Process for extracting trigonelline

An extraction process and fenugreek alkaloid technology, applied in the direction of organic chemistry and the like, can solve the problems of unsuitable industrialization, low extraction rate, and high cost of fenugreek alkaloid extraction, and achieve the effects of shortening extraction time, less dissolved impurities, and increased content

Inactive Publication Date: 2011-02-09
NANJING ZELANG MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, the research on fenugreek is limited to its determination method of trigonelline content and preliminary pharmacological research, and there are few studies on the extraction method of fenugreek medicinal materials. In the literature, water, methanol, absolute ethanol and three ratios of methanol-water are used as solvents, and the extraction rate of ultrasound and other methods is investigated, but considering the effect of a large amount of methanol on the nervous system and blood system of the operator Toxic influence, the inventor thinks that this method is not suitable for industrialization
Xu Yaqin et al. published "Study on the O

Method used

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  • Process for extracting trigonelline

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Example Embodiment

[0024] Example 1:

[0025] Take the fenugreek medicinal material to remove impurities, crush it with a BFM-6 ultra-low temperature ultrafine high-frequency vibration type ultrafine grinder, weigh 10kg, put it into the extraction tank, add 6 times the amount of ammonia alcohol solution to soak and perform 25kHz ultrasonic treatment, soaking time For 45 minutes, the soaked fenugreek medicinal materials are extracted 3 times (6 times, 3 times, 3 times) by reflux extraction, 2 hours each time, the extracts are combined, the medicinal residue is filtered, and the filtrate is recovered to 15 kg of ethanol. The same volume of petroleum ether is extracted 4 times, the extract is discarded, the raffinate is mixed with 3 times the amount of 160-200 mesh alumina, and the sample is dried and crushed at 40-60°C, and then packed through a 150-200 mesh sieve. Enter the chromatographic column, elution with isopropanol, TLC detection, collect the eluate, concentrate and dry the eluate under reduc...

Example Embodiment

[0026] Example 2:

[0027] Take the fenugreek medicinal material to remove impurities, pulverize with the FWS350 type winnowing type micro pulverizer, weigh 10kg, put it into the extraction tank, add 5 times the amount of ammonia alcohol solution soak and carry out 30kHz ultrasonic treatment, soaking time is 60 minutes, after soaking Fenugreek medicinal material was extracted 3 times (5 times, 4 times, 3 times) by reflux extraction method, 3 hours each time, the extracts were combined, the medicine residue was filtered out, the filtrate was recovered to 15 kg of ethanol, and the same volume of petroleum ether was used for 5 After extraction, discard the extract, mix the raffinate with 4 times the amount of 160-200 mesh alumina, mix the sample, dry and crush at 40-60°C, pass through a 150-200 mesh sieve, and load into a chromatography column, 95% Ethanol elution, TLC detection, collect the eluate, concentrate the eluate to dryness under reduced pressure, reconstitute the dried ext...

Example Embodiment

[0028] Example 3:

[0029] Take the fenugreek medicinal material to remove impurities, crush it with a GZM high-frequency resonance mill, weigh 10kg, put it into an extraction tank, add 4 times the amount of 90% ethanol solution to soak and carry out 25kHz ultrasonic treatment, soaking time is 45 minutes, after soaking The fenugreek medicinal material is extracted 3 times (4 times, 4 times, 4 times) by reflux extraction method, 4 hours each time, the extracts are combined, the medicine residue is filtered, the filtrate is recovered to 15 kg of ethanol, and the same volume of petroleum ether is used to separate Extract 4 times, discard the extract, mix the raffinate with 3 times the amount of 160-200 mesh alumina, mix the sample, dry and crush at 40-60 ℃, pass through a 150-200 mesh sieve, and load it into a chromatography column. Elute with propanol, detect by TLC, collect the eluate, concentrate and dry the eluate under reduced pressure, reconstitute the dried extract with ethan...

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Abstract

The invention relates to a process for extracting trigonelline. The process comprises the following steps of: crushing raw materials, soaking the powder into amino alcohol solution or aqueous ethanol, performing reflux extraction on the solution with heating, concentrating the extract to be small volume, extracting the concentrate by using petroleum ether, removing the extract, filling the raffinate into an aluminum oxide column for chromatography, eluting the column by using isopropyl alcohol or ethanol as eluent, concentrating the eluted solution and drying the concentrate. The product produced by the process has low impurity content and high effective ingredient yield, and the operation is simple and convenient to master.

Description

Technical field: [0001] The invention belongs to the field of natural medicine extraction, and relates to an extraction process of trigonelline. Background technique: [0002] Trigonelline (TRG), [0003] Molecular formula: C 7 h 7 NO 2 ;Molecular weight: 137.14; [0004] Molecular formula: [0005] [0006] Fenugreek is the dry mature seed of Trigonella foenum-graecum L., a leguminous plant. It has the functions of warming the kidney, dispelling cold, and relieving pain. It is bitter in nature and warm, and returns to the kidney meridian. It is used for kidney deficiency and coldness, cold pain in the lower abdomen, small intestinal hernia, and cold-damp beriberi. [0007] Modern pharmacological studies have shown that fenugreek has anti-diabetic, cholesterol-lowering and protective effects on acute chemical liver injury. Trigonelline, the main component of fenugreek, has anti-tumor effects, and can prolong the expression of leukemia P-388 mice by 31% at the leve...

Claims

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Application Information

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IPC IPC(8): C07D213/80C07D213/803
Inventor 刘东锋郭琴杨成东
Owner NANJING ZELANG MEDICAL TECH
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