CN105213755A - From Fritillary flower, the method for fritillaria total alkaloids is extracted with supercritical fluid - Google Patents
From Fritillary flower, the method for fritillaria total alkaloids is extracted with supercritical fluid Download PDFInfo
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- CN105213755A CN105213755A CN201510676691.1A CN201510676691A CN105213755A CN 105213755 A CN105213755 A CN 105213755A CN 201510676691 A CN201510676691 A CN 201510676691A CN 105213755 A CN105213755 A CN 105213755A
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Abstract
The invention discloses the method extracting fritillaria total alkaloids with supercritical fluid from Fritillary flower, Fritillary flower powder is in supercritical extraction reactor, and extraction temperature is 30 ~ 50 DEG C, CO
2fluid pressure is 20 ~ 40MPa, entrainer ethanol flow velocity 0.2 ~ 0.5ml/min, extraction time 1 ~ 3h, use methanol absorption again, then macroporous resin chromatographic column chromatography is used, ethanol elution, the Fritillary flower eluent concentrating under reduced pressure of 95% ethanol elution, dry 24h under 105 DEG C of conditions again, obtains the light yellow Fritillary flower extract that Main Ingredients and Appearance is fritillaria total alkaloids.The method step is simple, and extraction time shortens, and extraction efficiency is higher, and per kilogram Fritillary flower can extract fritillaria total alkaloids about 17g, and purity is also higher, and fritillaria total alkaloids weight accounts for more than 60%, and is made full use of by Fritillary flower, improves the value of plantation Bulbus Fritillariae Uninbracteatae.
Description
Technical field
The present invention relates to the extraction of fritillaria total alkaloids, be specifically related to the method extracting fritillaria total alkaloids with supercritical fluid from Fritillary flower.
Background technology
Bulbus Fritillariae Uninbracteatae be Liliaceae (
liliaceae) Fritillaria (
fritillaria) plant, traditional medicinal part is its bulb, and Bulbus Fritillariae Uninbracteatae cures mainly typhoid fever dysphoria with smothery sensation, cough only gas, settling five organs, sharp bone marrow, expectorant profit cardiopulmonary, has the effect such as antiinflammatory detumescent, treatment pain furuncle and phyma poison concurrently.Nineteen eighty-two version " Chinese medicinal herbal " is stated: have " effect such as clearing heat and moistening lung, preventing phlegm from forming and stopping coughing, eliminating stagnation function ", clinical in phlegm-heat cough, the vexed expectorant of face, controls scrofula and sore swollen toxin.The main medicinal component of Bulbus Fritillariae Uninbracteatae is Bulbus Fritillariae Uninbracteatae alkaloid, comprises Peimine, Peiminine etc., and Bulbus Fritillariae Uninbracteatae alkaloid has free radical scavenging activity.From Bulbus Fritillariae Uninbracteatae, the method for extract total alkaloids is traditional organic solvent extraction at present, if notification number is the patent of invention of CN1146425, disclose and first Bulbus Fritillariae Uninbracteatae is used 95% alcohol reflux, after adding 2% salt water dissolution, use petroleum ether, ethyl acetate extraction successively repeatedly, use chloroform extraction again, obtain fritillaria total alkaloids.But traditional method extraction is complicated, and need repeatedly extract, extraction time is long, and extraction efficiency is low, and is using Bulbus Fritillariae Uninbracteatae bulb as raw material, and Fritillary flower is rotted afield mostly, is not used.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind ofly extracts the method extracting fritillaria total alkaloids with supercritical fluid from Fritillary flower simple, the time is short, efficiency is high.
