CN109400599A - A kind of extracting method of tetrahydropalmatine - Google Patents
A kind of extracting method of tetrahydropalmatine Download PDFInfo
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- CN109400599A CN109400599A CN201811440811.8A CN201811440811A CN109400599A CN 109400599 A CN109400599 A CN 109400599A CN 201811440811 A CN201811440811 A CN 201811440811A CN 109400599 A CN109400599 A CN 109400599A
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- tetrahydropalmatine
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D455/00—Heterocyclic compounds containing quinolizine ring systems, e.g. emetine alkaloids, protoberberine; Alkylenedioxy derivatives of dibenzo [a, g] quinolizines, e.g. berberine
- C07D455/03—Heterocyclic compounds containing quinolizine ring systems, e.g. emetine alkaloids, protoberberine; Alkylenedioxy derivatives of dibenzo [a, g] quinolizines, e.g. berberine containing quinolizine ring systems directly condensed with at least one six-membered carbocyclic ring, e.g. protoberberine; Alkylenedioxy derivatives of dibenzo [a, g] quinolizines, e.g. berberine
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Abstract
The invention discloses a kind of extracting methods of tetrahydropalmatine.Method includes the following steps: rhizoma corydalis is placed in vinegar after impregnating 30~40min by (1), add water, boils to solution whole distilled-to-dryness, crush；(2) ultrasonic alcohol extracting；(3) filtrate is extracted with petroleum ether-ethyl acetate mixed liquor, merges organic phase, be concentrated under reduced pressure, lye is then added, after mixing evenly, stood filtering, collect solid product；(4) solid product obtained by step (3) is dissolved, and be added into non-polar macroporous resin, then washing is eluted with chloroform-methanol mixed liquor, and collect merging eluent again；(5) it is spin-dried for eluent, is dissolved, then is saturated with water ether and extracts 2~3 times, merges organic phase, is evaporated.The tetrahydropalmatine with high-purity in high yield can be prepared in the method for the present invention.
Description
Technical field
The invention belongs to natural drug extractive technique fields, and in particular to a kind of extracting method of tetrahydropalmatine.
Background technique
Rhizoma corydalis is Papaveraceae (Papaveraceae) Genus Corydalis rhizoma corydalis (Corydalis yanhusuo
W.T.Wang ex Z.Y.Su et C.Y.Wu) dry tuber, be born in wilderness thick grass or the gentle slope border of low altitude area.Rhizoma corydalis
Acrid flavour, hardship, warm-natured, return heart, liver, the spleen channel；The effect of recording promoting blood circulation to remove blood stasis, regulating qi-flowing for relieving pain according to ancient medical book, for chest side of body,
Epigastric pain, menostasis promoting menstruation, postpartum stasis, tumbling and swelling etc.；Modern medicine, which shows rhizoma corydalis also, has good analgesia, calmness
With the pharmacological action of hypnosis.
Yanhusu main composition is alkaloid, and the alkaloid contained is mainly tertiary amine, Amine quarter alkaloid, and its
In the tetrahydropalmatine that plays a major role also belong to tertiary amine Alkaloid, but existing technique prepares tetrahydropalmatine in extraction
When, often have that impurity is more, the problem of purity deficiency.
Summary of the invention
For above-mentioned deficiency in the prior art, the present invention provides a kind of extracting method of tetrahydropalmatine, can effectively solve
When certainly prior art extracts tetrahydropalmatine, yield and the lower problem of purity.
To achieve the above object, the technical solution adopted by the present invention to solve the technical problems is:
A kind of extracting method of tetrahydropalmatine, comprising the following steps:
(1) rhizoma corydalis is placed in vinegar after impregnating 30~40min, adds water, boils to solution whole distilled-to-dryness, drying and crushing
It is 10~50 mesh at partial size；The weight ratio of rhizoma corydalis and vinegar is 3~5:1；
(2) powder particle is added in 70~95% ethyl alcohol, adjusting pH value is 3~5, and in 40~60 DEG C, 300~500W is super
Sound extracts 60~90min, and filtrate is collected in filtering；Wherein, the solid-liquid ratio of powder particle and ethyl alcohol is 1~3:20~40；
(3) it is extracted filtrate 2~3 times with petroleum ether-ethyl acetate mixed liquor, merges organic phase, be concentrated under reduced pressure, be then added
Lye stands 30~50min after mixing evenly, and solid product is collected in filtering；Wherein, the volume ratio of petroleum ether and ethyl acetate
For 1~3:4~8；
(4) solid product obtained by step (3) is dissolved, and be added into non-polar macroporous resin, washing 2~3 times, then
It is eluted again with chloroform-methanol mixed liquor, and collects merging eluent；The volume ratio of chloroform and methanol is 3~5:0.5~1；
(5) it is spin-dried for eluent, is dissolved, then is saturated with water ether and extracts 2~3 times, merges organic phase, is evaporated.
