CN102992940B - Method for extracting delta-elemene - Google Patents
Method for extracting delta-elemene Download PDFInfo
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- CN102992940B CN102992940B CN201210554755.7A CN201210554755A CN102992940B CN 102992940 B CN102992940 B CN 102992940B CN 201210554755 A CN201210554755 A CN 201210554755A CN 102992940 B CN102992940 B CN 102992940B
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Abstract
The invention provides a method for extracting delta-elemene. The method comprises the following steps of: (1) carrying out ordinary rectification by using zedoary turmeric oil of which the delta-elemene content is more than 1.5% as the raw material, wherein the vacuum degree inside a rectifying column is 150-300Pa and the rectification ratio is 2:1, and collecting distillate with a temperature of 128-135 DEG C; (2) carrying out primary fine rectification by using the distillate obtained in the step (1) as the raw material, subsequently carrying out the secondary fine rectification by using the obtained distillate as the raw material, wherein the rectification ratios are different (4:1 in the primary fine rectification, and 6:1 in the secondary fine rectification) and the vacuum degrees in precise rectifying columns are both set as 50-150Pa, and collecting distillate with a temperature of 120-125 DEG C; and (3) carrying out axial compression high pressure column separation by using the obtained distillate in the step (2) as the raw material. According to the method, a method of primary ordinary rectification, secondary precise rectification and axial compression high pressure column separation is utilized, delta-elemene with high purity is obtained, and the difficult problem that no reference substances of the delta-elemene are available for years is solved.
Description
Technical field
The invention belongs to pharmaceutical technology sectors, be specifically related to a kind of extracting method of δ-Elemenum.
Background technology
Elemenum is the effective ingredient in zedoary turmeric oil, and containing δ-Elemenum, beta-elemene, γ-Elemenum three kinds of isomerss, be national two class PTS, it is extensively approved with obvious anticancer effect and lower toxic side effect.
Being extracted in " preparation method and the composition thereof that take beta-elemene as the cancer therapy drug of effective constituent " (CN 1200266A) of beta-elemene is on the books, but due to the isomers that γ-Elemenum and δ-Elemenum are beta-elemenes, therefore when preparing beta-elemene, γ-Elemenum and δ-Elemenum also can together be separated, need to adopt comparatively accurate extraction means just can be isolated.At present report be there is no to the extraction of γ-Elemenum and δ-Elemenum.
In addition, owing to there is no suitable separating and extracting method, do not have reference substance to use when detecting the content of γ-Elemenum and δ-Elemenum, thus cause the content of γ-Elemenum and δ-Elemenum in pharmaceutical cpd to estimate and can not be quantitative.
Summary of the invention
The object of this invention is to provide a kind of extracting method of δ-Elemenum.
Specifically, the extracting method of δ-Elemenum of the present invention, is characterized in that, comprise the steps:
(1) take δ-Examination of Content of Elemene as the zedoary turmeric oil of more than 1.5% be raw material, the heating kettle being placed in rectifying tower starts rectifying, and the vacuum tightness controlled in rectifying column is 150 ~ 300Pa, and fractionation, than being 2:1, collects the fraction that temperature is 128 ~ 135 DEG C;
(2) with step (1) gained fraction for raw material, be placed in the heating kettle of precise rectification tower, carry out precise distillation, the vacuum tightness controlled in precise distillation post is 50 ~ 150Pa, and fractionation, than being 4:1, collects the fraction that temperature is 120 ~ 125 DEG C;
(3) with step (2) gained fraction for raw material, be placed in the heating kettle of precise rectification tower, carry out secondary precise distillation, the vacuum tightness controlled in precise distillation post is 50 ~ 150Pa, and fractionation, than being 6:1, collects the fraction that temperature is 120 ~ 125 DEG C;
(4) with step (3) gained fraction be raw material enter axial compression high-pressure post be separated: use tlc silica gel is for sorbent material, with the sherwood oil of boiling point 30 ~ 60 DEG C for eluent, wash-out is carried out with the elution speed of 12L/h, collecting δ-Elemenum purity is the elutriant of more than 92%, reclaim the sherwood oil in elutriant, obtain δ-Elemenum.
In the present invention, the rectifying column be preferably as follows:
Conventional distillation post: be highly 140cm, internal diameter is 3.5cm, with the stainless steel net volume of diameter 3mm × long 3mm for filler, post effect is more than 40 stage number;
Precise distillation post: be highly 150cm, internal diameter is 3.5cm, with the stainless steel net volume of diameter 2mm × long 2mm for filler, post effect is more than 60 stage number.
