A method for efficiently extracting and separating high-purity ligustrazine from Podocarpus seeds

A technology of ligustrazine and podocarpus, which is applied in the fields of natural medicinal chemistry, medicine and traditional Chinese medicine chemistry, can solve the problems of using a large amount of chemical reagents, cumbersome preparation steps, and low product purity, and achieve solvent saving, few operation steps, and low boiling point Effect

Inactive Publication Date: 2018-08-14
黄增琼
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The purpose of the present invention is to provide a new method for fast extraction and separation to obtain high-purity ligustrazine for the problems of cumbersome preparation steps, long production cycle, low product purity or the need to use a large amount of chemical reagents in the prior art.

Method used

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  • A method for efficiently extracting and separating high-purity ligustrazine from Podocarpus seeds
  • A method for efficiently extracting and separating high-purity ligustrazine from Podocarpus seeds
  • A method for efficiently extracting and separating high-purity ligustrazine from Podocarpus seeds

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Experimental program
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Effect test

Embodiment 1

[0020] Take 100g of podocarpus seeds, remove impurities, pulverize, pass through a 10-mesh sieve, put into a round bottom flask, add water 10 times the mass of medicinal materials, soak for 30 minutes, steam distillation, heat extraction for 6 hours, collect distillate, Put it in a separatory funnel, add petroleum ether with a boiling range of 30-60°C for extraction twice, the amount of petroleum ether is equal to the volume of the distillate each time, combine the petroleum ether layers extracted twice, and reduce at 30°C with a rotary evaporator. Recover petroleum ether under pressure until the recovered petroleum ether volume is equal to 99% of the initial volume, stop the recovery, evaporate the solvent naturally from the concentrated solution, and obtain ligustrazine crystals, the purity of which is detected by HPLC is 95.2%, recrystallize with water, wash and dry to obtain Ligustrazine fine product 0.01g, HPLC detection purity is 98.5%.

Embodiment 2

[0022] Take 100g of podocarpus seeds, remove impurities, pulverize, pass through a 10-mesh sieve, put into a round bottom flask, add 15 times the amount of water of the medicinal material, soak for 30 minutes, steam distillation, heat extraction for 8 hours, collect the distillate, Put it in a separatory funnel, add petroleum ether with a boiling range of 30-60°C for extraction twice, each time the volume of petroleum ether added is 1.5 times the volume of the distillate, combine the petroleum ether layers extracted twice, and use a rotary evaporator to Recover petroleum ether under reduced pressure at 40°C. When the recovered petroleum ether volume is equal to 98% of the initial volume, the recovery is stopped. The concentrated solution is allowed to stand at room temperature for 12 hours, and filtered with suction to obtain Ligustrazine crystals. The purity detected by HPLC is 96.4%. Crystallized, washed and dried to obtain 0.012 g of Ligustrazine fine product, with a purity ...

Embodiment 3

[0024] Take 100g of podocarpus seeds, remove impurities, pulverize, pass through a 10-mesh sieve, put into a round bottom flask, add 20 times the amount of water of the medicinal material, soak for 30 minutes, steam distillation, heat extraction for 9 hours, collect the distillate, Put it in a separatory funnel, add petroleum ether with a boiling range of 30-60°C for extraction three times, each time the volume of petroleum ether added is 0.5 times the volume of the distillate, combine the petroleum ether layers extracted three times, and use a rotary evaporator to Recover petroleum ether under reduced pressure at 50°C, stop the recovery when the volume of petroleum ether recovered is equal to 95% of the initial volume, refrigerate the concentrated solution at 4°C for 8 hours, and filter with suction to obtain tetramethylpyrazine crystals, the purity of which is detected by HPLC is 96.0%. Crystallized, washed and dried to obtain 0.015 g of Ligustrazine fine product, with a puri...

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Abstract

The invention relates to a method for efficiently extracting and separating high-purity ligustrazine from podocarpus macrophyllus seeds. The method includes the steps that podocarpus macrophyllus seed coarse powder is taken, water is added for soaking for 30 min, the mixture is heated and extracted for 6-9 hours through a steam distillation method, distillate is collected, petroleum ether is added for extraction, a petroleum ether layer reduced pressure recycled solvent is taken, a concentrated solution is subjected to suction filtration after standing or being refrigerated, drying is carried out, coarse crystals are obtained, water is added for re-crystalization, washing and drying are carried out, and the high-purity ligustrazine is obtained. The ligustrazine is prepared through the method, fewer steps are adopted, the period is short, operation is easy and convenient, the product is high in purity, equipment investment is small, and the production cost can be greatly reduced.

Description

technical field [0001] The invention belongs to the technical fields of traditional Chinese medicine chemistry, natural medicine chemistry and medicine, and in particular relates to a method for efficiently extracting, separating and purifying high-purity ligustrazine from podocarpus seeds. Background technique [0002] Podocarpus is actually the seed and receptacle of Podocarpus macrophyllus (Thunb.) D.Don or Podocarpus macrophyllus (Thunb.) D.Don var.maki (Sieb.) Endl. According to literature records, podocarpus has the effect of invigorating the kidney and lung, treating blood deficiency, sallow complexion, heart and stomach pain. Podocarpus has been planted on a large scale in Beihai City, Guangxi, with a planting area of ​​15,000 mu, and a large amount of Podocarpus can be produced every year. The receptacle part of the podocarpus fruit can be directly eaten as a fruit, or made into fruit wine or health wine and sold on the market. However, the seed part of Podocarpus...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D241/12
CPCC07D241/12
Inventor 黄增琼曾凡艳
Owner 黄增琼
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