Method for preparing high-purity rutin via two-dimensional liquid chromatography-mass spectrometry combined technology

A two-dimensional liquid chromatography and two-dimensional preparation technology, which is applied in the field of high-purity rutin preparation by two-dimensional liquid chromatography-mass spectrometry, can solve the problems of insufficient medicinal material resources, low utilization rate of medicinal materials, and doping of hydrolyzed products. Achieve the effects of wide sources of medicinal materials, high purity of rutin, and long application time

Active Publication Date: 2013-05-29
北京华润高科天然药物有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] In view of the above-mentioned defects, and in view of the problems that the current extraction and preparation of rutin will have hydrolyzate doping, cumbersome operation, low utilization rate of medicinal materials, and insufficient medicinal material resources, the present invention provides a method using ginkgo biloba extract as raw material, using two-dimensional Method for preparing rutin by liquid chromatography-mass spectrometry

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] Weigh 10 g of Ginkgo biloba extract, dissolve it in 50 mL of 50% methanol-water solution to obtain a Ginkgo biloba extract solution with a concentration of 200 mg / mL, pass it through a 0.45 μm microporous membrane, and prepare it by one-dimensional liquid chromatography. The one-dimensional liquid chromatography adopts XUnion C18, the mobile phase adopts acetonitrile (containing 0.1% formic acid) as the organic phase, water (containing 0.1% formic acid) as the aqueous phase, and the gradient elution method: the concentration of the organic phase increases from 10% to 25%. DAD ultraviolet detector is used to select the absorption wavelength at 360nm, the preparation temperature is room temperature, the injection volume is 500μL / needle, the mobile phase flow rate is 90mL / min, the fractions collected for 12-14 minutes are concentrated to dryness by rotary evaporation, which is one-dimensional preparation Crude rutin. Dissolve crude rutin in 40% methanol-water solution wit...

Embodiment 2

[0049] Weigh 10 g of Ginkgo biloba extract, dissolve it in 100 mL of 25% methanol-water solution to obtain a Ginkgo biloba extract solution with a concentration of 10 mg / mL, pass it through a 0.45 μm microporous membrane, and perform one-dimensional liquid chromatography preparation. The one-dimensional liquid chromatography adopts XTerra, the mobile phase adopts methanol as the organic phase, water as the aqueous phase, the organic phase concentration is 65% isocratic, the DAD ultraviolet detector is used to select the absorption wavelength at 360nm, the preparation temperature is 40°C, and the injection volume is 200 μL / needle, the flow rate of the mobile phase is 60mL / min, the fractions collected for 5-7 minutes are concentrated to dryness by rotary evaporation, and the crude rutin is prepared as one-dimensional. Dissolve crude rutin in 50% methanol-water solution with a concentration of 10 mg / mL, filter through a microporous membrane, and prepare for two-dimensional liquid ...

Embodiment 3

[0051] Weigh 10 g of Ginkgo biloba extract, dissolve it in 20 mL of 75% methanol-water solution to obtain a Ginkgo biloba extract solution with a concentration of 500 mg / mL, pass it through a 0.45 μm microporous membrane, and perform one-dimensional liquid chromatography preparation. One-dimensional liquid chromatography adopts Click OEG, the mobile phase uses methanol (containing 0.1% formic acid) as the organic phase, water (containing 0.1% formic acid) as the aqueous phase, and adopts 5% organic equivalence method for elution. The DAD ultraviolet detector is used to select the absorption wavelength at 360nm, the preparation temperature is 30°C, the injection volume is 3000μL / needle, the flow rate of the mobile phase is 120mL / min, and the fractions collected for 25-30 minutes are concentrated to dryness by rotary evaporation, which is one-dimensional Preparation of crude rutin. Dissolve crude rutin in 60% methanol-water solution with a concentration of 80 mg / mL, filter throu...

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Abstract

The invention relates to the technical field of medicines, and discloses a method for preparing high-purity rutin via a two-dimensional liquid chromatography-mass spectrometry combined technology. The method comprises the following steps of: adopting the two-dimensional liquid chromatography-mass spectrometry combined technology, taking methanol-water or acetonitrile-water as a mobile phase, using a reversed chromatographic column as the first dimension for preparing a chromatographic column, performing component cutting on a ginkgo leaf extract, and collecting a target component, namely, a rutin crude product; and using the reversed chromatographic column as the second dimension for preparing a chromatographic column, performing component cutting on the rutin crude product under the guide of a mass spectrometry selected ion peak, collecting, rotationally evaporating and concentrating, and then obtaining the high-purity rutin having a purity which can achieve more than 80%. In the method disclosed by the invention, heating is not needed, so that the doping of a hydrolysate is avoided; the preparation is simple in process, high in repeatability, and good in operability; simultaneously, ginkgo leaves are abundant in resource and easy to obtain, thus reducing the cost; and the method is suitable for large-scale production.

Description

technical field [0001] The invention belongs to the technical field of medicine, and in particular relates to a method for preparing high-purity rutin by two-dimensional liquid chromatography-mass spectrometry. Background technique [0002] Rutin, also known as rutin, widely exists in the plant kingdom. More than 50 kinds of plants containing rutin have been found. Rutin belongs to flavonoids, which can reduce capillary permeability and fragility, promote cell proliferation and prevent blood cell aggregation, and play a pivotal role in the treatment of cardiovascular and cerebrovascular diseases. At the same time, rutin also has anti-inflammatory, anti-allergic, diuretic, antispasmodic, antitussive, and hypolipidemic effects. Clinically, rutin is mainly used for adjuvant treatment of hypertension and prevention and treatment of other hemorrhagic diseases caused by rutin deficiency, such as prevention and treatment of cerebrovascular hemorrhage, hypertension, retinal hemorr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): A61K36/16G01N30/06G01N30/12A61P9/10A61P9/12A61P9/14A61P7/04A61P13/12A61P11/00A61P3/10A61P3/06A61K127/00
Inventor 丰加涛付冬梅王海涛冯志琼
Owner 北京华润高科天然药物有限公司
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