In addition, the axial compression high-pressure post be preferably as follows: specification is diameter 10cm × high 100cm, and column pressure processed is 50MPa, uses 100 order silica gel.
The present invention adopts conventional distillation, a secondary precise distillation to be separated with axial compression high-pressure post the method combined, highly purified δ-Elemenum (its average purity can reach 92 ~ 98%) can be obtained, solve δ-Examination of Content of Elemene detect without reference substance can a difficult problem.When the weighting material that particularly axial compression high-pressure post uses in being separated is through the silica gel of 115 ~ 125 DEG C of activation, owing to improve the absorption property of silica gel, effectively can removes the impurity in cut further, improve the purity of δ-Elemenum.
Accompanying drawing explanation
Fig. 1 is the extraction schema of δ-Elemenum.
Embodiment
The present invention is described in detail below in conjunction with embodiment; but the following examples are only the present invention's preferably embodiment; protection scope of the present invention is not limited thereto; anyly be familiar with those skilled in the art in the technical scope that the present invention discloses; be equal to according to technical scheme of the present invention and inventive concept thereof and replace or change, all should be encompassed within protection scope of the present invention.
Embodiment 1
(1) the zedoary turmeric oil 2300ml of 1.8% is about for raw material with δ-Examination of Content of Elemene, be placed in rectifying tower heating kettle and start rectifying, controlling rectifying column (is highly 140cm, internal diameter is 3.5cm, with the stainless steel net volume of diameter 3mm × long 3mm for filler, post effect is more than 40 stage number) in vacuum tightness be 180Pa, fractionation, than for 2:1, collects the fraction that temperature is 128 ~ 135 DEG C.
(2) with step (1) gained fraction for raw material, be placed in the heating kettle of precise rectification tower, carry out precise distillation, controlling precise distillation post (is highly 150cm, internal diameter is 3.5cm, with the stainless steel net volume of diameter 2mm × long 2mm for filler, post effect be more than 60 stage number) in vacuum tightness be 100Pa, fractionation, than being 4:1, collects the fraction that temperature is 120 ~ 125 DEG C.
(3) with step (2) gained fraction for raw material, be placed in the heating kettle of precise rectification tower, carry out secondary precise distillation, controlling precise distillation post (is highly 150cm, internal diameter is 3.5cm, with the stainless steel net volume of diameter 2mm × long 2mm for filler, post effect be more than 60 stage number) in vacuum tightness be 100Pa, fractionation, than being 6:1, collects the fraction that temperature is 120 ~ 125 DEG C.
This step gained fraction is carried out to the purity detecting of δ-Elemenum, result shows that the purity of δ-Elemenum reaches more than 90%.
(4) be that raw material carries out axial compression high-pressure post (diameter 10cm × high 100cm with step (3) gained fraction, use 100 order silica gel, column pressure processed is 50MPa, use the sherwood oil of front boiling point 30 ~ 60 DEG C with the flow velocity of 1000ml/min by filled silica gel compacting) be separated: with the sherwood oil of boiling point 30 ~ 60 DEG C for eluent, elution speed is 200ml/min(12L/h), every 200ml is a wash-out section.δ in each wash-out section-Elemenum purity is detected.
(5) δ-Elemenum purity of collecting step (4) gained is the elutriant of more than 95%, and with the sherwood oil in decompression Rotary Evaporators removing elutriant, pressure is 100MPa, obtains δ-Elemenum.
In the above-mentioned methods, the purity detecting of δ-Elemenum adopts capillary gas chromatography.Chromatographiccondition is as follows.
Chromatographic column: model PEG-20M, diameter 0.32mm, long 60m, thickness 0.25 μm (the Dalian Chemistry and Physics Institute)
Detector: flame ionization ditector (Shimadzu Corporation's production)
Gas chromatograph: GC-14C gas chromatograph (Shimadzu Corporation's production)
Chromatographic working station: N2000 chromatographic working station (Zhejiang University)
Chromatographic condition: column temperature is first set to 120 DEG C, keep 5 minutes, be then warmed up to 200 DEG C with the speed program of 2 DEG C/minute, the temperature of injection port and detector is set to 230 DEG C respectively.Open the gas source switch of nitrogen (60ml/min) and hydrogen (40ml/min) and air (400ml/min), splitting ratio 1:20, open gas chromatograph and chromatographic working station, after nitrogen, air-stable, igniting, after its baseline stability, gets δ-Elemenum sample 1 μ l sample introduction, respectively normalization method automatic integration is pressed to the area of the chromatographic peak of δ-Elemenum and the chromatographic peak of impurity, obtain the purity of δ-Elemenum.
