Method for simultaneously separating flavonoid and chlorogenic acid compounds in hawthorn leaf crude extracts

Abstract

The invention discloses a method for simultaneously separating flavonoid and chlorogenic acid compounds in hawthorn leaf crude extracts. The method is characterized by including the steps: taking thehawthorn leaf crude extracts as raw materials, sufficiently dissolving the hawthorn leaf crude extracts by distilled water, filtering out insoluble substances, enabling filter liquid to pass a macro-porous resin column, eluting the filter liquid by eluant in a section dividing manner, collecting the eluant, and performing reduced pressure distillation on the collected eluant to obtain hawthorn leaf flavonoid with the purity of 58% or more and chlorogenic acid compounds the purity of 67% or more; continuing to refine the hawthorn leaf flavonoid by a preparative chromatography to obtain vitexinglucoside and vitexin rhamnoside with the purity of 96% or more. According to the method, high-purity hawthorn leaf flavonoid (the purity is 58% or more), vitexin glucoside (the purity is 96% or more), vitexin rhamnoside (the purity is 96% or more) and chlorogenic acid compounds (the purity is 67% or more) is simultaneously acquired by the aid of a simple process, the process is simple and feasible, production efficiency is high, the utilization rate of raw materials is high, and the method is applicable to industrial production and has high production and practical values.

Description

Technical field:

[0001] The invention relates to the technical field of separation of crude extract of hawthorn leaves, in particular to a method for simultaneously separating flavonoids and chlorogenic acid compounds from the crude extract of hawthorn leaves. Background technique:

[0002] Hawthorn leaf is a commonly used traditional Chinese medicine. It is a plant of Rosaceae Shanlihong ( Crataegus pinnatifida Bge .Var. major N. E. Br.) or hawthorn ( Crataegus pinnatifida Bge . ) dry leaves, which belong to the liver meridian, have the effects of promoting blood circulation, removing blood stasis, regulating qi and dredging channels, etc., and are mainly used for the clinical treatment of qi stagnation and blood stasis, chest pain and heartache, chest tightness and shortness of breath, palpitation and forgetfulness, dizziness, tinnitus, hyperlipidemia, etc. my country's Northeast, North China, Yunnan, Xinjiang and other places are all important hawthorn producing ar...

Examples

Embodiment 1

[0018] Example 1, 60g of hawthorn leaf crude extract, add 500mL distilled water for ultrasonic dissolution, filter out the insoluble matter, and the filtrate flows through the HPD-400 macroporous resin column at a flow rate of 3BV / h; after the adsorption is completed, the HPD-400 macroporous resin column First fully eluted with 5BV of distilled water, collected the eluate of the first stage, concentrated and freeze-dried, and obtained 5.49g of chlorogenic acid compounds with a purity of 70.3%; HPD-400 macroporous resin column was then washed with 5BV of 50% ethanol The aqueous solution is fully eluted, the second stage eluent is collected, and after the solvent is recovered by distillation under reduced pressure, 19.32g of total flavonoids from hawthorn leaves with a purity of 59.7% are obtained; the total flavonoids from hawthorn leaves are dissolved in 50mL of methanol, and refined using preparative chromatography. 18 Chromatography column (50´250 mm, 10 μm), 35 / 65 (V / V) 0.1%...

Embodiment 2

[0019] Example 2, 300g of hawthorn leaf crude extract, add 2500mL distilled water for ultrasonic dissolution, filter out the insoluble matter, and the filtrate flows through the HPD-300 macroporous resin column at a flow rate of 2BV / h; after the adsorption is completed, the HPD-300 macroporous resin column First fully eluted with 8BV of distilled water, collected the eluate of the first stage, concentrated and freeze-dried to obtain 25.4g of chlorogenic acid compounds with a purity of 67.1%; The aqueous solution was fully eluted, and the second eluent was collected. After the solvent was recovered by distillation under reduced pressure, 96.87g of total flavonoids from hawthorn leaves with a purity of 58.1% were obtained; 18 Chromatographic column (50´250 mm, 10 μm), 35 / 65 (V / V) 0.1% acetic acid aqueous solution / formonitrile}, collected monomer eluents and distilled under reduced pressure to obtain 1.37 g of 96.0% purity Vitexin glucoside and 6.39 g of vitexin rhamnoside with a...

