New method for extracting Swainsonine from locoweed

Abstract

This invention discloses a novel method for extracting swainsonine from locoweed. The method comprises: (1) extracting locoweed powder with ethanol at a ratio of 1:(6-10) for 3 times (4 h each time), filtering, recovering ethanol, dissolving the residue with 3-5 times of ethanol, recovering ethanol to obtain an extractum, adding 2% acetic acid to adjust the pH value to 4.5-6, adding 50-100 times of chloroform, and recovering the chloroform layer; (2) extracting the acidic water layer with 50 times of chloroform for twice, recovering chloroform, drying the acidic water at 50-60 deg.C to obtain crude alkaloids, completely dissolving in 1 M ammonium solution, adding 10% NaOH solution (1 mL / 45-75 g) and methanol (5 mL / 45-75 g) into alkaloids solution, extracting with dichloromethane repeatedly until the solution color is light, adding ammonium solution to completely dissolve the residue, extracting with dichloromethane, and recovering dichloromethane to obtain crude swainsonine; (3) dissolving with methanol, evaporating methanol, and sublimating to obtain white needle-like crystals. The method has such advantages as easy operation, and high extraction rate.

Description

technical field

[0001] The invention belongs to the technical field of material components, and in particular relates to a new method for extracting swainsonine from locoweed. Background technique

[0002] Swainsonin is the main toxic component in locoweeds. Long-term consumption of locoweeds by animals can cause toxic diseases characterized by central nervous system dysfunction. Since locoweeds are widely distributed in the world, they are the most serious hazards to grassland animal husbandry. The poisonous weed has attracted much attention. At the same time, swainsonine is an inhibitor of α-mannosidase in lysosomes. It has received great attention as a new anticancer drug in recent years. It is characterized by its ability to kill cancer cells and immune regulation. function to inhibit tumor growth and metastasis [1] . At present, the research on the mechanism of locoweed poisoning requires a large amount of swainsonine. At the same time, swainsonine has broad applicat...

Examples

Embodiment 1

[0046] Example 1 Extraction of swainsonine in Oxytropis glacier

[0047] 1. Extraction of extract: add 1Kg of Oxytropis glacier powder to 6L ethanol for extraction 3 times, each time for 4 hours, filter, recover ethanol with a rotary evaporator, dissolve the residue with 6L ethanol, recover ethanol with a rotary evaporator to obtain 420.5g of extract .

[0048] 2) Add 2% acetic acid and 500mL chloroform to every 40g of the extract, collect the chloroform layer, and recover the chloroform; the acid water part is extracted twice with 500mL chloroform, and the acid water is placed in a 20×20cm glass baking dish at 50°C Dry the moisture in a ventilated oven to obtain 51.8 g of crude alkaloids.

[0049] 3) Dissolve the crude alkaloid with 1M ammonia water, add 1mL 10% NaOH, 5mL methanol, extract with dichloromethane, dissolve the residue with ammonia water, extract with dichloromethane, recover dichloromethane, and obtain crude swainsonine 0.6 g.

[0050] 4) Dissolve the crude s...

Embodiment 2

[0051] Example 2 Extraction of swainsonine in Oxytropis gansu

[0052] 1. Extraction of extract: add 2Kg of Oxytropis gansuensis powder to 14L ethanol and extract 3 times, 4 hours each time, filter, recover ethanol with a rotary evaporator, dissolve the residue with 14L ethanol, recover ethanol with a rotary evaporator to obtain 968.8g of extract .

[0053] 2) Add 2% acetic acid and 1000mL chloroform to every 50g of the extract, collect the chloroform layer, and recover the chloroform; the acidic water part is extracted twice with 500mL chloroform, and the acidic water is placed in a 20×20cm glass baking dish at 60°C Dry the moisture in a ventilated oven to obtain 131.5 g of crude alkaloids.

[0054] 3) Dissolve 131.5 g of crude alkaloids with 1M ammonia water, add 2 mL of 10% NaOH and 10 mL of methanol, extract with dichloromethane, dissolve the residue with ammonia water, extract with dichloromethane, recover dichloromethane, and obtain horse bean Vegetable crude product 1...

Embodiment 3

[0057] 1 Extraction of extract: add 2Kg of Oxytropis gansuensis powder to 20L ethanol for extraction 3 times, 4 hours each time, filter, recover ethanol with a rotary evaporator, dissolve the residue with 12L ethanol, recover ethanol with a rotary evaporator to obtain 968.8g of extract .