Claims (3)
1. an extracting method for δ-Elemenum, is characterized in that, comprises the steps:
(1) take δ-Examination of Content of Elemene as the zedoary turmeric oil of more than 1.5% be raw material, the heating kettle being placed in rectifying tower starts rectifying, and the vacuum tightness controlled in rectifying column is 150 ~ 300Pa, and fractionation, than being 2:1, collects the fraction that temperature is 128 ~ 135 DEG C;
(2) with step (1) gained fraction for raw material, be placed in the heating kettle of precise rectification tower, carry out precise distillation, the vacuum tightness controlled in precise distillation post is 50 ~ 150Pa, and fractionation, than being 4:1, collects the fraction that temperature is 120 ~ 125 DEG C;
(3) with step (2) gained fraction for raw material, be placed in the heating kettle of precise rectification tower, carry out secondary precise distillation, the vacuum tightness controlled in precise distillation post is 50 ~ 150Pa, and fractionation, than being 6:1, collects the fraction that temperature is 120 ~ 125 DEG C;
(4) with step (3) gained fraction be raw material enter axial compression high-pressure post be separated: use tlc silica gel is for sorbent material, with the sherwood oil of boiling point 30 ~ 60 DEG C for eluent, wash-out is carried out with the elution speed of 12L/h, collecting δ-Elemenum purity is the elutriant of more than 92%, reclaim the sherwood oil in elutriant, obtain δ-Elemenum.
2. extracting method according to claim 1, is characterized in that, the height of described rectifying column is 140cm, and internal diameter is 3.5cm, and with the stainless steel net volume of diameter 3mm × long 3mm for filler, post effect is more than 40 stage number; The height of described precise distillation post is 150cm, and internal diameter is 3.5cm, and with the stainless steel net volume of diameter 2mm × long 2mm for filler, post effect is more than 60 stage number.
3. extracting method according to claim 1, is characterized in that, the specification of described axial compression high-pressure post is diameter 10cm × high 100cm, and column pressure processed is 50MPa, uses 100 order silica gel.
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| CN201210554755.7A CN102992940B (en) | 2012-12-19 | 2012-12-19 | Method for extracting delta-elemene |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105797417B (en) * | 2016-04-29 | 2018-07-06 | 大连德泽药业有限公司 | Monitor fractionating device, method and system that temperature prepares high-purity fraction |
| CN110903156A (en) * | 2019-11-18 | 2020-03-24 | 贵州景诚制药有限公司 | Method for separating and purifying β -elemene, gamma-elemene and delta-elemene |
| CN115554282B (en) * | 2022-11-01 | 2023-09-29 | 健民药业集团股份有限公司 | Application of delta-elemene in preparation of medicine for resisting hyperplasia of mammary glands |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1200266A (en) * | 1997-04-14 | 1998-12-02 | 中国科技开发院医药科技开发所 | Method for preparing anti-cancer medicine using beta-elemene as main effective ingredient, and components of the medicine |
| CN1554331A (en) * | 2003-12-23 | 2004-12-15 | 英属维尔京群岛远大国际有限公司 | High nurity beta-elemene medicine and its preparing method |
| CN101229989A (en) * | 2008-01-08 | 2008-07-30 | 沈阳万爱普利德医药科技有限公司 | Method for preparing high-purity beta-elemene by citronella oil byproduct |
| CN101402543A (en) * | 2008-11-14 | 2009-04-08 | 沈阳万爱普利德医药科技有限公司 | Beta-elemi alkene bulk medicament and method of preparing its preparations |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1200266A (en) * | 1997-04-14 | 1998-12-02 | 中国科技开发院医药科技开发所 | Method for preparing anti-cancer medicine using beta-elemene as main effective ingredient, and components of the medicine |
| CN1554331A (en) * | 2003-12-23 | 2004-12-15 | 英属维尔京群岛远大国际有限公司 | High nurity beta-elemene medicine and its preparing method |
| CN101229989A (en) * | 2008-01-08 | 2008-07-30 | 沈阳万爱普利德医药科技有限公司 | Method for preparing high-purity beta-elemene by citronella oil byproduct |
| CN101402543A (en) * | 2008-11-14 | 2009-04-08 | 沈阳万爱普利德医药科技有限公司 | Beta-elemi alkene bulk medicament and method of preparing its preparations |
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