Method for simultaneously preparing chemical reference substances of parishin, parishin B and parishin C

A reference substance and chemical technology, applied in the field of preparing parishin, parishin B, parishin C chemical reference substances at the same time, can solve the problem of high preparation cost, and achieve the effects of low price, high yield and easy scale.

Inactive Publication Date: 2011-05-25
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

N. Li et al. reported that the 80% ethanol extract of Gastrodia elata was extracted, sephadex LH-20 column, and reversed-phase high-performance liquid phase preparation to obtain parishin (Journa

Method used

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  • Method for simultaneously preparing chemical reference substances of parishin, parishin B and parishin C
  • Method for simultaneously preparing chemical reference substances of parishin, parishin B and parishin C
  • Method for simultaneously preparing chemical reference substances of parishin, parishin B and parishin C

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] 1. Coarse separation by resin column: 10 g of commercially available Gastrodia elata water extract is dissolved in 20% ethanol solution (the mass ratio of Gastrodia elata extract to water is 1: 4), filtered through four layers of gauze, and the clear liquid is separated by HPD-100 resin column, wherein The sample:resin ratio is 1:6 (g:ml), eluted with 3 times column volume of water, 3 times column volume of 10% ethanol solution, and 5 times column volume of 20% ethanol solution, and collected 20% ethanol solution Dematerialized, concentrated and dried to obtain 350 mg of yellow powder;

[0034] 2. Reverse-phase HPLC preparative chromatographic purification: the yellow powder is dissolved in aqueous solution, the sample concentration is 50mg / ml, and filtered through a 0.45μm microporous membrane; Separation, preparation of chromatographic column packing material is 6 μ m C18 (Novapak); injection volume is 1ml, the mobile phase that adopts is methanol and the aqueous solu...

Embodiment 2

[0036]1. Coarse separation by resin column: Gastrodia elata medicinal material 1230g, reflux extraction with 5 times the amount of 70% ethanol, 2 hours each time, 3 times. The three extracts were combined, concentrated under reduced pressure to a volume of about 3L, filtered through four layers of gauze, and the clear liquid was separated on a Diaion column. 10% ethanol solution of twice the column volume and 25% ethanol solution of 4 times the column volume were eluted, and the 25% ethanol eluate was collected, concentrated and dried to obtain 8.61 g of yellow powder;

[0037] 2. Reverse-phase high-performance liquid phase preparative chromatographic purification: the yellow powder is dissolved in aqueous solution, the sample concentration is 200 mg / ml, and filtered through a 0.45 μm microporous membrane; the filtrate uses a high-performance liquid phase preparative chromatographic column with a column length of 20 cm and a diameter of 7.5 cm Separation is carried out, and th...

Embodiment 3

[0039] 1. Coarse separation with resin column: Gastrodia elata medicinal material 2000g, extracted with 8 times the amount of water, extracted 3 times for 2 hours, 1.5 hours and 1 hour respectively. Combine three extracts, concentrate under reduced pressure to a volume of about 5 L, filter through four layers of gauze, and separate the supernatant on an AB-8 column. , 5 times column volume of 10% ethanol solution, 3 times column volume of 30% ethanol solution for elution, collect 30% ethanol eluate, concentrate and dry to obtain 20g of yellow powder;

[0040] 2. Reversed-phase high-performance liquid chromatography preparation and purification: the yellow powder was dissolved in 25% methanol solution, the sample concentration was 500 mg / ml, and filtered through a 0.45 μm microporous membrane; the filtrate was prepared by high-performance liquid phase with a column length of 30 cm and a diameter of 10 cm The chromatographic column is separated, and the filling material of the p...

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Abstract

The invention relates to a new process for simultaneously preparing chemical reference substances of parishin, parishin B and parishin C. The method provided by the invention comprises the following steps: extracting rhizoma gastrodiae crude drugs to obtain a crude extract or directly using rhizoma gastrodiae extract as a raw material, and efficiently purifying the rhizoma gastrodiae extract by resin column separation and reversed-phase high-efficiency liquid phase preparative chromatography, thereby obtaining the three chemical reference substances of parishin, parishin B and parishin C, wherein the purity of each chemical reference substance is higher than 98%. The invention has the advantages of simple procedure, high purity and favorable color, and can be favor of large-scale production.

Description

technical field [0001] The invention relates to a new preparation process for simultaneously preparing parishin, parishin B and parishin C chemical reference substances. It mainly includes two-step high-efficiency purification of resin column separation and reversed-phase high-performance liquid chromatography, and three reference substances can be obtained at the same time by collecting fractions reasonably. Its structural formula is as follows: [0002] [0003] Parishin: R 1 = R 2 = R 3 [0004] Parishin B:R 1 = R 2 = R, R 3 =H [0005] Parishin C:R 1 = R 3 = R, R 2 =H Background technique [0006] Gastrodia elata (Gastrodia elata Bl.) is one of the 34 kinds of precious medicinal materials announced by my country. It is mainly used for headache, dizziness, numbness of limbs, epilepsy and convulsions. Gastrodin is the active ingredient of Gastrodia elata, and it is also the content determination component of Gastrodia elata medicinal materials in the 2005 e...

Claims

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Application Information

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IPC IPC(8): C07H15/203C07H1/08
Inventor 肖红斌王莉彭杰
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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