CN103191177B - Method for improving extraction ratio of general flavones of liana beans by quick-freezing and pulse technique - Google Patents
Method for improving extraction ratio of general flavones of liana beans by quick-freezing and pulse technique Download PDFInfo
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- CN103191177B CN103191177B CN201310117351.6A CN201310117351A CN103191177B CN 103191177 B CN103191177 B CN 103191177B CN 201310117351 A CN201310117351 A CN 201310117351A CN 103191177 B CN103191177 B CN 103191177B
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- FDRQPMVGJOQVTL-UHFFFAOYSA-N quercetin rutinoside Natural products OC1C(O)C(O)C(CO)OC1OCC1C(O)C(O)C(O)C(OC=2C(C3=C(O)C=C(O)C=C3OC=2C=2C=C(O)C(O)=CC=2)=O)O1 FDRQPMVGJOQVTL-UHFFFAOYSA-N 0.000 description 10
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Abstract
The invention provides a method for improving extraction ratio of general flavones of liana beans by a quick-freezing and pulse technique, belonging to the technical field of chemical extraction of a natural drug. The method comprises the steps of crushing and rapidly freezing the dried liana bean grains, combining with a strong pulse light to extract in an auxiliary manner; and finally filtering and collecting extracting solution to obtain a flavone crude product of the liana bean. The general flavones of climbing beans are prepared by a joint treatment technology of quick-freezing and the strong pulse light. According to the method, the technology is scientific and reasonable, the operation is simple, steps are few, the extraction flow is fast, the extraction yield is high, the product is stable, the cost is low, requirements on industrial production can be met, and the environmental pollution is avoided.
Description
Technical field
The present invention relates to a kind of method that adopts quick-freezing and pulse technique to improve liana bean total flavones extraction ratio, belong to Natural Medicine Chemistry extractive technique field.
Background technology
Liana bean is to utilize the technological meanses such as wild " liana bean " maternal male infertile and large oily bean hybridization, graininess are brought out, selfing is separated, acclimatization, a kind of high-efficiency agriculture vegetable new species of developing, has both various types such as grain, oil, dish, woods, flower, drink, medicine.Research shows, the nutrition of liana bean is extremely abundant, is rich in 18 seed amino acids of full price high-quality protein and proportioning equilibrium, and it up to more than 50%, is a kind of high-quality protein resource that has more nutritive value than soybean protein to human body institute essential amino acids content.In addition, liana bean is containing flavone, polysaccharide and other multiple active components, and medicine and health care function is remarkable, can obviously strengthen the propagation of T lymphocyte and bone-marrow-derived lymphocyte, particularly, to high-cholesterol disease, there is the serum cholesterol level of adjusting function, cardiovascular and cerebrovascular vessel are had to good health-care effect.
Flavone compound is the polyphenols that a class extensively distributes at nature, is also one of natural activity product receiving much concern at present.At present, the main extracting method of flavone has: hot water extraction method, organic solvent extractionprocess, alkaline water lifting manipulation, ultrasonic extraction, microwave method, supercritical extraction.Wherein, hot water extraction method's equipment is simple, but extraction ratio is low; Organic solvent extractionprocess is current domestic and international most popular extracting method, but has that blowdown flow rate is large, loss of effective components is many, volume is residual and the defect such as extraction efficiency is low; That alkaline water lifting manipulation has is simple, the economic feature such as convenient, but has highly basic environmental pollution problem; Ultrasonic extraction energy consumption is low, do not destroy effective ingredient, but efficiency is low while extracting in a large number; Microwave method extraction time is short, extraction ratio is high, but the composition of its finished product is not highly stable; Supercritical extraction speed is fast, penetrating power strong, dissolution extraction efficiency is high, but equipment investment is high, and extraction cost is high.And this project adopts quick-freezing and pulse strong-light Combined Treatment to extract liana bean total flavones, extraction ratio is high, cost is low, and non-environmental-pollution.
Summary of the invention
The object of the present invention is to provide a kind of method that adopts quick-freezing and pulse technique to improve liana bean total flavones extraction ratio, the method has the features such as extraction ratio is high, pollution-free, process is easy to control.
Technical scheme of the present invention is as follows:
Described method comprises the steps:
(1) dry: the fresh liana bean after gathering obtains dried liana bean seed after drying, peel off, arranging;
(2) pulverize: dried liana bean seed is pulverized, and granularity is 20～40 orders, obtains liana Semen Glycines powder;
(3) quick-freezing: liana Semen Glycines powder is put into-40～-18 ℃ of quick freezing unit quick-freezing 1.5～2.5h;
(4) pulse strong-light assisted extraction: take w/v1:15～25 solid-to-liquid ratio rapidly by the liana Semen Glycines powder after quick-freezing and volume ratio after 50～60% ethanol mix, put into container and at once carry out pulse strong-light irradiation; Then at 40～60 ℃ of temperature, extract 1～2h, finally filter and collect extracting solution, obtain liana Glycine max (L.) Merr. ketone crude product.
