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Production of high-purity peiminine and fritimine

A technique of fritillin A and fritillin B, which is applied in the field of preparation of monomer alkaloids and achieves the effects of peak shape resolution, solvent saving and large separation amount

Inactive Publication Date: 2009-08-12
NAT ENG RES CENT FOR TRADITIONAL CHINESE MEDICINE +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0013] At present, HSCCC has not been used to separate the effective components in Fritillaria decoction pieces—Piimin A and Peimin B

Method used

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  • Production of high-purity peiminine and fritimine
  • Production of high-purity peiminine and fritimine
  • Production of high-purity peiminine and fritimine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Take 20g of Fritillaria powder (through a 60-mesh sieve), add 20ml of ammonia water to soak for 1 hour, add 100ml of chloroform-methanol (4:1) mixed solution, heat in a water bath at 80°C for 2 hours, filter, evaporate the filtrate to dryness, and use the residue for later use .

[0031] Select chloroform-ethanol-0.2M hydrochloric acid solution from the system to separate and prepare peiminin A and peiminin B on a semi-preparative high-speed countercurrent chromatograph. Put the solvent system in a separatory funnel at a volume ratio of 4:3:2, shake well and let stand to separate layers. After equilibrating for a certain period of time, separate the upper phase (stationary phase) and the lower phase (mobile phase). Set the experimental temperature as: 25°C. A TBE-300A high-speed countercurrent chromatograph is used, with a column volume of 119ml, a sample injection loop of 10ml, an AKTA purifier P-900 pump, an ELSD detector, and a HX-1050 constant temperature circulat...

Embodiment 2

[0034] Take 20g of Fritillaria powder (through a 60-mesh sieve), add 20ml of ammonia water to infiltrate for 1 hour, add 100ml of chloroform-methanol (4:1) mixed solution, heat in a water bath at 80°C for 2 hours, filter, evaporate the filtrate to dryness, and set aside the residue .

[0035] Select chloroform-ethanol-0.1mol / l hydrochloric acid solution from the system to separate and prepare peiminine A and peiminin B on a semi-preparative high-speed countercurrent chromatograph. Put the solvent system in a separatory funnel at a volume ratio of 2:1:2, shake well and let stand to separate layers. After equilibrating for a certain period of time, separate the upper phase (stationary phase) and the lower phase (mobile phase). Set the experimental temperature as: 25°C. A TBE-300A high-speed countercurrent chromatograph is used, with a column volume of 119ml, a sample injection loop of 10ml, an AKTA purifier P-900 pump, an ELSD detector, and a HX-1050 constant temperature circu...

Embodiment 3

[0038] Take 20g of Fritillaria powder (through a 60-mesh sieve), add 20ml of ammonia water to infiltrate for 1 hour, add 100ml of chloroform-methanol (4:1) mixed solution, heat in a water bath at 80°C for 2 hours, filter, evaporate the filtrate to dryness, and set aside the residue .

[0039] Select chloroform-ethanol-0.2mol / l phosphoric acid solution from the system to separate and prepare peiminine A and peiminin B on a semi-preparative high-speed countercurrent chromatograph. Put the solvent system in a separatory funnel according to the volume ratio of 6:4:2, shake well and let stand to separate layers. After equilibrating for a certain period of time, separate the upper phase (stationary phase) and the lower phase (mobile phase). Set the experimental temperature as: 25°C. A TBE-300A high-speed countercurrent chromatograph is used, with a column volume of 119ml, a sample injection loop of 10ml, an AKTA purifier P-900 pump, an ELSD detector, and a HX-1050 constant tempera...

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Abstract

The invention discloses a preparation method of high-purity peiminin A and peiminin B, which adopts high-speed countercurrent chromatographic technology, and comprises the following steps: preparing Fritillaria japonicus extract as a sample; configuring to form a stationary phase and a mobile phase Solvent system; when the stationary phase and flow are the same, the pump is pumped into the column; the main engine rotates, the sample is injected by the injection valve, the elution solvent is detected, the target component is received, and the product is collected. The solvent system used can be composed of chlorinated alkanes, aliphatic alcohols or aliphatic ketones, dilute acidic solutions. The method can obtain high-purity monomeric alkaloids: peimin A and peimin B from the crude extract of Fritillaria japonicus, and the purity is as high as 98% and 95% respectively. The method is simple and convenient to operate, low in cost, high in recovery rate and easy to popularize and use.

Description

technical field [0001] The invention relates to a preparation method of monomeric alkaloids, in particular to a preparation method of high-purity peiminin A and peiminin B. Background technique [0002] Fritillaria fritillaria is a perennial herb of the genus Fritillaria in the family Liliaceae. Its bulbs have the effects of clearing heat and resolving phlegm, relieving cough, resolving depression, and dispelling stagnation. Epidemic is a commonly used decoction piece in clinical prescriptions of traditional Chinese medicine. There are three types of decoction pieces: big shellfish, pearl shellfish, and Zhejiang shellfish slices. The active ingredients in Fritillaria japonicus are steroidal alkaloids and their glycosides. There are mainly peiminine (peiminine A, verticine, peimine), dehydropeiminine (peiminine B, verticinone, peiminine) and trace amounts of peiminine (peimisine), peimiphine (peimiphine), peimidine, peimitidine. In addition, it still contains the steroida...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07J71/00C07J69/00C07J75/00
Inventor 沈平孃张继全刘峻金艳
Owner NAT ENG RES CENT FOR TRADITIONAL CHINESE MEDICINE
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