[0058] 2) Add 2% acetic acid and 1000mL chloroform to every 50g of the extract, collect the chloroform layer, and recover the chloroform; the acidic water part is extracted twice with 500mL chloroform, and the acidic water is placed in a 20×20cm glass baking dish at 60°C Dry the moisture in a ventilated oven to obtain 131.5 g of crude alkaloids.

[0059] 3) Dissolve 131.5 g of crude alkaloids with 1M ammonia water, add 2 mL of 10% NaOH and 10 mL of methanol, extract with dichloromethane, dissolve the residue with ammonia water, extract with dichloromethane, recover dichloromethane, and obtain horse bean Vegetable crude product 1.5g.

[0060] 4) Dissolve the crude swainsonine in methanol, t...

technical field

[0001] The invention belongs to the technical field of material components, and in particular relates to a new method for extracting swainsonine from locoweed. Background technique

[0002] Swainsonin is the main toxic component in locoweeds. Long-term consumption of locoweeds by animals can cause toxic diseases characterized by central nervous system dysfunction. Since locoweeds are widely distributed in the world, they are the most serious hazards to grassland animal husbandry. The poisonous weed has attracted much attention. At the same time, swainsonine is an inhibitor of α-mannosidase in lysosomes. It has received great attention as a new anticancer drug in recent years. It is characterized by its ability to kill cancer cells and immune regulation. function to inhibit tumor growth and metastasis [1] . At present, the research on the mechanism of locoweed poisoning requires a large amount of swainsonine. At the same time, swainsonine has broad applicat...

Examples

Embodiment 1

[0046] Example 1 Extraction of swainsonine in Oxytropis glacier

[0047] 1. Extraction of extract: add 1Kg of Oxytropis glacier powder to 6L ethanol for extraction 3 times, each time for 4 hours, filter, recover ethanol with a rotary evaporator, dissolve the residue with 6L ethanol, recover ethanol with a rotary evaporator to obtain 420.5g of extract .

[0048] 2) Add 2% acetic acid and 500mL chloroform to every 40g of the extract, collect the chloroform layer, and recover the chloroform; the acid water part is extracted twice with 500mL chloroform, and the acid water is placed in a 20×20cm glass baking dish at 50°C Dry the moisture in a ventilated oven to obtain 51.8 g of crude alkaloids.

[0049] 3) Dissolve the crude alkaloid with 1M ammonia water, add 1mL 10% NaOH, 5mL methanol, extract with dichloromethane, dissolve the residue with ammonia water, extract with dichloromethane, recover dichloromethane, and obtain crude swainsonine 0.6 g.

[0050] 4) Dissolve the crude s...

Embodiment 2

[0051] Example 2 Extraction of swainsonine in Oxytropis gansu

[0052] 1. Extraction of extract: add 2Kg of Oxytropis gansuensis powder to 14L ethanol and extract 3 times, 4 hours each time, filter, recover ethanol with a rotary evaporator, dissolve the residue with 14L ethanol, recover ethanol with a rotary evaporator to obtain 968.8g of extract .

[0053] 2) Add 2% acetic acid and 1000mL chloroform to every 50g of the extract, collect the chloroform layer, and recover the chloroform; the acidic water part is extracted twice with 500mL chloroform, and the acidic water is placed in a 20×20cm glass baking dish at 60°C Dry the moisture in a ventilated oven to obtain 131.5 g of crude alkaloids.

[0054] 3) Dissolve 131.5 g of crude alkaloids with 1M ammonia water, add 2 mL of 10% NaOH and 10 mL of methanol, extract with dichloromethane, dissolve the residue with ammonia water, extract with dichloromethane, recover dichloromethane, and obtain horse bean Vegetable crude product 1...

Embodiment 3

[0057] 1 Extraction of extract: add 2Kg of Oxytropis gansuensis powder to 20L ethanol for extraction 3 times, 4 hours each time, filter, recover ethanol with a rotary evaporator, dissolve the residue with 12L ethanol, recover ethanol with a rotary evaporator to obtain 968.8g of extract .

[0058] 2) Add 2% acetic acid and 1000mL chloroform to every 50g of the extract, collect the chloroform layer, and recover the chloroform; the acidic water part is extracted twice with 500mL chloroform, and the acidic water is placed in a 20×20cm glass baking dish at 60°C Dry the moisture in a ventilated oven to obtain 131.5 g of crude alkaloids.

[0059] 3) Dissolve 131.5 g of crude alkaloids with 1M ammonia water, add 2 mL of 10% NaOH and 10 mL of methanol, extract with dichloromethane, dissolve the residue with ammonia water, extract with dichloromethane, recover dichloromethane, and obtain horse bean Vegetable crude product 1.5g.

[0060] 4) Dissolve the crude swainsonine in methanol, t...

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