Wherein w/v represents mass volume ratio, and unit is g/mL or kg/L.
The water content of the liana bean after drying in step (1) is 12～14%.
Described in step (4), container is square or rectangular, material container surface opening during irradiation, and in container, material bed thickness is 4～8 cm.
Described in step (4), the intensity of pulse strong-light is 3.2～4.9J/cm
2, irradiation distance is 6～12cm, and irradiation time is 2～4s, and sudden strain of a muscle per second is according to 3 times.
Remarkable advantage of the present invention:
A) the present invention adopts quick-freezing and pulse strong-light Combined Treatment technology to carry out the preparation of liana bean total flavones, can obtain that extraction ratio is high, Functionality, quality and appealing design and free of contamination flavonoid product.
B) the present invention adopts quick-freezing and pulse strong-light Combined Treatment technology to carry out the preparation of liana bean total flavones, utilize quick-freezing and pulse strong-light Combined Treatment to destroy liana bean cell wall on the one hand, be conducive to the leaching of flavone in cell, at utmost improved extraction ratio; Utilize on the other hand instantaneous, the high-intensity pulsed light energy of pulse strong-light, shortened the subsequent extracted time, greatly improved extraction efficiency.
C) the present invention adopts quick-freezing and pulse strong-light Combined Treatment technology to carry out the preparation of liana bean total flavones, and preparation technology is simple, easy to operate, can meet the requirement of suitability for industrialized production.
The specific embodiment
Be below several specific embodiment of the present invention, further illustrate the present invention, but the present invention be not limited only to this.
Embodiment 1
Get the fresh liana bean of 100g after drying (moisture content 12.6%), peeling off, arrange, be crushed to 40 orders, put into-40 ℃ of quick freezing unit quick-freezing 1.5h; Then add the ethanol (solid-to-liquid ratio 1:20) of volume fraction 55% to be mixed, packing (material bed thickness 4 cm) after container into is 4.9J/cm by the intensity that pulse strong-light irradiates 4s(pulse strong-light
2, irradiation distance is 12cm); After extracting 2h again at 40 ℃, filter and collect extracting solution, make liana Glycine max (L.) Merr. ketone crude product.
Measure: adopt ultraviolet spectrophotometry, using rutin as standard reference material, draw rutin standard curve, measure the content of total flavones in liana bean.
(1) drafting of rutin standard curve
The rutin standard substance 12.5mg that accurately takes dry constant weight at 120 ℃, the slight fever ethanol that is 60% by concentration is settled to 50.0mL, shakes up, stand-by.
Accurately draw rutin standard substance 0,0.4,0.8,1.2,1.6,2.0,2.4mL in 6 color comparison tubes, adding respectively concentration is 60% ethanol to 2.4 mL, then adds 0. 4 mL 5% sodium nitrite, shakes up, and places 6min; Add people 0.4mL10% aluminum nitrate solution, shake up, place 6 min; Add again 4.0ml 1mol/L sodium hydroxide, shake up, place 10 ~ 15min, measure absorbance.The rutin standard substance concentration (C) of take is abscissa, and absorbance (y) is vertical coordinate drawing standard curve.
(2) mensuration of general flavone content in liana bean
The accurate sample solution 2mL that draws, is placed in 10mL band plug glass tubing, by standard curve method, measures general flavone content, according to following formula, calculates total flavones extraction ratio.
Total flavones extraction ratio Y (mg/g)=CV/M
In formula: C is flavone concentration mg/mL in sample solution;
V is sample solution cumulative volume mL;
M is the liana bean quality g taking.
According to above-mentioned formula, in liana bean, the extraction ratio of total flavones is 5.32 mg/g; Liana bean (other condition is the same) the total flavones extraction ratio of processing with pulse strong-light without quick-freezing is 4.96 mg/g; Liana bean (other condition is the same) total flavones extraction ratio without pulse strong-light processing through fast frozen is 5.07mg/g; Liana bean (other condition is the same) the total flavones extraction ratio of processing through pulse strong-light without fast frozen is 5.12 mg/g.Visible, adopt quick-freezing and pulse strong-light Combined Treatment technology to carry out the preparation of liana bean total flavones, can obtain that extraction ratio is high, Functionality, quality and appealing design and free of contamination flavonoid product.
