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Separation and purification method for lappaconitine

A technology of separation and purification, high acetaminophen, applied in organic chemistry and other directions, can solve the problems of large residual solvent, long production cycle, large chloroform, etc., and achieve the effects of high yield, short production cycle and reduced dosage

Inactive Publication Date: 2011-02-09
NANJING ZELANG MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The process has a long production cycle and uses a large amount of chloroform, which is not easy to recycle and has a large amount of solvent residue

Method used

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  • Separation and purification method for lappaconitine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Take by weighing 1kg crushed particle size and be the high aconitum root tuber powder of 40-60 purpose, be dissolved in 80% ethanol (50 ℃) by solid-liquid ratio 1: 10 (W / V), extract 40 minutes in the ultrasonic extractor, power is 75W, extract 3 times, filter, remove the dregs, combine the extracts, dissolve the extracts with 1% hydrochloric acid after concentration, pass through a macroporous cation exchange resin (diameter-to-height ratio 1:6) at 5BV / h, and wash with water until washed out The color of the solution becomes lighter, and then eluted with 5% hydrochloric acid solution, the elution rate is 2BV / h, and the eluate is collected until the alkaloid reaction is negative (the effluent is dropped on a thin-layer plate or a filter paper sheet, sprayed with modified iodide Bismuth potassium reagent has no reddish-brown spots). Neutralize with sodium hydroxide to a pH of 7, dialyze to remove salt, concentrate the filtrate into a concentrated solution with a relative ...

Embodiment 2

[0030] Take by weighing 1kg crushed particle size and be the high aconitum root tuber powder of 40-60 purpose, be dissolved in 90% ethanol (40 ℃) by solid-liquid ratio 1: 14 (W / V), extract 60 minutes in the ultrasonic extractor, power is 50W, extract 4 times, filter, remove the dregs, combine the extract, dissolve the extract with 1% hydrochloric acid after concentration, pass through the macroporous cation exchange resin (diameter-to-height ratio 1:8) at 5BV / h, and wash with water until it is washed out The color of the solution becomes lighter, and then eluted with 1.0% hydrochloric acid solution, the elution rate is 2BV / h, and the eluate is collected until the alkaloid reaction is negative (the effluent is dropped on a thin-layer plate or filter paper, sprayed with modified iodide Bismuth potassium reagent has no reddish-brown spots). Neutralize with sodium hydroxide to pH 7, dialyze to remove salt, concentrate the filtrate into a concentrated solution with a relative densi...

Embodiment 3

[0032] Take by weighing 2kg of pulverized particle size and be the high aconitum root tuber powder of 40-60 purpose, be dissolved in 75% ethanol (45 ℃) by solid-liquid ratio 1: 16 (W / V), extract 90 minutes in the ultrasonic extractor, power is 150W, extract 3 times, filter, remove medicinal residues, combine extracts, concentrate and dissolve extracts with 1% hydrochloric acid, pass through macroporous cation exchange resin (diameter-height ratio 1:10) at 5BV / h, wash with water until washed out The color of the solution becomes lighter, and then eluted with 2.0% hydrochloric acid solution, the elution rate is 2BV / h, and the eluate is collected until the alkaloid reaction is negative (the effluent is dropped on a thin-layer plate or filter paper, sprayed with modified iodide Bismuth potassium reagent has no reddish-brown spots). Use sodium hydroxide to neutralize the total pH to 7, dialyze to remove salt, concentrate the filtrate into a concentrated solution with a relative den...

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Abstract

The invention relates to a separation and purification method for lappaconitine, which is used for preparing high-purity lappaconitine by integrating a solvent extraction-ion resin column-alumina column-recrystallization method and comprises the following steps: ultrasonically extracting the lappaconitine by utilizing ethanol, dissolving the concentrated lappaconitine by utilizing 1% of hydrochloric acid, adding cation exchange resins in a countercurrent mode, carrying out acid elution, regulating the pH value to neutral and desalting, wherein a column chromatography adopts a short and thick column; a filler is alumina; a mobile phase is the ethanol; and a recrystallization solvent is acetone-ethanol (the ratio is 1 to 1). The separation and purification method has the advantages of obvious reduction of organic solvents, in particular to toxic solvents, low cost, high yield, short production period and easy industrialization.

Description

Technical field: [0001] The invention belongs to the field of purification of effective components of traditional Chinese medicines, and relates to a method for separation and purification of quinine. Background technique: [0002] Lappaconitine [0003] Molecular formula: C 32 h 44 N 2 o 8 ; [0004] Chemical Structure: [0005] [0006] Aconitum sinomontanum Nakai is the dry tuberous root of Aconitum sinomontanum Nakai in Ranunculaceae. Also known as keel seven, nine chains, linen seven, Tongtian bag. Gaowujiain is an alkaloid isolated from the root of Aconitum aconitum, which is used to treat moderate to severe pain. Preemptive analgesia of 0.15 mg / kg urine for gynecological laparoscopic surgery can produce better analgesic effect and reduce the dosage of opioids without affecting recovery from anesthesia. It can also be used for postoperative thyroid surgery patients. analgesia. Its hydrobromide is commonly used clinically. Urine hydrobromide has obvious an...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D221/22
Inventor 刘东锋郭琴杨成东
Owner NANJING ZELANG MEDICAL TECH
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