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Method for efficiently separating and purifying caffeoylquinic acid isomers from mulberry leaves

A technology for separation, purification and caffeoyl, which is applied in the field of efficient separation and purification of caffeoylquinic acid isomers, can solve problems such as not being used, and achieve the effects of reducing the number of extractions, reducing industrial costs and saving time.

Active Publication Date: 2019-07-16
BEIJING FORESTRY UNIVERSITY +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] However, at present, there are few studies on the separation and purification of caffeoylquinic acid isomers in mulberry leaves at home and abroad, and high-speed countercurrent chromatography has not yet been applied in the separation of caffeoylquinic acid isomers. A high-speed countercurrent chromatography method for the rapid separation of caffeoylquinic acid isomers in mulberry leaves is necessary

Method used

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  • Method for efficiently separating and purifying caffeoylquinic acid isomers from mulberry leaves
  • Method for efficiently separating and purifying caffeoylquinic acid isomers from mulberry leaves
  • Method for efficiently separating and purifying caffeoylquinic acid isomers from mulberry leaves

Examples

Experimental program
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Effect test

Embodiment 1

[0068] (1) Ultrasound-enhanced extraction: Accurately weigh 1 kg of mulberry leaf sample powder, use 4 L of ethanol with a volume concentration of 50% as a solvent, conduct ultrasonic treatment at room temperature for 45 minutes, extract 3 times, combine 3 extracts and filter, and concentrate the filtrate Until there is no alcohol smell, the concentrated extract is obtained;

[0069] (2) Ultrasonic vibration flocculation: Dissolve the concentrated extract in 2000mL of 40°C water for ultrasonic vibration flocculation. The ultrasonic vibration time is 5min and the frequency is 30KHz.

[0070] (3) pH-induced liquid-liquid extraction: use n-butanol to extract the supernatant, the volume ratio of n-butanol and supernatant is 1:1, the pH value of the extraction is 4, the extraction times is 5 times, and the n-butanol is concentrated The alcohol layer was dried to obtain the extracted product, and the extracted product was mixed with water and subjected to ultrasonic vibration floccu...

Embodiment 2

[0084] The separation effect of the high-speed countercurrent chromatography (HSCCC) method mainly depends on the selection of the two-phase solvent system, and the selection of the two-phase solvent system mainly considers the partition coefficient K and separation factor α of the separated substance in the solvent system. The best K value of HSCCC is generally 0.2-2.0. If the K value > 2.0, the separation time of the target component will be prolonged; when the K value < 0.2, the target component overlaps with other components and cannot be separated. In order to obtain better The separation factor α is preferably greater than 1.5.

[0085] In this example, the partition coefficient K of different caffeoylquinic acids in different two-phase solvent systems was measured by HPLC method, and the results are shown in Table 1.

[0086] Table 1 Distribution coefficient table of different caffeoylquinic acids in different two-phase solvent systems

[0087]

[0088]

[0089] ...

Embodiment 3

[0091] Other steps are the same as in Example 1, except that the pH value extracted in step (3) is changed to 5, the number of extractions is 5 times, the n-butanol layer is concentrated and dissolved in water to 2000mL, and the macroporous adsorption resin static adsorption sample solution is obtained. , the initial concentration of neochlorogenic acid in the sample solution was 0.47 mg / mL, the initial concentration of chlorogenic acid was 1.29 mg / mL, and the initial concentration of cryptochlorogenic acid was 0.65 mg / mL.

[0092] Carry out macroporous adsorption resin enrichment, high-speed countercurrent chromatography fast separation, low-temperature crystallization and recrystallization according to the method in embodiment 1, wherein the yield of new chlorogenic acid, chlorogenic acid and cryptochlorogenic acid after high-speed countercurrent chromatography fast separation Respectively can reach 80.59%, 99.56%, 94.21%, purity can reach 93.75%, 93.62%, 95.22%.

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Abstract

The invention relates to the field of separation purification of natural products, and provides a method for efficiently separating and purifying caffeoylquinic acid isomers from mulberry leaves. Themethod comprises the following steps: performing ultrasonic wave enhanced extraction on the mulberry leaves, and performing separation purification by adopting an original pH induction liquid-liquid extraction technology, a macroporous adsorption resin enrichment technology and a high-speed countercurrent chromatography rapid separation technology to obtain the three caffeoylquinic acid isomers with purity of 93% or more. According to the method provided by the invention, caffeoylquinic acid rapidly enters an organic phase by the pH induction liquid-liquid extraction to reduce extraction times, so that the time is saved, chemical reagent consumption is reduced, and the industrial costs are reduced; and the method realizes the purpose of separating the caffeoylquinic acid isomers from the mulberry leaves by using the high-speed countercurrent chromatography rapid separation technology for the first time, the method has the advantages of simple steps, low solvent consumption, a short separation period, high product purity and a high yield, and is suitable for industrial production and application.

Description

technical field [0001] The invention relates to the technical field of separation and purification of natural products, in particular to a method for efficiently separating and purifying caffeoylquinic acid isomers from mulberry leaves. Background technique [0002] Mulberry leaf (English name: Mulberry Leaf, medicinal material name: Folium Mori) is the dry leaf of Moraceae plant mulberry. In my country, mulberry leaves are widely used as feed for silkworms, and they are also traditional bulk Chinese medicinal materials and homologous plants with various pharmacological activities. According to the "Chinese Pharmacopoeia-2015 Edition Part One", mulberry leaves are sweet, bitter, and cold in nature and have the effects of dispersing wind-heat, clearing lungs and moistening dryness, clearing liver and improving eyesight, and are often used for wind-heat cold and red eyes, swelling and pain , lung heat dry cough, wind fire eye disease and other diseases treatment. Modern medi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/732C07C67/48C07C67/58C07C67/56C07C67/52
CPCC07B2200/07C07C67/48C07C67/52C07C67/56C07C67/58C07C2601/14C07C69/732
Inventor 付玉杰王立涛孟冬杨清崔琦董明珠高明珠
Owner BEIJING FORESTRY UNIVERSITY
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