Method of extracting 2-hydroxylbenzyl amine from tartary buckwheat

Abstract

The invention discloses a method of extracting 2-hydroxylbenzyl amine from tartary buckwheat. The method comprises following steps: taking roots, stems, and seeds of tartary buckwheat as raw materials; grinding roots, stems, and seeds in liquid nitrogen; carrying out enzymatic hydrolysis, ultrasonic extraction, and alkaline solution extraction; acidifying the alkaline liquor by hydrochloric acid; adopting NDA-150 resin to carry out adsorption; eluting the NDA-150 resin by different alkaline solutions and water, and finally carrying out recrystallization to obtain 2-hydroxylbenzyl amine. Roots, stems, and seeds of tartary buckwheat are taken as the raw materials, novel raw materials and extraction method are provided for extraction of 2-hydroxylbenzyl amine, the raw materials are cheap, the yield of the extraction method is high, the purity of obtained 2-hydroxylbenzyl amine is high, and prepared 2-hydroxylbenzyl amine can be applied to industrial production.

Description

technical field

[0001] The invention belongs to the technical field of active ingredient extraction, and in particular relates to a method for extracting 2-hydroxybenzylamine from tartary buckwheat. Background technique

[0002] 2-Hydroxybenzylamine (2-HOBA), also known as salicylamine, is a potent γKA scavenger that clears γKAs 980 times faster than the formation of γKA protein adducts, thus protecting cells Protection from deleterious effects of γKA adducts. In vitro studies have demonstrated that 2-HOBA protects HepG2 cells from H 2 o 2 The effect of inducing cytotoxicity; the beneficial effect of 2-HOBA in oxidative stress-related diseases has also been found in multiple organs and systems in the body. 2-HOBA administration dose-dependently reduced biomarkers of oxidant damage and prolonged lifespan in C. elegans. Beneficial effects of 2-HOBA have been observed in various mouse models of neuropathology. After oral administration, 2-HOBA can pass through the blood-br...

Examples

Embodiment 1

[0032] A method for extracting 2-hydroxybenzylamine from tartary buckwheat, specifically comprising the following steps:

[0033] (1) drying tartary buckwheat roots, stems and grains respectively, adding liquid nitrogen and grinding to obtain powder;

[0034] (2) Mix the powder with deionized water, adjust the pH value of the solution to 5.0, then add 0.5% powder weight mixed enzyme for enzymolysis, the enzymolysis temperature is 25°C, and the enzymolysis time is 40min. After the enzymolysis is completed, filter , to obtain the filter residue; wherein, the mixed enzyme is a mixture of cellulase and pectinase in a weight ratio of 2:1;

[0035](3) The filter residue obtained in step (2) is mixed with 95% ethanol at a solid-to-liquid ratio of 1g:10mL, and then the ultrasonic power density is 100W / cm 2 1. Ultrasonic extraction was carried out under the condition of ultrasonic frequency of 30kHz, the extraction temperature was 20°C, the extraction time was 30min, the extraction wa...

Embodiment 2

[0045] A method for extracting 2-hydroxybenzylamine from tartary buckwheat, specifically comprising the following steps:

[0046] (1) drying tartary buckwheat roots, stems and grains respectively, adding liquid nitrogen and grinding to obtain powder;

[0047] (2) Mix the powder with deionized water, adjust the pH value of the solution to 6.0, then add 0.8% powder weight mixed enzyme for enzymolysis, the enzymolysis temperature is 50°C, the enzymolysis time is 30min, and filter after the enzymolysis is completed , get filter residue; Wherein, mixed enzyme is the mixture that cellulase and pectinase are mixed in 5:1 by weight ratio;

[0048] (3) The filter residue obtained in step (2) is mixed with 95% ethanol at a solid-to-liquid ratio of 1g:20mL, and then the ultrasonic power density is 150W / cm 2 1. Ultrasonic extraction was carried out under the condition of ultrasonic frequency of 50kHz, the extraction temperature was 40°C, the extraction time was 20min, the extraction was ...

