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Process for extracting thymoquinone from nigella plant seeds

A technology of Nigella and thymoquinone, which is applied in the field of natural medicine extraction and separation, can solve the problems of unfavorable separation and purification, instability of thymoquinone to light, etc.

Inactive Publication Date: 2015-06-03
JIANGNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Thymoquinone is unstable to light, is volatile, and is easily soluble in organic solvents of different polarities. The seeds of Nigella genus contain a lot of oil. When thymoquinone is extracted by traditional solvent extraction method, it will be extracted at the same time A large number of impurities are not conducive to further separation and purification

Method used

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  • Process for extracting thymoquinone from nigella plant seeds

Examples

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Embodiment 1

[0020] Weigh 1g of crushed seeds of Nigella japonica that have passed through a standard sieve with an aperture of 0.5mm, put it in a 50mL conical flask, add 20mL of absolute ethanol, adjust the microwave output power to 400W, extract for 15 seconds, and filter to obtain a solid filter residue and thymoquinone extract, re-transfer the filter residue into the original Erlenmeyer flask, add 20mL of absolute ethanol, adjust the microwave output power to 400W, extract again for 15 seconds, filter, and combine the extracts; the extracts are evaporated by rotary film The solvent was recovered to dryness at 30°C, and the residue was dissolved in 2 mL of petroleum ether-ethyl acetate (9:1) solution as a sample solution. Weigh 10 g of 200-300 mesh silica gel, fill it with petroleum ether into a glass chromatography column with a diameter of 1.5 cm, and pre-elute with 50 mL of petroleum ether-ethyl acetate (9:1) for later use. Transfer all the sample solution to the top of the pre-treat...

Embodiment 2

[0022] Weigh 50g of black cumin seeds harvested and dried in the same year, and quickly pulverize them with a universal grinder to pass through a standard sieve with an aperture of 0.5mm; place them in a 1000mL conical flask, add 500mL of absolute ethanol, and adjust the microwave output power to 600W , extract for 100 seconds, filter to obtain solid filter residue and thymoquinone extract, transfer the filter residue to the original Erlenmeyer flask again, add 500mL absolute ethanol, adjust the microwave output power to 600W, extract again for 100 seconds, filter, The extracts were combined; the extract was passed through a rotary thin film evaporator, and the solvent was recovered to dryness at 30°C, and the residue was dissolved in 20mL of petroleum ether-ethyl acetate (9:1) solution as a sample solution. Weigh 400 g of 200-300 mesh silica gel, fill it in a glass chromatography column with a diameter of 10 cm with petroleum ether, and pre-elute with 1000 mL of petroleum ethe...

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Abstract

The invention discloses a method for extracting thymoquinone in nigella plant seeds on the basis of a microwave-assisted solvent extraction method and separating the thymoquinone in nigella plant seeds by virtue of silica gel column chromatography. The method comprises the following steps: extracting: weighing the crushed nigella plant seeds, adding absolute ethyl alcohol according to a certain ratio of material to liquor, extracting under the condition of the microwave irradiation power of 400-700W, filtering, thereby obtaining solid filter residues and thymoquinone extracting solution; repeatedly extracting the filter residues for 1-2 times according to the previous extraction step, and mixing the extracting solution; and separating and purifying: recycling the solvent from the extracting solution at a low temperature until the solution is dry, adding a proper amount of petroleum ether-ethyl acetate (9:1) solution for dissolving, totally transferring the dissolving solution to the top end of the pretreated silica gel chromatography column, eluting by using petroleum ether-ethyl acetate (8:2), collecting the eluent, performing vacuum concentration on the eluent, drying at a low temperature, thereby obtaining the thymoquinone.

Description

technical field [0001] The invention relates to a method for extracting and separating natural active ingredients, in particular to a process for extracting and separating thymoquinone in the seeds of Ranunculaceae Nigella plants, and belongs to the field of extraction and separation of natural medicines. Background technique [0002] Nigella nigella is the dry mature seed of Nigella glandulifera Freyn, a plant of Ranunculaceae. It is mainly distributed in Xinjiang and Yunnan of my country. It has been used for thousands of years as a traditional medicinal material of the Uyghur and Dai people, and has been included in the Pharmacopoeia of the People's Republic of China. "In one part, it has the effects of nourishing the kidney and brain, stimulating the menstrual flow, and diuresis. There are mainly Nigella sativa L. and Nigella damascena L. which are more researched and used in the world. Now the utilization of Nigella cumin is mainly to extract its oil and use it in relat...

Claims

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Application Information

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IPC IPC(8): C07C50/02C07C46/10
CPCC07C46/10C07C50/02
Inventor 刘学曹光群杨成
Owner JIANGNAN UNIV
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