Further, the weight ratio of rhizoma corydalis and vinegar is 5:1 in step (1).
Further, the detailed process extracted in step (2) are as follows:
Powder particle is added in 80% ethyl alcohol, adjusting pH value is 3.5, in 40 DEG C, 350W ultrasonic extraction 60min.
Further, the volume ratio of petroleum ether and ethyl acetate is 1:5 in step (3).
Further, lye is ammonium hydroxide in step (3).
Further, the volume ratio of chloroform and methanol is 3:1 in step (4).
Further, non-polar macroporous resin is H103 non-polar macroporous resin in step (4).
Of the invention is effective are as follows:
1, it is essentially all to exist in plant in a salt form due to alkaloid, cooks the rhizoma corydalis not crushed with vinegar
Stem tuber, can be so that it becomes the acylate of small molecule can effectively promote the recovery rate of alkaloid convenient for extracting.
2, it is 3~5 in pH value, in 40~60 DEG C, under conditions of 300~500W, is extracted and passed through with 70~95% EtOH Sonicates
Yanhusuo obtained after vinegar cooks, the effective components such as alkaloid therein can be extracted, ensure that as far as possible
Its recovery rate.
3, obtained tetrahydropalmatine can will be extracted using petroleum ether-ethyl acetate mixed liquor to extract as far as possible
Come, meanwhile, it can also be separated with big molecular impurities such as carbohydrates, ensure that the yield of the tetrahydropalmatine being obtained by extraction and pure
Degree.
4, by the precipitation and separation of lye, further tetrahydropalmatine is separated with remaining alkaloid component, then passes through
It is adsorbed by non-polar macroporous resin, can further remove the stronger alkaloid of depolarization, then elute and separate through chloroform-methanol,
It is finally saturated with water ether extraction again, the yield and purity for extracting obtained tetrahydropalmatine is effectively guaranteed.
Specific embodiment
A specific embodiment of the invention is described below, in order to facilitate understanding by those skilled in the art this hair
It is bright, it should be apparent that the present invention is not limited to the ranges of specific embodiment, for those skilled in the art,
As long as various change is in the spirit and scope of the present invention that the attached claims limit and determine, these variations are aobvious and easy
See, all are using the innovation and creation of present inventive concept in the column of protection.
Embodiment 1
A kind of extracting method of tetrahydropalmatine, which comprises the following steps:
(1) rhizoma corydalis is placed in vinegar after impregnating 30min, adds water, boils to solution whole distilled-to-dryness, drying and crushing granulating
Diameter is 40 mesh；Wherein, the weight ratio of rhizoma corydalis and vinegar is 5:1；
(2) powder particle is added in 80% ethyl alcohol, adjusting pH value is 3.5, in 40 DEG C, 350W ultrasonic extraction 60min, mistake
Filtrate is collected in filter；Wherein, the solid-liquid ratio of powder particle and ethyl alcohol is 3:20；
(3) it is extracted filtrate 3 times with petroleum ether-ethyl acetate mixed liquor, merges organic phase, be concentrated under reduced pressure, ammonia is then added
Water stands 50min after mixing evenly, and solid product is collected in filtering；Wherein, the volume ratio of petroleum ether and ethyl acetate is 1:5；
(4) solid product obtained by step (3) is dissolved, and be added into H103 non-polar macroporous resin, washing 2 times, so
It is eluted again with chloroform-methanol mixed liquor afterwards, and collects merging eluent；Wherein, the volume ratio of chloroform and methanol is 3:1；
(5) it is spin-dried for eluent, is dissolved, then is saturated with water ether and extracts 3 times, merges organic phase, is evaporated up to rhizoma corydalis second
Element.
