Preparation method of secoxyloganin

A technology for oxidizing horse and schistosides, which is applied in chemical instruments and methods, preparation of sugar derivatives, organic chemistry, etc., can solve the problems of high cost, low sample load, high price, etc., and achieves short preparation cycle and good technology. The effect, the effect of the large amount of preparation

Active Publication Date: 2016-05-18
JIANGSU KANION PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there is a common problem in the above studies. The broken-oxyloganin is discovered in the process of chemical composition research. The amount of broken-oxyloganin obtained is very small, the reproducibility is poor, and it is difficult to scale up.
In addition, Sephadex LH-20 filler is used in most refining and purification processes. The filler has a small sample load, low flow rate, takes a long time, and is difficult to operate on a large scale. Moreover, the filler is expensive and expensive, and is not suitable for industrialization.

Method used

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  • Preparation method of secoxyloganin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] 1. A preparation method for deoxygenated loganin, which comprises the following steps:

[0031] (1) Get 5 kg of honeysuckle medicinal material, add 8 times the volume concentration of the medicinal material and extract 2 times with 70% ethanol under reflux, each time for 2 hours, filter, combine the filtrate, concentrate, put on the D101 macroporous resin column, first elute with water, and then Elute with a gradient of 20% ethanol, and collect the elution site of 20% ethanol;

[0032] (2) Industrial preparation chromatographic preparation and separation: the fraction of deoxygenated loganin was prepared by industrial preparation chromatography, and the chromatographic column was reversed-phase C 18 Chromatographic column (50×250mm), the flow rate is 20mL / min, the wavelength is 242nm, the mobile phase is methanol and water with a volume ratio of 25:75, the injection volume is 1.0g, and the elution curve is monitored at 242nm wavelength to guide product collection After...

Embodiment 2

[0036] 1. A method for rapidly preparing broken oxidized loganin from Flos Lonicerae, comprising the following steps:

[0037] (1) Get 10 kg of honeysuckle medicinal material, add 16 times of volume concentration of medicinal material and extract 3 times with 80% ethanol under reflux, each time for 2 hours, filter, combine filtrate, concentrate, put on D101 macroporous resin column, first elute with water, then Elute with a gradient of 20% ethanol, and collect the elution site of 20% ethanol;

[0038] (2) Industrial preparation chromatographic preparation and separation: the fraction of deoxygenated loganin was prepared by industrial preparation chromatography, and the chromatographic column was reversed-phase C 18 Chromatographic column (80×600mm), the flow rate is 60mL / min, the wavelength is 242nm, the mobile phase is methanol and water with a volume ratio of 25:75, the injection volume is 5.0g, and the elution curve is monitored at a wavelength of 242nm To guide product co...

Embodiment 3

[0041] 1. A method for rapidly preparing broken oxidized loganin from Flos Lonicerae, comprising the following steps:

[0042] (1) Get 20 kg of honeysuckle medicinal materials, add 8 times the volume concentration of medicinal materials and extract 3 times with 70% ethanol under reflux, each time for 2 hours, filter, combine the filtrates, concentrate, put on D101 macroporous resin column, first wash with water, and then Elute with 20% ethanol, collect the eluted part of 20% ethanol;

[0043] (2) Industrial preparation chromatographic separation: the deoxidized loganin part is prepared by industrial preparation chromatography, the chromatographic column is a reverse phase C18 chromatographic column (150×600mm), the flow rate is 1L / min, the wavelength is 242nm, and the mobile phase is The volume ratio of methanol and water is 25:75, the injection volume is 20g, and the outflow curve is monitored at a wavelength of 242nm to guide product collection. The collected solution is con...

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Abstract

The invention discloses a preparation method of secoxyloganin. The preparation method includes the steps of firstly, taking a honeysuckle medicinal material, adding ethyl alcohol for reflux extraction, conducting filtration, combining filtrate, conducting concentration, putting the concentrate on a macroporous resin column to be eluted with water and then eluted with ethyl alcohol with the concentration of 20-95% in a gradient mode, and collecting eluted parts containing secoxyloganin; secondly, conducting separation through industrial preparative chromatography, wherein preparation is conducted through the inverse industrial preparative chromatography, methyl alcohol and water are used as the flowing phase, an elution curve is monitored under the wavelength of 242 nm so that product collection can be guided, and secoxyloganin is obtained by concentrating collected liquid. According to the preparation method, the optimal extraction method and the optimal macroporous resin purification method are screened out through system experiments, and high-purity secoxyloganin is prepared through optimal industrial preparative chromatography purification. The method is industrially reasonable, and is particularly large in preparation amount, high in efficiency and high in preparation yield, and obtained secoxyloganin is high in purity and suitable for large-scale preparation.

Description

technical field [0001] The present invention relates to a preparation method of deoxygenated loganin, in particular to a method for rapidly preparing deoxyloganin from honeysuckle. Background technique [0002] Deoxygenated loganin is a product extracted and refined from the dried flower buds of Lonicera japonica Thunb., that is, Flos Lonicerae japonicae. Broken-oxygenated loganin is an iridoid compound, which is an active ingredient of honeysuckle. Modern pharmacological research has found that iridoids have pharmacological effects such as nervous system protection, anti-inflammatory, antibacterial, anti-viral, anti-tumor, liver protection and gallbladder, hypoglycemic, antispasmodic and analgesic, and can also be used to treat cardiovascular diseases. Raw materials for diseases, diabetes and its complications. It has been reported in the literature that under the dose of 20mg / kg, deoxidized loganin has no effect on CCl 4 The mice with liver injury show significant hepat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H17/04C07H1/08
CPCC07H1/08C07H17/04
Inventor 萧伟王振中宋亚玲倪付勇赵祎武王雪晶谢雪罗鑫温建辉张宏达黄文哲
Owner JIANGSU KANION PHARMA CO LTD
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