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Method for extracting, separating, purifying and detecting alangium total alkaloids

A technology for separation and purification of total alkaloids, applied in the field of pharmaceutical inventions, can solve problems such as low recovery rate, drug poisoning, and poor repeatability, and achieve a stable extraction process

Active Publication Date: 2022-05-27
贵州中医药大学
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] The technical problems in the above technology: 1) adopt high-performance liquid chromatography to measure, and the recovery rate is low; 2) adopt high-performance liquid chromatography to measure, and the repeatability is poor; drug poisoning

Method used

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  • Method for extracting, separating, purifying and detecting alangium total alkaloids
  • Method for extracting, separating, purifying and detecting alangium total alkaloids
  • Method for extracting, separating, purifying and detecting alangium total alkaloids

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0060] Example 1 Extraction, separation and purification

[0061] (1) Preparation of crude extract: Accurately weigh 200 g of the medicinal powder of Maple anise, put it in a round-bottomed flask, add 10 times the amount of 80% ethanol, reflux for 2 times, 2h each time, filter, combine the crude extract, and set aside for later use ;

[0062] (2) Preparation of sample solution: take the crude extract to recover ethanol with a rotary evaporator, concentrate to 500mL, add an appropriate amount of 80% ethanol to dilute to obtain a solution with a concentration of 3.02mg / mL, and then adjust it with sodium hydroxide and hydrochloric acid The pH of the solution is 6, that is, the sample solution;

[0063] (3) Separation and purification: Take D101 macroporous adsorption resin, pack the column by wet method with a diameter-to-height ratio of 1:3, take 15 mL of the sample solution, load the sample at a flow rate of 1 mL / min, collect the effluent, and let it stand for 1 h Then; elute...

Embodiment 2

[0064] Example 2 Extraction, separation and purification

[0065] (1) Preparation of crude extract: Accurately weigh 150 g of the medicinal powder of Maple anise, put it in a round-bottomed flask, add 8 times the amount of 60% ethanol, extract by reflux once, 1h each time, filter, combine the crude extracts, and set aside for later use ;

[0066] (2) Preparation of sample solution: take the crude extract to recover ethanol with a rotary evaporator, concentrate to 400mL, add an appropriate amount of 60% ethanol to dilute to obtain a solution with a concentration of 2.00mg / mL, and then adjust it with sodium hydroxide and hydrochloric acid The pH of the solution is 2, that is, the sample solution;

[0067] (3) Separation and purification: Take D101 macroporous adsorption resin, pack the column by wet method with a diameter-to-height ratio of 1:1, take 5 mL of the sample solution, load the sample at a flow rate of 1 mL / min, collect the effluent, and let it stand for 1 h Then; el...

Embodiment 3

[0068] Example 3 Extraction, separation and purification

[0069] (1) Preparation of crude extract: Accurately weigh 250g of the medicinal powder of Maple anise, put it in a round-bottomed flask, add 12 times the amount of 90% ethanol, reflux for 3 times, 3h each time, filter, combine the crude extract, and set aside for later use ;

[0070] (2) Preparation of sample solution: take the crude extract to recover ethanol with a rotary evaporator, concentrate it to 450mL, add an appropriate amount of 90% ethanol to dilute to obtain a solution with a concentration of 6.00mg / mL, and then adjust it with sodium hydroxide and hydrochloric acid The pH of the solution is 8, that is, the sample solution;

[0071] (3) Separation and purification: Take D101 macroporous adsorption resin, pack the column by wet method with a diameter-to-height ratio of 1:4, take 45 mL of the sample solution, load the sample at a flow rate of 1 mL / min, collect the effluent, and let it stand for 1 h Then; elu...

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Abstract

The invention relates to a method for extracting, separating, purifying and detecting alangium total alkaloids, D101 type macroporous adsorption resin is used for separating and purifying the alangium total alkaloids, and the purity of the total alkaloids in the obtained alangium extract is increased from 21.61% to 63.03%; the total alkaloids in the alangium platanifolium are determined by adopting an acid dye colorimetric method, and the precision RSD is 0.34%; the repeatability RSD is 1.40%; according to the method, the sample adding recovery rate is 102.72%, the RSD (Relative Standard Deviation) is 2.66%, and the method can be used for truly, effectively and accurately determining the content of the analangium potoxicochin, so that the medication safety and effectiveness are ensured.

Description

technical field [0001] The present invention relates to the field of medical inventions, in particular to a method for extraction, separation, purification and detection of total alkaloids of A. Background technique [0002] Alangium chinense (Alangium chinense), alias: Chinese melon, white dragon beard, wood star anise, orange wood. Deciduous small trees or shrubs, 4-5m high. The leaves are alternate, with different shapes, mainly distributed in the vast areas of southern China; also produced in eastern and southeastern Asia. Born in the mountains, shrubs and forests, it is also common on the side roads of the village. Warm in nature, pungent and bitter in taste, it has the effects of dispelling wind and dampness, relaxing tendons and activating collaterals, dispersing silt and relieving pain. [0003] Anise maple clears heat and detoxifies, promotes blood circulation and disperses stasis. The root and bark have the best medicinal effect, the root name is Bailongxu, and...

Claims

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Application Information

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IPC IPC(8): A61K36/185G01N21/78
CPCA61K36/185G01N21/78A61K2236/333A61K2236/39A61K2236/53A61K2236/51A61K2236/55Y02A50/30
Inventor 刘耀张永萍徐剑刘杰曹国琼程纯
Owner 贵州中医药大学
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