Embodiment 3

[0058] A method for extracting 2-hydroxybenzylamine from tartary buckwheat, specifically comprising the following steps:

[0059] (1) drying tartary buckwheat roots, stems and grains respectively, adding liquid nitrogen and grinding to obtain powder;

[0060] (2) Mix the powder with deionized water, adjust the pH value of the solution to 5.5, then add 0.6% powder weight mixed enzyme for enzymolysis, the enzymolysis temperature is 35°C, and the enzymolysis time is 35min. After the enzymolysis is completed, filter , to obtain the filter residue; wherein, the mixed enzyme is a mixture of cellulase and pectinase in a weight ratio of 3:1;

[0061] (3) the filter residue obtained in step (2) is mixed with 95% ethanol at a solid-to-liquid ratio of 1g:13mL, and then the ultrasonic power density is 120W / cm 2 1. Ultrasonic extraction was carried out under the condition of ultrasonic frequency of 35kHz, the extraction temperature was 25°C, the extraction time was 15min, the extraction w...

technical field

[0001] The invention belongs to the technical field of active ingredient extraction, and in particular relates to a method for extracting 2-hydroxybenzylamine from tartary buckwheat. Background technique

[0002] 2-Hydroxybenzylamine (2-HOBA), also known as salicylamine, is a potent γKA scavenger that clears γKAs 980 times faster than the formation of γKA protein adducts, thus protecting cells Protection from deleterious effects of γKA adducts. In vitro studies have demonstrated that 2-HOBA protects HepG2 cells from H 2 o 2 The effect of inducing cytotoxicity; the beneficial effect of 2-HOBA in oxidative stress-related diseases has also been found in multiple organs and systems in the body. 2-HOBA administration dose-dependently reduced biomarkers of oxidant damage and prolonged lifespan in C. elegans. Beneficial effects of 2-HOBA have been observed in various mouse models of neuropathology. After oral administration, 2-HOBA can pass through the blood-br...

Examples

Embodiment 1

[0032] A method for extracting 2-hydroxybenzylamine from tartary buckwheat, specifically comprising the following steps:

[0033] (1) drying tartary buckwheat roots, stems and grains respectively, adding liquid nitrogen and grinding to obtain powder;

[0034] (2) Mix the powder with deionized water, adjust the pH value of the solution to 5.0, then add 0.5% powder weight mixed enzyme for enzymolysis, the enzymolysis temperature is 25°C, and the enzymolysis time is 40min. After the enzymolysis is completed, filter , to obtain the filter residue; wherein, the mixed enzyme is a mixture of cellulase and pectinase in a weight ratio of 2:1;

[0035](3) The filter residue obtained in step (2) is mixed with 95% ethanol at a solid-to-liquid ratio of 1g:10mL, and then the ultrasonic power density is 100W / cm 2 1. Ultrasonic extraction was carried out under the condition of ultrasonic frequency of 30kHz, the extraction temperature was 20°C, the extraction time was 30min, the extraction wa...

Embodiment 2

[0045] A method for extracting 2-hydroxybenzylamine from tartary buckwheat, specifically comprising the following steps:

[0046] (1) drying tartary buckwheat roots, stems and grains respectively, adding liquid nitrogen and grinding to obtain powder;

[0047] (2) Mix the powder with deionized water, adjust the pH value of the solution to 6.0, then add 0.8% powder weight mixed enzyme for enzymolysis, the enzymolysis temperature is 50°C, the enzymolysis time is 30min, and filter after the enzymolysis is completed , get filter residue; Wherein, mixed enzyme is the mixture that cellulase and pectinase are mixed in 5:1 by weight ratio;

[0048] (3) The filter residue obtained in step (2) is mixed with 95% ethanol at a solid-to-liquid ratio of 1g:20mL, and then the ultrasonic power density is 150W / cm 2 1. Ultrasonic extraction was carried out under the condition of ultrasonic frequency of 50kHz, the extraction temperature was 40°C, the extraction time was 20min, the extraction was ...

Embodiment 3

[0058] A method for extracting 2-hydroxybenzylamine from tartary buckwheat, specifically comprising the following steps:

[0059] (1) drying tartary buckwheat roots, stems and grains respectively, adding liquid nitrogen and grinding to obtain powder;

[0060] (2) Mix the powder with deionized water, adjust the pH value of the solution to 5.5, then add 0.6% powder weight mixed enzyme for enzymolysis, the enzymolysis temperature is 35°C, and the enzymolysis time is 35min. After the enzymolysis is completed, filter , to obtain the filter residue; wherein, the mixed enzyme is a mixture of cellulase and pectinase in a weight ratio of 3:1;

[0061] (3) the filter residue obtained in step (2) is mixed with 95% ethanol at a solid-to-liquid ratio of 1g:13mL, and then the ultrasonic power density is 120W / cm 2 1. Ultrasonic extraction was carried out under the condition of ultrasonic frequency of 35kHz, the extraction temperature was 25°C, the extraction time was 15min, the extraction w...