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Method for rapidly separating catalpol from rehmanniae by use of triple column chromatography technology

A column chromatography and Rehmannia glutinosa technology, applied in chemical instruments and methods, organic chemistry, sugar derivatives, etc., can solve the problems of catalpol loss, high operating cost, and heavy environmental burden, so as to avoid serious losses and low operating cost , the effect of less capital investment

Active Publication Date: 2014-01-22
JIANGSU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The above method has the following deficiencies, which are difficult to meet the requirements of large-scale production of catalpol: one, the silica gel column is used for separation, and the packing cannot be reused, and the polarity of catalpol is large, and serious dead adsorption causes a large amount of loss of catalpol; 2. Petroleum ether, ethyl acetate, chloroform, methanol, acetone and other toxic, flammable, and controlled reagents are used in the purification process, which has a heavy environmental burden and high management costs; 3. Before column chromatography, the extract needs to be concentrated, Preliminary impurity removal and other treatments consume a lot of manpower, time and energy; Fourth, membrane separation technologies such as microfiltration, ultrafiltration, and nanofiltration have large capital investment, high operating costs, and poor quality of final products

Method used

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  • Method for rapidly separating catalpol from rehmanniae by use of triple column chromatography technology
  • Method for rapidly separating catalpol from rehmanniae by use of triple column chromatography technology
  • Method for rapidly separating catalpol from rehmanniae by use of triple column chromatography technology

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Take 0.1kg of commercially available Rehmannia glutinosa medicinal materials, dry at below 60℃, crush, pass through a 20-mesh sieve, collect the fine powder, add 1.2L of water, heat to a slight boiling, decoct 2 times, 2h each time, filter, and collect the filtrate , Get the water decoction; weigh 1 kg of D101 type macroporous adsorption resin, wet the column with ethanol and carry out conventional pretreatment, load the water decoction into the D101 type macroporous adsorption resin column, elution with water, the flow rate is 1L·h -1 , The elution volume is 6L, collect the water eluate; weigh 1kg of H103 type macroporous adsorption resin, pack the column with ethanol wet method and perform conventional pretreatment, load the water eluate into the H103 type macroporous adsorption resin column, Elute with water at a flow rate of 1L·h -1 , The elution volume is 6L, discard the water eluent and use 30% ethanol ( v / v ) Perform elution with a flow rate of 2L·h -1 , The eluti...

Embodiment 2

[0032] Take 0.1kg of commercially available raw dihuang decoction pieces, dry at below 60℃, smash, pass through a 20-mesh sieve, collect the fine powder, add 1L of water, heat to a slight boiling, decoct 2 times, 2h each time, filter, and collect the filtrate , Get the water decoction; weigh 0.5 kg of D101 type macroporous adsorption resin, use ethanol wet method to pack the column and carry out conventional pretreatment, load the water decoction into D101 type macroporous adsorption resin column, elution with water, flow rate 0.25L·h -1 , The elution volume is 2L, collect the water eluate; weigh 0.5 kg of H103 type macroporous adsorption resin, pack the column with ethanol wet method and perform conventional pretreatment, and load the water eluate into the H103 type macroporous adsorption resin column , Eluted with water at a flow rate of 0.25L·h -1 , The elution volume is 2L, discard the water eluent, and replace with 10% ethanol ( v / v ) Perform elution at a flow rate of 0.5L...

Embodiment 3

[0034] Take 0.5 kg of commercially available Rehmannia glutinosa medicinal materials, dry at below 60°C, crush, pass through a 20-mesh sieve, collect the fine powder, add 4L of water, heat to a slight boiling, decoct 3 times, 1h each time, filter, collect the filtrate, Obtain the water decoction; weigh 5 kg of D101 type macroporous adsorption resin, use ethanol wet method to pack the column and carry out conventional pretreatment, load the water decoction into the D101 type macroporous adsorption resin column, elution with water, the flow rate is 4L ·H -1 , The elution volume is 30L, collect the water eluate; weigh 4kg of H103 type macroporous adsorption resin, pack the column with ethanol wet method and carry out routine pretreatment, load the water eluent into the H103 type macroporous adsorption resin column, Elute with water at a flow rate of 2L·h -1 , The elution volume is 20L, discard the water eluent, and replace with 10% ethanol ( v / v ) Perform elution with a flow rate ...

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Abstract

The invention relates to a method for rapidly separating catalpol from rehmanniae by use of triple column chromatography technology, belonging to the technical field of traditional Chinese medicines. D101 type macroporous adsorption resin, H103 type macroporous adsorption resin and activated carbon, which are commonly used as chromatographic paddings, are sequentially used in separating and purifying processes, so that catalpol with the purity higher than 95% can be obtained from the rehmanniae. Compared with the prior art, the method has the following advantages that the adopted three paddings can be repeatedly used after being subjected to the conventional regeneration treatment, the capital investment is low and the operating cost is low; only ethanol and water are used in the separating and purifying processes, so that environmental requirement is met; and extracting solution and macroporous resin eluant do not need to be subjected to concentration and impurity removal before the triple column chromatography is performed, the operation steps are greatly simplified, the operating time is shortened and the manpower and energy consumption is reduced.

Description

technical field [0001] The invention relates to a method for rapidly separating catalpol, in particular to a method for rapidly separating catalpol from traditional Chinese medicine rehmannia glutinosa by triple column chromatography, and belongs to the technical field of traditional Chinese medicine. [0002] Background technique [0003] Rehmanniae Radix (Rehmanniae Radix) is a perennial herb of Scrophulariaceae (Scrophulariaceae) Rehmannia glutinosa Libosch.) dry tuber root, sweet and cold in nature, Guixin, liver and kidney meridian, has the effect of clearing away heat and cooling blood, nourishing yin and promoting body fluid, and is mainly used to treat blood entering the camp due to heat, warm toxin and spotting, vomiting blood and epistaxis. Pharmacological experiments have proved that the chemical components of iridoid glycosides are the main medicinal material basis of rehmannia glutinosa, especially catalpol has outstanding anti-cancer, neuroprotective, hypogly...

Claims

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Application Information

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IPC IPC(8): C07H17/04C07H1/08
Inventor 杨欢王海艳顾芹英沈玉萍夏国华
Owner JIANGSU UNIV
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