CN103933187B - A kind of method for quickly purifying of longan pericarp flavones - Google Patents
A kind of method for quickly purifying of longan pericarp flavones Download PDFInfo
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- CN103933187B CN103933187B CN201410138802.9A CN201410138802A CN103933187B CN 103933187 B CN103933187 B CN 103933187B CN 201410138802 A CN201410138802 A CN 201410138802A CN 103933187 B CN103933187 B CN 103933187B
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Abstract
The present invention relates to a kind of method for quickly purifying of longan pericarp flavones, belong to Effective Component of Chinese Medicine and extract purification technique field, specifically, by regulating longan pericarp flavone extractive pH value, longan pericarp flavones is separated out at isoelectric point crystallizing, more after filtration, washing, dissolve, recrystallization, obtains highly purified longan pericarp flavones, agents useful for same of the present invention is sodium hydroxide solution, the hydrochloric acid solution of non-toxic inexpensive, and the longan pericarp flavones purification process providing is a kind of simple to operate, efficiency is high, cost is low method.
Description
[technical field]
The present invention relates to a kind of natural plant active component purification process, be specifically related to a kind of longan pericarpThe method for quickly purifying of flavones, belongs to Effective Component of Chinese Medicine and extracts purification technique field.
[background technology]
Longan DimocarpusLonganLour. latin name DimocarpuslonganLour,Popular name longan is the famous subtropical fruit of China. Longan originates in south China and Vietnam northThe south subtropics of portion, at existing more than the 2000 year cultivation history of China, is one of four good fruits in the large south of the Five Ridges.Meat, core, flower and the root of longan all can be used as Chinese medicine preparation. Every year in arillus longan processIn, producing a large amount of longan pericarps, these longan pericarps are often dropped, or as farm manure, adoptExtract by the method for high efficiency, low cost the Flavonoid substances that has economic worth in longan pericarp, will createMake high economic benefit.
In longan pericarp, contain the bioactive ingredients such as a large amount of alkaloids, flavones, polyphenol. DomesticThe nutritional labeling of what outer scholar studied at most to longan is research longan pulp, chemical composition,Pharmacological action and health-care effect; What next studied morely is longan seed. Forefathers are to longan seedResearch mainly concentrates on the research of longan seed chemical composition, nutritional labeling and mineralogical composition; ResearchMinimum be longan pericarp, the research of longan pericarp is partial in extending longan shelf life process to longan pericarpBrown stain, and the research of chemical composition to longan pericarp is little. What on a small quantity longan pericarp is carried outIn research, can see, research is mostly around longan pericarp chemical composition analysis, antioxidant contentUltrasonic wave assisted extraction or Microwave-assisted Extraction are got, and carry out the qualification aspect of antioxidant content.Wherein Zhou Mengqing etc. is in " microwave assisting method extract longan pericarp in the research of flavone compound "Carry out the research that microwave assisting method extracts flavone compound in longan pericarp.
That does in the research aspect longan pericarp flavones purifying is also fewer, and wherein Wang Wei etc. is " dragonThe research of anti-oxidation active substance in eye " in adopted the dragon to alcohol extract through polyamideAntioxidant content in eye has carried out purifying, detects to analyze to show and may contain through high efficiency liquid phaseGallic acid, rutin and ellagic acid. Liao Na passes through in " research of longan pericarp chemical composition "Silica gel column chromatography, the method for thin-layer chromatography is carried out the Antioxidation of Extract from Longan Pericarp composition that purifying ethanol extracts,Obtain Quercetin. At present the purifying of various Flavonoid substances is substantially all adopted to column chromatography, thinAnalyse layer by layer, the method such as preparative high-efficient liquid phase technique. In the patent of invention of Jiang Huidi etc., " chrysanthemum is totalFlavones purifying resin method " in, adopting HPD-100 large aperture resin to carry out purifying corn must be total yellowKetone. It is low that but above flavones purification process all has efficiency, and cost is high, solvent-oil ratio and residualThe problems such as allowance is large, output is restricted.
