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Liquid chromatography-circular dichroism (LC-CD) identification method of Arnebia Euchroma and Radix Lithospermi

A technique of LC-CD and circular dichroism, which is applied in the field of identification of soft comfrey and hard comfrey, can solve confusion, and it is difficult to identify the components of soft comfrey and hard comfrey naphthoquinones, which affect the efficacy and safety of drugs and other issues to achieve the effect of accurate identification

Active Publication Date: 2013-06-26
SUZHOU LEINA PHARMA RES DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Soft comfrey and hard comfrey are difficult to distinguish in terms of appearance and the proportion of naphthoquinones contained in them, and it is generally difficult to accurately distinguish soft comfrey and hard comfrey
Soft comfrey and hard comfrey have different functions and functions. If they are not accurately distinguished, confusion will arise in the process of market circulation and clinical application, which can seriously affect the efficacy and safety of drugs. Therefore, it is necessary to find a method to accurately distinguish and identify soft comfrey. Grass and hard comfrey medicinal materials, especially soft comfrey and hard comfrey extracts (including compound Chinese medicines containing comfrey, naphthoquinone component monomers), will have important theoretical significance and practical application value

Method used

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  • Liquid chromatography-circular dichroism (LC-CD) identification method of Arnebia Euchroma and Radix Lithospermi
  • Liquid chromatography-circular dichroism (LC-CD) identification method of Arnebia Euchroma and Radix Lithospermi
  • Liquid chromatography-circular dichroism (LC-CD) identification method of Arnebia Euchroma and Radix Lithospermi

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0063] Example 1: Identification of soft comfrey and hard comfrey

[0064] Chromatographic conditions: chromatographic column is Scienhome Kromasil C18 (4.6mm×200mm, 5μm) and pre-column, mobile phase is acetonitrile (A)-0.3% phosphoric acid water (B), gradient elution process (A gradient) 0-10 minutes 70 %, 70%-75% in 10-30 minutes, 75%-95% in 30-31 minutes, 95% in 31-36 minutes, 95%-70% in 36-37 minutes, 70% in 37-50 minutes. The detection wavelength is 274nm, the column temperature is 30°C, the flow rate is 1.0mL / min, and the number of theoretical plates is not less than 3000 based on naphthoquinone. The regression equation, linear range, minimum detection limit and limit of quantification results of its ultraviolet spectrum are shown in Table 1.

[0065] Table 1 Results of regression equation, linear range, minimum detection limit and limit of quantification of nine naphthoquinone compounds

[0066] Table 1 Regression equations.correlation coefficients.linear range.LOD an...

Embodiment 2

[0072] Embodiment 2: Preparation of naphthoquinone derivatives in soft comfrey

[0073]Soft comfrey coarse powder 1.8kg, 95% ethanol cold soaking extraction, 10 times the amount of extraction three times, 24 hours each time, combined extracts, using a rotary evaporator to recover the solvent to obtain soft comfrey extract 105g.

[0074] Take 95g of soft comfrey extract and 400g of silica gel, and carry out column chromatography gradient elution with petroleum ether: ethyl acetate, each 700mL fraction is identified by silica gel thin layer chromatography, and the same fractions are combined.

[0075] The combined fractions 12-13 (2.7g) were eluted with petroleum ether, and subjected to silica gel column chromatography, petroleum ether: ethyl acetate gradient elution (100:1), to obtain compounds 7 (1g) and 8 (1g); 17 (0.97g) was subjected to silica gel column chromatography, petroleum ether: ethyl acetate gradient elution (100:0.5), to obtain compound 4 (15mg), 6 (300mg); Fracti...

Embodiment 3

[0081] Embodiment 3: Preparation of naphthoquinone derivatives in Sclerophylla

[0082] Comfrey coarse powder 1.0kg, 95% ethanol cold soaking extraction, 10 times the amount of extraction three times, 24 hours each time, combined extracts, using a rotary evaporator to recover the solvent to obtain 18 g of comfrey extract, which was dispersed with 1L of water The suspension was extracted three times with an equal volume of petroleum ether for 12 hours each time, and part of the petroleum ether extract was recovered, and the recovered solvent was concentrated to obtain 5.7 g of petroleum ether partial extract.

[0083] Take 5 g of the petroleum ether extract of Sclerophyllum, 100 g of silica gel for column chromatography, carry out column chromatography gradient elution with petroleum ether: ethyl acetate, each 300 mL fraction is identified by silica gel thin-layer chromatography, and the same fractions are combined.

[0084] Petroleum ether: ethyl acetate (100:0.5) was eluted, ...

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Abstract

The invention relates to an identification technology of Arnebia Euchroma and Radix Lithospermi, and concretely relates to a method for accurately identifying medicinal materials and extracts (comprising Radix Arnrbiae-containing compound traditional Chinese medicines, and naphthoquinone component monomers) of Arnebia Euchroma and Radix Lithospermi by establishing LC-CD through utilizing the inverse relationship of canini enantiomers contained in Arnebia Euchroma and Radix Lithospermi respectively in the LC-CD. The medicinal materials and extracts (comprising Radix Arnrbiae-containing compound traditional Chinese medicines, and naphthoquinone component monomers) of Arnebia Euchroma and Radix Lithospermi can be accurately identified and distinguished through the method.

Description

technical field [0001] The present invention relates to the identification technology of Zicao soft and hard comfrey, in particular to liquid phase-circular dichroism (LC-CD) to accurately identify medicinal materials and extracts of Zicao soft and hard comfrey (including compound Chinese medicines containing comfrey) , naphthoquinone component monomer) method. Background technique [0002] Comfrey has a long history of medicinal use in my country. It tastes sweet and salty, and is cold in nature. Drenching and bloody dysentery, hot knot constipation, burns, eczema, erysipelas, carbuncle and other diseases. [0003] Radix Arnrbiae (Radix Arnrbiae, Radix Lithospermi) is the dried root of Arnebiaeuchroma (Royle) Johnst., Lithospermum erythrorhizon Sieb.et Zucc. or Arnebiaguttata Bunge of the Boraginaceae plant [1] . Among them, Xinjiang comfrey is also known as soft comfrey, comfrey or Inner Mongolia comfrey is also called hard comfrey, and soft comfrey and hard comfrey are ...

Claims

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Application Information

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IPC IPC(8): G01N30/88
Inventor 王金辉刘珂李国玉冯文文郎跃武
Owner SUZHOU LEINA PHARMA RES DEV
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