Embodiment 3

[0020] Example 3, 600g of hawthorn leaf crude extract, add 5000mL distilled water for ultrasonic dissolution, filter out the insoluble matter, and the filtrate flows through the HPD-750 macroporous resin column at a flow rate of 2BV / h; after the adsorption is completed, the HPD-750 macroporous resin column First fully eluted with 10BV of distilled water, collected the eluate of the first stage, concentrated and freeze-dried, and obtained 51.13g of chlorogenic acid compounds with a purity of 67.2%; The aqueous solution is fully eluted, the second stage eluent is collected, and after the solvent is recovered by distillation under reduced pressure, 196.53g of total flavonoids from hawthorn leaves with a purity of 58.0% are obtained; the total flavonoids from hawthorn leaves are dissolved in 500mL of methanol and refined using preparative chromatography. 18 Chromatographic column (50´250 mm, 10 μm), 35 / 65 (V / V) 0.1% formic acid / methanol}, respectively collected monomer eluents and ...

Technical field:

[0001] The invention relates to the technical field of separation of crude extract of hawthorn leaves, in particular to a method for simultaneously separating flavonoids and chlorogenic acid compounds from the crude extract of hawthorn leaves. Background technique:

[0002] Hawthorn leaf is a commonly used traditional Chinese medicine. It is a plant of Rosaceae Shanlihong ( Crataegus pinnatifida Bge .Var. major N. E. Br.) or hawthorn ( Crataegus pinnatifida Bge . ) dry leaves, which belong to the liver meridian, have the effects of promoting blood circulation, removing blood stasis, regulating qi and dredging channels, etc., and are mainly used for the clinical treatment of qi stagnation and blood stasis, chest pain and heartache, chest tightness and shortness of breath, palpitation and forgetfulness, dizziness, tinnitus, hyperlipidemia, etc. my country's Northeast, North China, Yunnan, Xinjiang and other places are all important hawthorn producing ar...

Examples

Embodiment 1

[0018] Example 1, 60g of hawthorn leaf crude extract, add 500mL distilled water for ultrasonic dissolution, filter out the insoluble matter, and the filtrate flows through the HPD-400 macroporous resin column at a flow rate of 3BV / h; after the adsorption is completed, the HPD-400 macroporous resin column First fully eluted with 5BV of distilled water, collected the eluate of the first stage, concentrated and freeze-dried, and obtained 5.49g of chlorogenic acid compounds with a purity of 70.3%; HPD-400 macroporous resin column was then washed with 5BV of 50% ethanol The aqueous solution is fully eluted, the second stage eluent is collected, and after the solvent is recovered by distillation under reduced pressure, 19.32g of total flavonoids from hawthorn leaves with a purity of 59.7% are obtained; the total flavonoids from hawthorn leaves are dissolved in 50mL of methanol, and refined using preparative chromatography. 18 Chromatography column (50´250 mm, 10 μm), 35 / 65 (V / V) 0.1%...

Embodiment 2

[0019] Example 2, 300g of hawthorn leaf crude extract, add 2500mL distilled water for ultrasonic dissolution, filter out the insoluble matter, and the filtrate flows through the HPD-300 macroporous resin column at a flow rate of 2BV / h; after the adsorption is completed, the HPD-300 macroporous resin column First fully eluted with 8BV of distilled water, collected the eluate of the first stage, concentrated and freeze-dried to obtain 25.4g of chlorogenic acid compounds with a purity of 67.1%; The aqueous solution was fully eluted, and the second eluent was collected. After the solvent was recovered by distillation under reduced pressure, 96.87g of total flavonoids from hawthorn leaves with a purity of 58.1% were obtained; 18 Chromatographic column (50´250 mm, 10 μm), 35 / 65 (V / V) 0.1% acetic acid aqueous solution / formonitrile}, collected monomer eluents and distilled under reduced pressure to obtain 1.37 g of 96.0% purity Vitexin glucoside and 6.39 g of vitexin rhamnoside with a...

Embodiment 3

[0020] Example 3, 600g of hawthorn leaf crude extract, add 5000mL distilled water for ultrasonic dissolution, filter out the insoluble matter, and the filtrate flows through the HPD-750 macroporous resin column at a flow rate of 2BV / h; after the adsorption is completed, the HPD-750 macroporous resin column First fully eluted with 10BV of distilled water, collected the eluate of the first stage, concentrated and freeze-dried, and obtained 51.13g of chlorogenic acid compounds with a purity of 67.2%; The aqueous solution is fully eluted, the second stage eluent is collected, and after the solvent is recovered by distillation under reduced pressure, 196.53g of total flavonoids from hawthorn leaves with a purity of 58.0% are obtained; the total flavonoids from hawthorn leaves are dissolved in 500mL of methanol and refined using preparative chromatography. 18 Chromatographic column (50´250 mm, 10 μm), 35 / 65 (V / V) 0.1% formic acid / methanol}, respectively collected monomer eluents and ...

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