The present invention utilizes and regulates longan pericarp flavone extractive pH value, makes longan pericarp flavones in isoelectric pointCrystallization, the method purifying longan pericarp flavones, more than purity to 98%, yield reaches1.50%-1.65%, method of operating is simple, purification efficiency is high, cost is low, is worthy to be popularized.
[summary of the invention]
The object of this invention is to provide a kind of method for quickly purifying of longan pericarp flavones, simple to operate,Purification efficiency is high, cost is low.
For realizing the object of foregoing invention, the technical scheme that the present invention takes is as follows:
A method for quickly purifying for longan pericarp flavones, is characterized in that comprising the steps:
(1) filter: prepare longan pericarp flavone extractive, by circulation for longan pericarp flavone extractiveWater vavuum pump carries out suction filtration, discards filter residue, reserved filtrate;
(2) regulate pH value: with NaOH solution, HCl solution adjusting longan pericarp extract pHValue is to isoelectric point;
(3) crystallization: longan pericarp flavones solubility under this pH significantly reduces, and has crystallization;
(4) filter: wait to be crystallized completing, adopt vacuum pump using circulatory water to carry out suction filtration, tiedCrystal;
(5) washing: use distilled water flushing crystalline solid, crystal is shifted after washing away impurity;
(6) dissolve: with dissolve with ethanol solution longan pericarp flavones crystal;
(7) recrystallization: the method recrystallization of repeating step (2)～(5), obtains high-purityLongan pericarp flavones crystal.
As mentioned above, step (1) detailed process is as follows: longan pericarp powder is taking 80% ethanol as extractionSolvent, quality solid-to-liquid ratio is 1:25, soaks after 1 hour, under ultrasonic-microwave cooperating effectExtract twice and merging filtrate, then carry out suction filtration with vacuum pump using circulatory water, obtain longan pericarp HuangKetone extract.
As above ultrasonic-microwave cooperating effect refers to microwave power 300W, ultrasonic wave is opened.
What as mentioned above, step (2) was described uses NaOH solution, HCl solution to regulate longan pericarpExtracting liquid pH value refers to when pH value is too high and finely tunes with HCl solution, if pH value is too lowWith the fine setting of NaOH solution, pH value is transferred to isoelectric point, until there is crystal to separate out.
As mentioned above, in step (1) and step (4), vacuum pump using circulatory water is at vacuum 0.1MPaUnder carry out suction filtration.
As mentioned above, the described isoelectric point of step (2) is pH value 4.30～4.60.
As mentioned above, the described NaOH solution concentration of step (2) is 0.1moLL-1～ 0.5moL·L-1, HCl solution concentration is 0.5moLL-1～1moL·L-1。
As mentioned above, the medium deadline to be crystallized of step (4) is 3～5min.
What in step (6), adopt as mentioned above, is that quality solid-to-liquid ratio is the dense of 1:20～1:25Degree is that 80% ethanolic solution dissolves longan pericarp flavones crystal.
Compared with prior art, the present invention has following beneficial effect:
1, the method for quickly purifying of longan pericarp flavones provided by the invention is simple to operate, efficiency is high,Solvent-oil ratio and residual quantity are little;
2, agents useful for same NaOH, HCl and ethanolic solution are all cheap and nontoxic, and cost is low, safetyProperty is good, is convenient to crystallization;
3, purify longan pericarp flavones by the inventive method, its purity is high, and favorable reproducibility, easilyBe applied to suitability for industrialized production.
[detailed description of the invention]
Below by specific embodiment, the present invention is further described in detail, so that originally clearThe technical scheme that invention is protected.
Embodiment 1
(1) longan pericarp flavones extract: by 10.1g longan pericarp powder taking 80% ethanol as extract solvent,Quality solid-to-liquid ratio is 1:25, soaks after 1 hour, in ultrasonic-microwave cooperating effect (microwave meritRate 300W, ultrasonic wave is opened, 45 DEG C of constant temperature) lower extraction twice and merging filtrate, use recirculated waterVavuum pump is under vacuum 0.1MPa after suction filtration 20s, and Rotary Evaporators reclaims ethanol, must be higherConcentration extract.
