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Method and equipment for treating opium poppy

A processing method and extract technology are applied in the field of separating and purifying monomeric drugs morphine, thebaine, and codeine, and can solve the problems of being unsuitable for large-scale industrial production, low content of crude morphine, unable to recover, etc. The effect of automatic control of separation and purification, shortening the batch production cycle and reducing the input of production personnel

Active Publication Date: 2017-10-31
李显林
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] This method uses the traditional resin adsorption method. Due to the poor adsorption selectivity of the resin method, only the morphine component with the highest content in the poppy extract can be obtained, and other effective components such as codeine and thebaine with high medicinal value It cannot be recovered, and the content of the obtained crude morphine is low, generally only reaching about 80%, which cannot reach the medicinal standard, and complex purification treatment is still required in the later stage, resulting in low yields of these active alkaloids
At the same time, resin adsorption has the disadvantages of small adsorption amount and long adsorption time, which lead to a long production cycle of this method, large space occupation of required equipment, and high production cost.
In addition to the above problems, the resin method will generate a large amount of industrial wastewater during the production process. These wastewater need to be treated professionally, which virtually increases the cost of production and is not suitable for large-scale industrial production.

Method used

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  • Method and equipment for treating opium poppy
  • Method and equipment for treating opium poppy
  • Method and equipment for treating opium poppy

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Add a polar solvent to the poppy extract for extraction, add a filter aid to filter to obtain the extract; the extract is separated by a chromatographic column, the filler is spherical silica gel bonded with a stationary phase, and the mobile phase is alcohol-inorganic with increasing alcohol concentration. Acid mixture, three fractions obtained by using three mobile phases of different polarities. Concentrate the fractions separately, crystallize with an alcoholic solvent, and filter with suction to obtain solids of morphine, codeine and thebaine.

[0041] Morphine solids: MS (eg Figure 4 ): m / z 285.13; IR (cm-1) (such as Figure 5):3347.82,3208.97,2938.98,2823.28,2395.16,1814.69,1652.70,1633.41,1604.48,1473.35,1446.35,1369.21,1307.50,1247.72,1197.58,1118.51,977.73,943.02,802.24,759.82,653.75,522.61。

[0042] Codeine solid: MS (eg Image 6 ): m / z 299.15; IR (cm-1) (such as Figure 7 ):3600.45,3467.38,3102.90,2898.49,1830.11,1652.70,1633.41,1608.34,1500.35,1452.14,...

Embodiment 2

[0045] 1. Extraction process steps

[0046] Add 15L of 5% ethanol water to 5.0Kg poppy extract (the morphine content is 0.71Kg as measured by the external standard method), extract at room temperature for 30min, add 0.5kg of diatomaceous earth and stir for one minute to complete the extraction; after extraction, directly Transfer the extract to a filter and collect the filtrate. The filtrate was concentrated under reduced pressure to about 20 L. The resulting concentrated solution was filtered through a pre-column at a flow rate of 30 L / min, and the filtrate was collected. The obtained filter cake layer is recovered uniformly and then incinerated.

[0047] 2. Morphine separation process steps

[0048] (1) Preparation equipment and filler parameters:

[0049] Preparative column specification: 300mm*1200mm (effective packing column height is about 300mm to 400mm)

[0050] Packing type: 200-300 mesh spherical silica gel, C18 packing

[0051] Filling capacity: 15Kg

[0052]...

Embodiment 3

[0062] 1. Extraction process steps

[0063] Add 5% ethanol water 30L in 9.0Kg poppy extract (recording morphine-containing amount with external standard method is 1.284Kg), after leaching at room temperature for 20min, add graphite powder 1.8kg and stir for one minute, complete extraction; After extraction, directly Transfer the extract to a filter for filtration, collect the filtrate, and concentrate the filtrate to about 20L under reduced pressure. The resulting filtrate was filtered through a pre-column at a flow rate of 20 L / min, and the filtrate was collected. The obtained filter cake layer is recovered uniformly and then incinerated.

[0064] 2. Morphine separation process steps

[0065] (1) Preparation equipment and filler parameters:

[0066] Preparative column specification: 300mm*1200mm (effective packing column height is about 700mm to 800mm)

[0067] Packing type: 200-300 mesh spherical silica gel, C8 packing

[0068] Filling capacity: 30Kg

[0069] Mobile ph...

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PUM

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Abstract

The invention discloses a method for treating opium poppy extract, which comprises the following steps: a, adding a polar solvent into the opium poppy extract, and reacting to obtain a first treating fluid; b, adding a filter aid into the first treating fluid, and filtering to obtain a first extract liquid; c, separating the first extract liquid through a chromatographic column which is filled with spherical silica gel of a bonded stationary phase and a mixture of alcohol and inorganic acid serving as a mobile phase; and d, eluting to obtain a fraction containing alkaloid. Compared with the prior art, the method has the advantages of separating morphine, codeine, thebaine and other monomer alkaloids, and the alkaloid monomer has high purity and large yield.

Description

technical field [0001] The invention relates to a method for separating and purifying monomer drugs morphine, codeine and thebaine from poppy extract by using industrial preparation chromatography and traditional crystallization method. Background technique [0002] Pain is a protective response of the body to noxious stimuli in the internal and external environment, which includes both real or potential tissue damage and mental damage. There are hundreds of different types of drugs used to treat pain, and their mechanisms vary. It has become a trend to search for highly effective, low-toxic, and non-dependent analgesics from natural medicines. All kinds of active monomer substances contained in poppy extract are the most widely used and most demanded natural alkaloid analgesic drugs in the world. [0003] Unripe poppy fruit contains a large amount of milky white liquid, which can form a brown or brown-black paste after drying. Poppy extract is a crude alkaloid obtained b...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D489/02
CPCC07D489/02
Inventor 李显林郭毅民王述东唐海蓉胡延雷
Owner 李显林
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