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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 Optimum Technology of Extracting Trigonelline from Pumpkin Pulp by Ultrasonic Method", using 50% ethanol for ultrasonic extraction at 600W for 15 minutes, the ratio of liquid to material was 20ml / g, and the extraction rate was low, only 359.6μg / g
And the cost of extracting trigonelline from pumpkin is relatively high, because the content of trigonelline in pumpkin powder is low, which is 0.1219~0.4836mg / g (Zhang Yingchun, Yang Xin, Zhang Hua, etc. Determination of pumpkin by high performance liquid chromatography The content of trigonelline in powder. Food Science. 2008, 29 (1): 280-282), about 1 / 10 of the content of trigonelline in fenugreek seeds

Method used

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  • Process for extracting trigonelline

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Experimental program
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Effect test

Embodiment 1

[0025] Take the fenugreek medicinal material to remove impurities, pulverize it with a BFM-6 ultra-low temperature ultra-fine high-frequency vibration ultra-fine pulverizer, weigh 10kg, put it into an extraction tank, add 6 times the amount of ammonia alcohol solution for soaking and perform 25kHz ultrasonic treatment at the same time, soaking time For 45 minutes, the fenugreek medicinal material after soaking was extracted 3 times (6 times, 3 times, 3 times) with the reflux extraction method, each time for 2 hours, the combined extracts were filtered out, and the filtrate reclaimed ethanol to 15kg. Extract the same volume of petroleum ether in 4 times, discard the extract, mix the raffinate with 3 times the amount of 160-200 mesh alumina, dry and pulverize at 40-60°C, pass through a 150-200 mesh sieve and load into the chromatographic column, eluted with isopropanol, detected by TLC, collected the eluate, concentrated and dried the eluate under reduced pressure, reconstituted ...

Embodiment 2

[0027] Take the fenugreek medicinal material to remove impurities, pulverize it with a FWS350 winnowing type pulverizer, weigh 10kg, put it into an extraction tank, add 5 times the amount of ammonia alcohol solution to soak and carry out 30kHz ultrasonic treatment at the same time, the soaking time is 60 minutes, the soaked The fenugreek medicinal material is extracted 3 times (5 times, 4 times, 3 times) by reflux extraction method, each time for 3 hours, the extracts are combined, the dregs are filtered out, the filtrate recovers ethanol to 15kg, and is divided into 5 kg with an equal volume of petroleum ether. For secondary extraction, discard the extract, mix the raffinate with 4 times the amount of 160-200 mesh alumina, mix the sample, dry and pulverize at 40-60°C, pass through a 150-200 mesh sieve and load it into a chromatography column, 95% Eluted with ethanol, detected by TLC, collected the eluate, concentrated and dried the eluate under reduced pressure, reconstituted ...

Embodiment 3

[0029] Get the fenugreek medicinal material to remove impurities, crush it with a GZM type high-frequency resonance grinder, weigh 10kg, put it into an extraction tank, add 4 times the amount of 90% ethanol solution to soak and perform 25kHz ultrasonic treatment at the same time, the soaking time is 45 minutes, after soaking The fenugreek medical material extracted 3 times (4 times, 4 times, 4 times) with reflux extraction method, each time 4 hours, combined extracts, filtered off the medicine residues, the filtrate reclaimed ethanol to 15kg, and divided it with an equal volume of petroleum ether. Extract 4 times, discard the extract, mix the raffinate with 3 times the amount of 160-200 mesh alumina, dry and pulverize at 40-60°C, pass through a 150-200 mesh sieve, and put it into a chromatography column. Elute with propanol, detect with TLC, collect the eluate, concentrate and dry the eluate under reduced pressure, reconstitute the dried extract with ethanol, centrifuge, recove...

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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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