(2) longan pericarp general flavone purifying: use NaOH solution and HCl solution adjusting extractPH value is to isoelectric point 4.35, and longan pericarp flavones crystallization, uses vacuum pump using circulatory water in vacuumUnder 0.1MPa, suction filtration 25s obtains the crystallization of longan pericarp flavones, and crystallization is removed to crystal with distilled water washingSurface impurity, after be transferred to the second that the concentration that is 1:20 by quality solid-to-liquid ratio in small beaker is 80%Alcoholic solution dissolves longan pericarp flavones crystal, repeats above-mentioned steps and is recrystallized, and obtains longan pericarpAfter flavones crystal, weigh, obtain 0.162g, yield reaches 1.60%.
Embodiment 2
(1) longan pericarp flavones extract: by 10.0g longan pericarp powder taking 80% ethanol as extract solvent,Liquid-solid ratio is 1:25, soak after 1 hour, ultrasonic-microwave cooperating effect (microwave power 300W,Ultrasonic wave is opened, 45 DEG C of constant temperature) lower extraction twice and merging filtrate, use vacuum pump using circulatory water to existUnder vacuum 0.1MPa, after suction filtration 30s, Rotary Evaporators reclaims ethanol, obtains higher concentration and extractsLiquid.
(2) longan pericarp general flavone purifying: use NaOH solution and HCl solution adjusting extractPH value is to isoelectric point 4.31, and longan pericarp flavones crystallization, uses vacuum pump using circulatory water in vacuumUnder 0.1MPa, suction filtration 30s obtains the crystallization of longan pericarp flavones, and crystallization is removed to crystal with distilled water washingSurface impurity, after be transferred to the second that the concentration that is 1:23 by quality solid-to-liquid ratio in small beaker is 80%Alcoholic solution dissolves longan pericarp flavones crystal, repeats above-mentioned steps and is recrystallized, and obtains longan pericarpAfter flavones crystal, weigh, obtain 0.158g, yield reaches 1.58%.
Embodiment 3
(1) longan pericarp flavones extract: by 10.0g longan pericarp powder taking 80% ethanol as extract solvent,Liquid-solid ratio is 1:25, soak after 1 hour, ultrasonic-microwave cooperating effect (microwave power 300W,Ultrasonic wave is opened, 45 DEG C of constant temperature) lower extraction twice and merging filtrate, use vacuum pump using circulatory water to existUnder vacuum 0.1MPa, after suction filtration 20s, Rotary Evaporators reclaims ethanol, obtains higher concentration and extractsLiquid.
(2) longan pericarp general flavone purifying: use NaOH solution and HCl solution adjusting extractPH value is to isoelectric point 4.36, and longan pericarp flavones crystallization, uses vacuum pump using circulatory water in vacuumUnder 0.1MPa, suction filtration 20s obtains the crystallization of longan pericarp flavones, and crystallization is removed to crystal with distilled water washingSurface impurity, after be transferred to the second that the concentration that is 1:25 by quality solid-to-liquid ratio in small beaker is 80%Alcoholic solution dissolves longan pericarp flavones crystal, repeats above-mentioned steps and is recrystallized, and obtains longan pericarpAfter flavones crystal, weigh, obtain 0.165g, yield reaches 1.65%.
Embodiment 4
(1) longan pericarp flavones extract: by 10.2g longan pericarp powder taking 80% ethanol as extract solvent,Liquid-solid ratio is 1:25, soak after 1 hour, ultrasonic-microwave cooperating effect (microwave power 300W,Ultrasonic wave is opened, 45 DEG C of constant temperature) lower extraction twice and merging filtrate, use vacuum pump using circulatory water to existSuction filtration 35s under vacuum 0.1MPa, Rotary Evaporators reclaims ethanol, obtains higher concentration extract.
