A kind of preparation method and product of carboxy atractylodes tripotassium salt reference substance

A technology of glycoside tripotassium salt and reference substances, which is applied in the field of preparation of chemical reference substances, can solve problems such as perishability and difficulty in separating monomers, and achieve the effects of short time consumption, high academic value, and low solvent consumption

Active Publication Date: 2020-12-01
上海诗丹德标准技术服务有限公司
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AI Technical Summary

Problems solved by technology

[0005] At present, domestic literature reports on the separation and purification of tripotassium carboxyaxatriside reference substance are few. In addition, tripotassium carboxyaxatriside has been listed as a standard in the 2015 Pharmacopoeia, and the demand for it is increasing. However, domestic At present, the market is basically in a blank state. The main reason is that the tripotassium salt of carboxy atractylodes is unstable and easy to deteriorate. It is very difficult to separate the monomer from medicinal materials. Therefore, how to separate and purify carboxy atractylodes from cocklebur Tripotassium salt reference substance is one of the current research hotspots and difficulties for researchers in this field

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  • A kind of preparation method and product of carboxy atractylodes tripotassium salt reference substance
  • A kind of preparation method and product of carboxy atractylodes tripotassium salt reference substance

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preparation example Construction

[0026] A kind of preparation method of carboxy atractylodes tripotassium salt reference substance according to the first aspect, comprising the following steps:

[0027] S1: First, mix Xanthium medicinal material with water, extract by cold immersion at room temperature, concentrate the liquid part after solid-liquid separation, thereby obtaining the first concentrated liquid; then, dilute the volume to 3 to 4 times the volume of the first concentrated liquid methanol was added to the first concentrated solution, precipitated, filtered, the filtrate was collected, and then concentrated to obtain the second concentrated solution; then, a saturated KCl solution whose volume was 1 to 2 times the volume of the second concentrated solution was added to the second concentrated solution In the second concentrated solution, carry out salting out, suction filtration, and collect solid; finally, use MCI column to separate the solid after salting out, wherein adopt methanol-water as eluen...

Embodiment 1

[0040] Prepare carboxy atractylodes tripotassium salt reference substance according to the following steps:

[0041] (1) Raw material extraction: crush 10 kg of Fructus cocklebur medicinal material, add 80 L of water, extract by cold soaking at room temperature twice for 2 days each time, filter with suction, combine the filtrates, concentrate to a small volume, and obtain 4000 ml of the first concentrated solution; (2) Methanol precipitation and impurity removal: add 12L methanol to the first concentrated solution, precipitate, filter, collect the filtrate, and then concentrate to 1600ml to obtain the second concentrated solution; (3) salting out: 1600ml saturated The KCl solution is added to the second concentrated solution, salted out, suction filtered, and the solid is collected; (4) MCI purification: the solid after the salted out is dissolved with 200ml of pure water and then put on the MCI column (pure water wet packing, packing It is a polystyrene synthetic resin, the ...

Embodiment 2

[0043] Prepare carboxy atractylodes tripotassium salt reference substance according to the following steps:

[0044] (1) Raw material extraction: crush 50kg of cocklebur medicinal material, add 300L of water, extract by cold soaking at room temperature twice for 2 days each time, filter with suction, combine the filtrates, concentrate to a small volume, and obtain 20L of the first concentrated solution; (2) Methanol precipitation and impurity removal: add 60L methanol to the first concentrated solution, precipitate, filter, collect the filtrate, and then concentrate to 8000ml to obtain the second concentrated solution; (3) salting out: 8000ml saturated The KCl solution is added to the second concentrated solution, salted out, suction filtered, and the solid is collected; (4) MCI purification: the solid after the salted out is dissolved with 1000ml of pure water and then put on the MCI column (pure water wet column packing, packing It is a polystyrene synthetic resin, the parti...

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Abstract

The invention provides a carboxyatractyloside tripotassium salt reference substance and a preparation method thereof. The preparation method mainly includes: preparing carboxyatractyloside tripotassium salt aqueous extract; using purified water to dissolve the carboxyatractyloside tripotassium salt aqueous extract, allowing the dissolved carboxyatractyloside tripotassium salt aqueous extract to pass a gel column, using gel column eluent to perform elution, and separating to obtain crude carboxyatractyloside tripotassium salt; using purified water to dissolve the crude carboxyatractyloside tripotassium salt, allowing the dissolved crude carboxyatractyloside tripotassium salt to pass a high-pressure column, using high-pressure column eluent to perform elution, separating to obtain target components, and combining; performing freeze drying on the combined target components to obtain the carboxyatractyloside tripotassium salt reference substance. The preparation method is simple to operate, high in separation efficiency, stable in process, low in cost, high in product purity and suitable for industrial production.

Description

technical field [0001] The invention relates to the technical field of preparation of chemical reference substances, in particular to a preparation method of a carboxy atractylodes tripotassium salt reference substance, and also to a carboxy atractylodes tripotassium salt reference substance prepared by the preparation method. Background technique [0002] Xanthium is the dry and mature fruit with involucre of Xanthium sibiricum Patr. Acrid in the mouth, bitter, warm, poisonous, return lung meridian. Fructus Xanthii has the effects of dispersing wind and cold, dredging the nose, and dispelling rheumatism. It is mainly used for the treatment of wind-cold headache, nasal sinusitis runny nose, nasal sinusitis, rubella itching, damp arthralgia contracture and other diseases. . Fructus Xanthii is a poisonous traditional Chinese medicine that has curative effects in traditional records. There are clinical reports of poisoning and even death due to long-term, excessive, repeated ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07H15/256C07H1/08
CPCC07H1/08C07H15/256
Inventor 舒亚平辛振强冯宝军何晓义张田勇谢天培
Owner 上海诗丹德标准技术服务有限公司
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