Method for preparing allantoin from nitraria core residue

A technology of Nitraria japonica and allantoin, applied in the direction of organic chemistry, etc., to achieve the effect of simple preparation method and high extraction rate

Inactive Publication Date: 2011-04-20
QINGHAI QINGMEI BIOLOGICAL RESOURCES R&D
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Its fruit is rich in vitamins, amino acids, polysaccharides and other nutritional active ingredients, especially amino acids, which are easily abs

Method used

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  • Method for preparing allantoin from nitraria core residue

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Embodiment 1

[0008] Embodiment 1: Get 10Kg Nitraria fruit stone residue, add 40% ethanol to extract, its solid-liquid weight ratio is 1: 5, extraction temperature is 80 ℃, extracts 3 times, extraction time 2h; In the ethanol recovery device, recover ethanol at a temperature of 80°C and normal pressure to obtain a paste-like concentrate; then add water to completely disperse the paste-like concentrate, and then add petroleum ether according to 3 times the volume of the paste-like concentrate. Extraction under pressure for 40min, extraction 3 times; after 75μm silica gel column chromatography, and eluting with 20% ethanol, the eluate was heated to 50°C to crystallize, centrifuged, and washed once with water, and the crystals were placed in a constant temperature drying oven Heated to 50°C and dried for 6 hours to obtain 62.8g of 96.5% allantoin.

Embodiment 2

[0009] Embodiment 2: get 10kg Nitraria thorn residue, add 50% ethanol to extract, its solid-liquid weight ratio is 1: 10, extraction temperature is 75 ℃, extracts 2 times, extraction time 1.2h; In the ethanol recovery device, recover ethanol at a temperature of 85°C and normal pressure to obtain a paste-like concentrate; then add water to completely disperse the paste-like concentrate, and then add petroleum ether according to 4 times the volume of the paste-like concentrate. Extract under normal pressure for 50min, extract twice; go through 100μm silica gel column chromatography, and elute with 35% ethanol, heat the eluent to 40°C to crystallize, centrifuge, wash twice with water, and put the crystal in a constant temperature drying oven Heated to 60°C and dried for 5 hours to obtain 65g of 97% allantoin.

Embodiment 3

[0010] Embodiment 3: Get 10kg Nitraria thorn residue, add 60% ethanol to extract, its solid-liquid weight ratio is 1: 15, extraction temperature is 60 ℃, extraction 1 time, extraction time 1h; In the ethanol recovery device, recover ethanol at a temperature of 90°C under normal pressure to obtain a paste-like concentrate; then add water to completely disperse the paste-like concentrate, then add petroleum ether according to 5 times the volume of the paste-like concentrate. Extract under pressure for 60 min, extract once; after 150 μm silica gel column chromatography, and elute with 50% ethanol, heat the eluent to 30°C to crystallize, centrifuge, wash with water for 3 times, and store the crystal in a constant temperature drying oven Heated to 70°C and dried for 6 hours to obtain 63g of 96.8% allantoin.

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Abstract

The invention relates to a method for preparing allantoin from nitraria core residue, which comprises the processes of extraction, condensation, dispersion, extraction, chromatography, elution, crystallization, separation, washing and drying. The method is simple and has no pollution; the extraction rate reaches 90 percent; the method can comprehensively utilize waste resources and is favorable for industrialized production; and the method is the continuation of comprehensive utilization of nitraria, has the premises of protecting and recovering deserts, wildernesses and saline-alkali ecological environments, has the purpose of comprehensively utilizing the nitraria with regional characteristics and resource advantages, and provides a new technical scheme for developing the nitraria resources in large scale.

Description

1. Technical field [0001] The invention relates to a method for preparing allantoin, in particular to a method for preparing allantoin from the residue of Nitraria fruit stone. 2. Background technology [0002] Nitraria L. is a small deciduous shrub of the genus Nitraria L. in the family Zygophyllaceae. It is a common wild saline-alkali plant in Northwest my country, which has high economic, ecological and medicinal value. Its fruit is rich in vitamins, amino acids, polysaccharides and other nutritional active ingredients, especially amino acids, which are easily absorbed and utilized by the human body, and the average content of allantoin in the residue of Nitraria thorn fruit is 6.918mg / g , has not yet been exploited. [0003] Allantoin, alias: 5-ureidohydantoin, ureidoacetolactam, ureidohydantoin, ureidoimidazole dione. Molecular formula: C 4 h 6 o 3 N 4 , molecular weight: 158.12, melting point: 226~240℃. The structural formula is as follows: [0004] [0005...

Claims

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Application Information

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IPC IPC(8): C07D233/88
Inventor 山永凯李树志索有瑞任蓓蕾马宁安刘洪智杨莉华李兆千李安军年璟远张辉李宁
Owner QINGHAI QINGMEI BIOLOGICAL RESOURCES R&D
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