(2) longan pericarp general flavone purifying: use NaOH solution and HCl solution adjusting extractPH value is to isoelectric point 4.50, and longan pericarp flavones crystallization, uses vacuum pump using circulatory water in vacuumUnder 0.1MPa, suction filtration 35s obtains the crystallization of longan pericarp flavones, and crystallization is removed to crystal with distilled water washingSurface impurity, after be transferred to the second that the concentration that is 1:20 by quality solid-to-liquid ratio in small beaker is 80%Alcoholic solution dissolves longan pericarp flavones crystal, repeats above-mentioned steps and is recrystallized, and obtains longan pericarpAfter flavones crystal, weigh, obtain 0.160g, yield reaches 1.57%.
In the above embodiment of the present invention, the high-purity longan pericarp flavones crystal obtaining is by efficientLiquid chromatography detects it for rutin, and as mentioned above, above embodiment is only of the present invention preferredEmbodiment, can not limit protection scope of the present invention with this, and those skilled in the art existsThe variation of any unsubstantiality doing on basis of the present invention and replacement all belong to guarantor of the present inventionProtect scope.
Claims (7)
1. a method for quickly purifying for longan pericarp flavones, is characterized in that comprising the steps:
(1) filter: prepare longan pericarp flavone extractive, by circulation for longan pericarp flavone extractiveWater vavuum pump carries out suction filtration, discards filter residue, reserved filtrate;
(2) regulate pH value: with NaOH solution, HCl solution adjusting longan pericarp extract pHValue is to isoelectric point;
(3) crystallization: longan pericarp flavones solubility under this pH significantly reduces, and has crystallization;
(4) filter: wait to be crystallized completing, adopt vacuum pump using circulatory water to carry out suction filtration, tiedCrystal;
(5) washing: use distilled water flushing crystalline solid, crystal is shifted after washing away impurity;
(6) dissolve: with dissolve with ethanol solution longan pericarp flavones crystal;
(7) recrystallization: the method recrystallization of repeating step (2)～(5), obtains high-purityLongan pericarp flavones crystal;
Wherein, step (1) detailed process is as follows: longan pericarp powder taking 80% ethanol as extract solvent,Quality solid-to-liquid ratio is 1:25, soaks after 1 hour, under ultrasonic-microwave cooperating effect, extracts twoInferior and merging filtrate, then carries out suction filtration with vacuum pump using circulatory water, obtains longan pericarp flavones and extractsLiquid; The described isoelectric point of step (2) is pH value 4.30～4.60.
2. the method for quickly purifying of a kind of longan pericarp flavones according to claim 1, its spyLevy and be: described ultrasonic-microwave cooperating effect refers to microwave power 300W, ultrasonic wave is opened.
3. the method for quickly purifying of a kind of longan pericarp flavones according to claim 1, its spyLevy and be: what step (2) was described uses NaOH solution, HCl solution to regulate longan pericarp extractPH value refers to when pH value is too high and finely tunes with HCl solution, if the too low NaOH that uses of pH valueSolution fine setting, is transferred to isoelectric point by pH value, until there is crystal to separate out.
4. according to the fast purifying of a kind of longan pericarp flavones described in claim 1-3 any oneMethod, is characterized in that: in step (1) and step (4), vacuum pump using circulatory water is in vacuumUnder degree 0.1MPa, carry out suction filtration.
5. according to the fast purifying of a kind of longan pericarp flavones described in claim 1-3 any oneMethod, is characterized in that: the described NaOH solution concentration of step (2) is 0.1moLL-1～0.5moL·L-1, HCl solution concentration is 0.5moLL-1～1moL·L-1。
6. according to the fast purifying of a kind of longan pericarp flavones described in claim 1-3 any oneMethod, is characterized in that: the medium deadline to be crystallized of step (4) is 3～5min.
7. according to the fast purifying of a kind of longan pericarp flavones described in claim 1-3 any oneMethod, is characterized in that: what in step (6), adopt is that quality solid-to-liquid ratio is 1:20～1:25Concentration be that 80% ethanolic solution dissolves longan pericarp flavones crystal.
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| 龙眼壳总黄酮提取及鉴别;黄锁义等;《中药材》;20060831;第29卷(第8期);权利要求1-14 * |
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