as (8 days) normal saline simultaneously Injection of Adrenaline and calcium chloride bring out arrhythmia, result administration group has been compared obvious antagonism Arrhythmia (P<0.05) with matched group.

Claims (1)

1. the method based on total flavones in the blue or green Folium Alangii of ultrasound wave assisted extraction, is characterized in that step is as follows:

A, by fresh blue or green Folium Alangii sheet, under 60 ℃ of conditions, dry 24h, then pulverize, cross 0.45 μ m sieve for extracting raw material, after extraction raw material is weighed, pack in ultrasonic extraction still;

B, in ultrasonic extraction still, to add mass percentage concentration be the ethanol of 30-50 ℃, the mass volume ratio of described extraction raw material and ethanol is 1g:14-16ml, under gas-lifting type stirring condition, at 30-45 ℃, supersound extraction 30min obtains extracting solution, extracting solution concentrating under reduced pressure goes alcohol phase, and water concentrate drying obtains extractive of general flavone; Wherein ultrasonic occurring mode is: the ultrasonic sounding of independent-excited, and radial vibration column transducer, ultrasonic power is 300W, and supersonic frequency is 22-55kHz, and extracting mode is that interval 2min is once ultrasonic, each 3min.