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Fast production of high-purity radix ligustici sinensis lactone

A high-purity technology for ligustilide, applied in the field of rapid preparation of high-purity ligustilide, can solve the problems of uncommon, cumbersome detection methods, low production efficiency, etc., and achieve convenient and accurate identification methods, strong scientific and Exclusiveness, the effect of saving production costs

Inactive Publication Date: 2007-11-28
钱忠明 +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The operation of this method is also relatively complicated, and the detection method is not commonly used, the amount of adsorbent is large, the implementation is relatively difficult, and it cannot be used in large-scale production
[0015] The above-mentioned separation methods of ligustilide that have been reported are all separated by conventional chromatographic methods (such as: normal pressure or pressurized column chromatography), and its biggest feature is that the chromatographic column must Always keep a sufficient amount of eluent, and conventional column chromatography has the following disadvantages: complicated operation, slow separation speed, many and cumbersome separation steps, long separation time, and cannot be stopped and adjusted at will during the separation process, and The amount of adsorbent and organic solvent used is large, and the regeneration of the adsorbent is difficult, which is not conducive to the control of production cost and environmental protection
Moreover, none of the above-mentioned methods provides a very convenient and fast fraction detection method, and the purity of ligustilide in the fraction cannot be quickly judged after separation, which also leads to low production efficiency and greatly limits its application in industrial production.
[0016] And because of the instability of ligustilide itself, it is very prone to isomerization at a slightly higher temperature for a long time, so in industrial production, the production speed is a bottleneck for the preparation of high-purity ligustilide

Method used

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  • Fast production of high-purity radix ligustici sinensis lactone
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  • Fast production of high-purity radix ligustici sinensis lactone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0064] (1) Extraction and separation:

[0065] Extract ligustilide crude oil with ethanol reflux extraction method: weigh 20kg of angelica crude drug and chop it properly, add 8 times the amount of 95% ethanol to soak overnight in the extraction tank, heat and reflux extraction for 2 hours, filter, and separate the drug residues Add 6 times and 6 times the amount of 95% ethanol, heat and reflux for extraction for 2 hours respectively, filter and combine the filtrates, concentrate the filtrate under reduced pressure to recover the ethanol, and obtain about 800ml of dark brown thick liquid crude oil.

[0066] Mix the sample with 0.6kg of silica gel (100-200 mesh). Use a short thick column (diameter 25cm) to take 6kg of chromatography silica gel (200-300 mesh) and add silica gel while pumping with a water pump, and make it fully tightened so that the top surface is flat, and the height of the silica gel surface is about 30cm. Put the mixed sample silica gel on the short and thic...

Embodiment 2

[0089] Using 300-400 mesh silica gel, take 3 parts of 50ml of the same angelica volatile oil (the content of ligustilide is about 30%) respectively, add 50g of silica gel (80-100 mesh) to mix the samples respectively, and use vacuum column chromatography, Three different separation methods, such as normal pressure column chromatography and pressurized column chromatography, use the same petroleum ether-ethyl acetate elution system to complete a separation. The specific test is as follows:

[0090] Decompression column chromatography separation: use a sand core funnel (diameter 12.5cm) to take 250g of chromatography silica gel (300-400 mesh) and add silica gel while pumping with a water pump, and make it fully tightened so that the top surface is flat. The surface height is 5cm. Load the mixed sample on the top of the column, suck it with a water pump, first add 1L of petroleum ether to wash, and then wash with 4L of petroleum ether-ethyl acetate (30:1), 200ml (about 1 / 3 of th...

Embodiment 3

[0097] Ethanol leaching method to extract crude oil: Weigh 10kg of angelica crude drug and chop it properly, add 1 times the amount of 95% ethanol to moisten it, add it to the percolation irrigation, continue to add 2 times the amount of 95% ethanol, soak overnight, and then continue to add 15 times the amount of 95% ethanol was percolated at a drop rate of 1ml / kg.min, the leachate was collected, and concentrated under reduced pressure to obtain a crude oil of about 380ml of dark brown thick liquid.

[0098] The obtained crude oil was appropriately diluted with 400 ml of n-hexane. Use a sand core funnel (diameter 25cm) to take 3kg of chromatography silica gel (100-200 mesh) and add silica gel while pumping with a water pump, and make it fully tightened so that the top surface is flat, and the height of the silica gel surface is 12cm. Put the diluted sample on the silica gel column that has been installed, suck it with a water pump, first add 5L of n-hexane to rinse, then add 1...

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Abstract

Production of high-purity oshaic internal ester is carried out by separating out the high-purity oshaic internal ester from oshaic internal ester crude oil by reduced pressure column chromatography. Its advantages include fast separation, simple operation and recovery and re-utilization.

Description

technical field [0001] The invention relates to a method for extracting medicinal active ingredients, in particular to a method for rapidly preparing high-purity ligustilide. Background technique [0002] In 1960, Japanese scholar Mitsuhashi, H isolated ligustilide from Ligusticum acutilobum for the first time, and named it Ligustilide, which is a light yellow oily liquid with a fragrance and a boiling point of 168-169°C / 6mmHg , insoluble in water, soluble in ethanol, methanol, ether, ethyl acetate, petroleum ether, n-hexane and other organic solvents, the molecular formula is C 12 h 14 o 2 , the molecular weight is 190.24, and the chemical structural formula is as follows: [0003] [0004] The CA index name is 1(3H)-Isobenzofuranone, 3-butylidene-4, 5-dihydro-(9CI) [0005] The three chemical names are: [0006] ①1,5-Cyclohexadiene-1-carboxylic acid, 2-(1-hydroxy-1-pentenyl)-,-lactone (7CI); [0007] ②, Phthalide, 3-butylidene-4, 5-dihydro-(8CI); [0008] ③, 3-Bu...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D307/88
Inventor 钱忠明汪程远杜俊蓉
Owner 钱忠明
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