Method for extracting and purifying vitexin and isoviextin from cajanus cajan branches and leaves
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A technology of isovitexin and vitexin, applied in the field of separation and purification of functional components, can solve the problems of large amount of organic solvent, backward extraction process, low yield, etc., and achieves simple and easy method, efficient and reasonable utilization, and product high yield effect
Active Publication Date: 2011-06-15
NORTHEAST FORESTRY UNIVERSITY +1
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The traditional purification process is long and the loss of the target compound is large. Multiple silica gel column chromatography is used. The operation steps are numerous and the eluent is mainly toxic and expensive reagents such as chloroform, acetone, and ethyl acetate.
In the Chinese patent "Rapid Preparation Method of Several High-purity Medicinal Substances in Patrinia dahliae" (publication number CN1683386), isovitexin was prepared by traditional liquid-liquid extraction, column chromatography and high-efficiency countercurrent chromatography. Long, large amount of organic solvents, and restricted by instruments and equipment
Lin Li (1999) used traditional column chromatography to separate vitexin and isovitexin, which took a long time and the yield was low
[0005] In summary, in the process of using plant resources to separate and purify vitexin and isovitexin, the main influencing factors are the backward extraction process and the widespread loss of vitexin and isovitexin in the process of raw material treatment and separation , The purification process is long, which increases the cost
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Embodiment 1
[0021] Weigh 1000g of pigeon pea dry branches and leaves, add 8 times the volume of 75% ethanol, continuously homogenize and extract 3 times, each 1min, and then ultrasonically assist extraction 3 times under the condition of 35~50°C (add 75% ethanol for the second time The amount is 6 times of the solid mass, the third time is 4 times), each time for 45 minutes, the three extracts are combined, and concentrated under reduced pressure until no obvious liquid flows out.
[0022] Add the concentrated solution into warm water (4.5L) at 60°C, vibrate in an ultrasonic extractor at 30-50KHz for 15-25min, stand still for 10-15min, take the supernatant, and use 0.05MPa negative pressure as the power to extract it with 4L ethyl acetate. Negative pressure cavitation suspension was extracted 3 times, the extract was concentrated, and the obtained solid was warmed and suspended with 8% ethanol to prepare a sample solution with a feed concentration of 10mg / mL, and the maximum sample volume ...
Embodiment 2
[0026] Take by weighing 4.79kg of fresh pigeonpea branches and leaves (dry weight is 1kg), after adding 6 times the volume of 85% ethanol, continuous homogenate extraction 3 times, each time 1.5min, then ultrasonically assisted extraction 3 times under the condition of 35~50 ℃ ( The second and third additions of 85% ethanol are 4 times the solid mass), each time for 45 minutes, the three extracts are combined, concentrated under reduced pressure until no obvious liquid flows out.
[0027]Add the concentrated solution into warm water (4.5L) at 50-60°C, vibrate for 15-25min at 50-60KHz in an ultrasonic extractor, rest for 10-15min, take the supernatant, and use negative pressure as the power to extract it with 4L ethyl acetate. Negative pressure cavitation suspension was extracted 3 times, the extract was concentrated, the obtained solid was suspended with 8% ethanol, and the sample solution with a feed concentration of 12mg / mL was prepared, and the maximum sample volume was 15mg...
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Abstract
The invention relates to an extraction and purification method of the component with the Chinese herbal medicine functionality, and aims at providing a method of obtaining monomeric compound Vitexin and Isovitexin through extraction and purification from pigeon pea branches and leaves in a simple, safe, economical and high-efficient manner. The invention has the technical proposal of using the fresh and dried pigeon pea branches and the leaves as raw materials, and adopting the combination of a homogenate extraction technique, an ultrasonic assistance extraction technique, an ultrasonic oscillation flocculation technique, a negative pressure cavitation suspension extraction technique, a macropore absorbing resin collecting technique, an ODS-C18 reversed phase medium pressing silicagel column chromatography technique, a low temperature recrystallization and a recrystallization technique, and then the Vitexin and the Isovitexin with the purity of more than 90 percent are obtained, and the extraction rate is more than 0.17 percent and 0.13 percent respectively. The raw material used by the invention is the wasted fresh or dried pigeon pea branches and leaves in the agricultural production, thus the invention cannot damage the ecological balance of plants and affect the agricultural production, and can further get the pigeon pea functionality component. Moreover, the method has the steps of extraction, primary decontaminating and purification, and is simple and practical with little objective compound, thus the method is applicable for the industry application, and has important meaning to the industrialized production.
Description
technical field [0001] The invention relates to a method for separating and purifying functional components from plants, in particular extracting and purifying vitexin and isovitexin from fresh or dry branches and leaves of pigeonpea. Background technique [0002] Pigeon pea [Cajanus cajan (L.) Millsp.] is an annual or perennial woody plant and evergreen shrub of the genus Fabaceae. Also known as pigeon beans, tree soybeans, etc., it is a folk medicine. It has cooling, heat-reducing, detoxifying, analgesic, hemostatic, antibacterial and anti-inflammatory effects. It is used in folks to treat trauma, burns, infections, bedsores, antibacterial and anti-inflammatory, etc. (Liu Zhongqiu et al., 1998; Sun Shaomei et al., 1995). In addition, pigeonpea extract preparations are used in India, Brazil, Cuba, Mexico, South Africa and other countries to treat colds, bronchitis, measles, dysentery, hepatitis, skin diseases, burns, ulcers, tumors and other diseases (Abbiw DK., 1990; Duk...
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