Embodiment 2
Get the fresh liana bean of 200g after drying (moisture content 13.1%), peeling off, arrange, be crushed to 20 orders, put into-18 ℃ of quick freezing unit quick-freezing 2.5h; Then add the ethanol (solid-to-liquid ratio 1:25) of volume fraction 60% to be mixed, packing (material bed thickness 6cm) after container into is 4.9J/cm by the intensity that pulse strong-light irradiates 2s(pulse strong-light
2, irradiation distance is 6cm); After extracting 1.5h again at 50 ℃, filter and collect extracting solution, make liana Glycine max (L.) Merr. ketone crude product.
Assay method is with embodiment 1: adopt ultraviolet spectrophotometry, using rutin as standard reference material, draw rutin standard curve, the content of measuring total flavones in liana bean is 5.21 mg/g; 20 order liana bean (other condition is the same) the total flavones extraction ratios of processing with pulse strong-light without quick-freezing are 4.85 mg/g; Liana bean (other condition is the same) total flavones extraction ratio without pulse strong-light processing through fast frozen is 4.95mg/g; Liana bean (other condition is the same) the total flavones extraction ratio of processing through pulse strong-light without fast frozen is 5.03 mg/g.
Embodiment 3
Get the fresh liana bean of 180g after drying (moisture content 12.3%), peeling off, arrange, be crushed to 30 orders, put into-30 ℃ of quick freezing unit quick-freezing 2h; Then add the ethanol (solid-to-liquid ratio 1:15) of volume fraction 50% to be mixed, packing (material bed thickness 8cm) after container into is 3.2J/cm by the intensity that pulse strong-light irradiates 3s(pulse strong-light
2, irradiation distance is 8cm); After extracting 1h again at 60 ℃, filter and collect extracting solution, make liana Glycine max (L.) Merr. ketone crude product.
Assay method is with embodiment 1: adopt ultraviolet spectrophotometry, using rutin as standard reference material, draw rutin standard curve, the content of measuring total flavones in liana bean is 5.42 mg/g; 20 order liana bean (other condition is the same) the total flavones extraction ratios of processing with pulse strong-light without quick-freezing are 5.01 mg/g; Liana bean (other condition is the same) total flavones extraction ratio without pulse strong-light processing through fast frozen is 5.12mg/g; Liana bean (other condition is the same) the total flavones extraction ratio of processing through pulse strong-light without fast frozen is 5.17mg/g.
Claims (3)
1. adopt quick-freezing and pulse technique to improve a method for liana bean total flavones extraction ratio, it is characterized in that described method comprises the steps:
(1) dry: the fresh liana bean after gathering obtains dried liana bean seed after drying, peel off, arranging;
(2) pulverize: dried liana bean seed is pulverized, and granularity is 20～40 orders, obtains liana Semen Glycines powder;
(3) quick-freezing: liana Semen Glycines powder is put into-40～-18 ℃ of quick freezing unit quick-freezing 1.5～2.5h;
(4) pulse strong-light assisted extraction: take w/v1:15～25 solid-to-liquid ratio rapidly by the liana Semen Glycines powder after quick-freezing and volume ratio after 50～60% ethanol mix, put into container and at once carry out pulse strong-light irradiation; Then at 40～60 ℃ of temperature, extract 1～2h, finally filter and collect extracting solution, obtain liana Glycine max (L.) Merr. ketone crude product; The intensity of described pulse strong-light is 3.2～4.9J/cm
2, irradiation distance is 6～12cm, and irradiation time is 2～4s, and sudden strain of a muscle per second is according to 3 times.
2. a kind of method that adopts quick-freezing and pulse technique to improve liana bean total flavones extraction ratio according to claim 1, is characterized in that: the water content of the liana bean after drying in step (1) is 12～14%.
3. a kind of method that adopts quick-freezing and pulse technique to improve liana bean total flavones extraction ratio according to claim 1, it is characterized in that: described in step (4), container is square or rectangular, material container surface opening during irradiation, and in container, material bed thickness is 4～8 cm.
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| CN108523115A (en) * | 2018-03-30 | 2018-09-14 | 福建省农业科学院农业工程技术研究所 | A kind of chewable tablets and preparation method thereof with health-care effect |
| CN108477600B (en) * | 2018-03-30 | 2021-07-06 | 福建省农业科学院农业工程技术研究所 | Morchella esculenta slice and preparation method thereof |
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| CN102166004A (en) * | 2011-03-08 | 2011-08-31 | 马涛 | Method for preparing germinated brown rice by intensive pulse light |
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| CN102166004A (en) * | 2011-03-08 | 2011-08-31 | 马涛 | Method for preparing germinated brown rice by intensive pulse light |
Non-Patent Citations (5)
| Title |
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| 殷涌光,等.高压脉冲电场法提取干松针总黄酮及其体外抗氧化性检测.《天然产物研究与开发》.2009,第21卷第1032-1035页、第1056页. * |
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