Embodiment 2
A kind of extracting method of tetrahydropalmatine, which comprises the following steps:
(1) rhizoma corydalis is placed in vinegar and is impregnated, after impregnating 40min, added water, boil to solution whole distilled-to-dryness, xeraphium
Being broken into partial size is 10 mesh；Wherein, the weight ratio of rhizoma corydalis and vinegar is 3:1；
(2) powder particle is added in 70% ethyl alcohol, adjusting pH value is 5, in 60 DEG C, 500W ultrasonic extraction 90min, mistake
Filtrate is collected in filter；Wherein, the solid-liquid ratio of powder particle and ethyl alcohol is 1:40；
(3) it is extracted filtrate 2 times with petroleum ether-ethyl acetate mixed liquor, merges organic phase, be concentrated under reduced pressure, ammonia is then added
Water stands 30min after mixing evenly, and solid product is collected in filtering；Wherein, the volume ratio of petroleum ether and ethyl acetate is 1:8；
(4) solid product obtained by step (3) is dissolved, and be added into H103 non-polar macroporous resin, washing 2 times, so
It is eluted again with chloroform-methanol mixed liquor afterwards, and collects merging eluent；The volume ratio of the chloroform and methanol is 3:0.5；
(5) it is spin-dried for eluent, is dissolved, then is saturated with water ether and extracts 3 times, merges organic phase and is evaporated up to rhizoma corydalis second
Element.
Embodiment 3
A kind of extracting method of tetrahydropalmatine, which comprises the following steps:
(1) rhizoma corydalis is placed in vinegar and is impregnated, after impregnating 40min, added water, boil to solution whole distilled-to-dryness, xeraphium
Being broken into partial size is 50 mesh；The weight ratio of the rhizoma corydalis and vinegar is 4:1；
(2) powder particle is added in 95% ethyl alcohol, adjusting pH value is 3, in 55 DEG C, 300W ultrasonic extraction 60min, mistake
Filtrate is collected in filter；Wherein, the solid-liquid ratio of powder particle and ethyl alcohol is 3:40；
(3) it is extracted filtrate 3 times with petroleum ether-ethyl acetate mixed liquor, merges organic phase, be concentrated under reduced pressure, ammonia is then added
Water stands 40min after mixing evenly, and solid product is collected in filtering；Wherein, the volume ratio of petroleum ether and ethyl acetate is 3:8；
(4) solid product obtained by step (3) is dissolved, and be added into H103 non-polar macroporous resin, washing 3 times, so
It is eluted again with chloroform-methanol mixed liquor afterwards, and collects merging eluent；Wherein, the volume ratio of chloroform and methanol is 5:0.5；
(5) it is spin-dried for eluent, is dissolved, then is saturated with water ether and extracts 2~3 times, merges organic phase, is evaporated up to rhizoma corydalis
B prime.
Comparative example 1
Compared with Example 1, lack step (1), remaining process is same as Example 1.
Comparative example 2
Compared with Example 1, lack step (4), remaining process is same as Example 1.
Comparative example 3
Compared with Example 1, lack step (1) and step (4), remaining process is same as Example 1.Detection
The yield of obtained tetrahydropalmatine and pure is extracted with Examples 1 to 3 and comparative example 1~3 is detected under the same terms
Degree, the result is shown in tables 1.
The yield and purity of 1 tetrahydropalmatine of table
From the data in table 1, it can be seen that the yield and purity of the tetrahydropalmatine that Examples 1 to 3 is prepared are superior to comparative example 1
~3, wherein again be best with embodiment 1, and comparative example 1 is compared with better than comparative example 2 and comparative example 3, and what comparative example 3 was prepared
The yield and purity of product are minimum, thus illustrate, only under the cooperation of process and parameter that the method for the present invention refers to, could make
The standby tetrahydropalmatine obtained with high yield and high-purity.
Claims (7)
1. a kind of extracting method of tetrahydropalmatine, which comprises the following steps:
(1) rhizoma corydalis is placed in vinegar after impregnating 30~40min, adds water, boils to solution whole distilled-to-dryness, drying and crushing granulating
Diameter is 10~50 mesh；The weight ratio of the rhizoma corydalis and vinegar is 3~5:1；
(2) powder particle is added in 70~95% ethyl alcohol, adjusting pH value is 3~5, and in 40~60 DEG C, 300~500W ultrasound is mentioned
60~90min is taken, is filtered, filtrate is collected；Wherein, the solid-liquid ratio of the powder particle and ethyl alcohol is 1~3:20~40；
(3) it is extracted filtrate 2~3 times with petroleum ether-ethyl acetate mixed liquor, merges organic phase, be concentrated under reduced pressure, alkali is then added
Liquid stands 30~50min after mixing evenly, and solid product is collected in filtering；Wherein, the volume of the petroleum ether and ethyl acetate
Than for 1~3:4~8；
(4) solid product obtained by step (3) is dissolved, and be added into non-polar macroporous resin, washed 2~3 times, then use again
Chloroform-methanol mixed liquor elution, and collect merging eluent；The volume ratio of the chloroform and methanol is 3~5:0.5~1；
(5) it is spin-dried for eluent, is dissolved, then is saturated with water ether and extracts 2~3 times, merges organic phase, is evaporated.
2. the extracting method of tetrahydropalmatine according to claim 1, which is characterized in that prolong described in step (1) recklessly
The weight ratio of rope and vinegar is 5:1.
3. the extracting method of tetrahydropalmatine according to claim 1, which is characterized in that extracted described in step (2)
Detailed process are as follows:
Powder particle is added in 80% ethyl alcohol, adjusting pH value is 3.5, in 40 DEG C, 350W ultrasonic extraction 60min.
4. the extracting method of tetrahydropalmatine according to claim 1, which is characterized in that petroleum described in step (3)
The volume ratio of ether and ethyl acetate is 1:5.
5. the extracting method of tetrahydropalmatine according to claim 1, which is characterized in that lye described in step (3)
For ammonium hydroxide.
6. the extracting method of tetrahydropalmatine according to claim 1, which is characterized in that chloroform described in step (4)
Volume ratio with methanol is 3:1.
7. the extracting method of tetrahydropalmatine according to claim 1, which is characterized in that non-pole described in step (4)
Property macroreticular resin be H103 non-polar macroporous resin.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112939861A (en) * | 2019-12-10 | 2021-06-11 | 中国医学科学院药物研究所 | Benzylisoquinoline alkaloid with human carboxylesterase 2 inhibition effect and application thereof |
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| US3849561A (en) * | 1964-10-20 | 1974-11-19 | S Naruto | Anti-peptic ulcer substance from corydalis tubers |
| US5242926A (en) * | 1992-05-28 | 1993-09-07 | National Science Council Of Republic Of China | Therapeutic composition for treating hyperthyroidism |
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| CN106176981A (en) * | 2016-08-26 | 2016-12-07 | 江苏七O七天然制药有限公司 | A kind of extracting method of vinegar Rhizoma Corydalis |
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2018
- 2018-11-29 CN CN201811440811.8A patent/CN109400599A/en active Pending
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|---|---|---|---|---|
| US3849561A (en) * | 1964-10-20 | 1974-11-19 | S Naruto | Anti-peptic ulcer substance from corydalis tubers |
| US5242926A (en) * | 1992-05-28 | 1993-09-07 | National Science Council Of Republic Of China | Therapeutic composition for treating hyperthyroidism |
| CN103191198A (en) * | 2013-04-03 | 2013-07-10 | 中国中医科学院中药研究所 | Rhizoma corydalis extract as well as preparation method and use thereof |
| CN104415573A (en) * | 2013-09-10 | 2015-03-18 | 中国科学院大连化学物理研究所 | Method for classifying and preparing tertiary amine alkaloid and quaternary ammonium alkaloid from corydalis extract |
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Non-Patent Citations (1)
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| 李玉山: "延胡索乙素的制备工艺及药理作用研究进展", 《解放军药学学报》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112939861A (en) * | 2019-12-10 | 2021-06-11 | 中国医学科学院药物研究所 | Benzylisoquinoline alkaloid with human carboxylesterase 2 inhibition effect and application thereof |
| CN112939861B (en) * | 2019-12-10 | 2023-06-09 | 中国医学科学院药物研究所 | Benzyl isoquinoline alkaloid with human carboxylesterase 2 inhibition effect and application thereof |
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Application publication date: 20190301 |