The present invention solves the problems of the technologies described above adopted technical scheme: the method extracting fritillaria total alkaloids with supercritical fluid from Fritillary flower, and its step is as follows:
A, the air-dry rear pulverizing of the fresh Fritillary flower of being won the same day, cross 45 ~ 60 mesh sieves, obtain Fritillary flower powder, loads in supercritical extraction reactor;
B, in supercritical extraction reactor, extraction temperature is 30 ~ 50 DEG C, CO
2fluid pressure is 20 ~ 40MPa, entrainer ethanol flow velocity 0.2 ~ 0.5ml/min, extraction time 1 ~ 3h, after extract methanol absorption absorbing liquid, wherein after the extraction of 100g Fritillary flower powder with 20 ~ 30ml methanol absorption;
C, absorbing liquid D101 type macroporous resin chromatographic column chromatography, Tomography Velocity is two bed volume flow velocitys per hour, first with distillation washing chromatographic column after chromatography, be washed till effluent colourless, then chromatographic column is washed with mass percentage concentration 50% ethanol of 2 bed volumes, use mass percentage concentration 95% ethanol elution of 8 bed volumes again, the eluent collecting 95% ethanol elution obtains Fritillary flower eluent, Fritillary flower eluent is evaporated near dry under 450 ~ 500Pa condition, dry 24h under 105 DEG C of conditions again, obtain the light yellow Fritillary flower extract that Main Ingredients and Appearance is fritillaria total alkaloids.
Compared with prior art, the invention has the advantages that the method extracting fritillaria total alkaloids with supercritical fluid from Fritillary flower, Fritillary flower powder is in supercritical extraction reactor, and extraction temperature is 30 ~ 50 DEG C, CO
2fluid pressure is 20 ~ 40MPa, entrainer ethanol flow velocity 0.2 ~ 0.5ml/min, extraction time 1 ~ 3h, use methanol absorption again, then macroporous resin chromatographic column chromatography is used, ethanol elution, the Fritillary flower eluent concentrating under reduced pressure of 95% ethanol elution, dry 24h under 105 DEG C of conditions again, obtains the light yellow Fritillary flower extract that Main Ingredients and Appearance is fritillaria total alkaloids.The method step is simple, and extraction time shortens, and extraction efficiency is higher, and per kilogram Fritillary flower can extract fritillaria total alkaloids about 17g, and purity is also higher, and fritillaria total alkaloids weight accounts for more than 60%, and is made full use of by Fritillary flower, improves the value of plantation Bulbus Fritillariae Uninbracteatae.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described in further detail.
Embodiment 1
Fresh Fritillary flower (can be Bulbus Fritillariae Thunbergii, Bulbus Fritillariae Cirrhosae etc.) the air-dry rear pulverizing of being won the same day, cross 45 ~ 60 mesh sieves, obtain Fritillary flower powder, weigh 50g, and load in supercritical extraction reactor, extraction temperature is 38 DEG C, CO
2fluid pressure is 33MPa, entrainer ethanol flow velocity 0.25ml/min, extraction time 2h, extract obtains absorbing liquid with after 10 ~ 15ml methanol absorption, absorbing liquid D101 type macroporous resin chromatographic column chromatography, effluent is washed with distilled water to colourless with two bed volume flow velocitys per hour, then mass percentage concentration 50% washing with alcohol of 2 bed volumes is used, use mass percentage concentration 95% ethanol elution of 8 bed volumes again, collect the Fritillary flower eluent of 95% ethanol elution, Fritillary flower is evaporated near dry under 450 ~ 500Pa condition, dry 24h under 105 DEG C of conditions, obtain lurid Fritillary flower extract 0.85g, adopting the UV-VIS spectrophotometry of visualization Bromocresol green to measure fritillaria total alkaloids content in every gram of extract is 613mg.
Embodiment 2
Substantially the same manner as Example 1, difference is extraction temperature is 30 DEG C, CO
2fluid pressure is 20MPa, entrainer ethanol flow velocity 0.20ml/min, extraction time 3h, and extract obtains absorbing liquid with after 30ml methanol absorption, and Fritillary flower extract 0.84g, in every gram of extract, fritillaria total alkaloids content is 608mg.
Embodiment 3
Substantially the same manner as Example 1, difference is extraction temperature is 50 DEG C, CO
2fluid pressure is 40MPa, entrainer ethanol flow velocity 0.50ml/min, extraction time 1h, and extract obtains absorbing liquid with after 20ml methanol absorption, and Fritillary flower extract 0.82g, in every gram of extract, fritillaria total alkaloids content is 601mg.
Claims (3)
1. from Fritillary flower, extract the method for fritillaria total alkaloids with supercritical fluid, it is characterized in that step is as follows:
A, the air-dry rear pulverizing of the fresh Fritillary flower of being won the same day, cross 45 ~ 60 mesh sieves, obtain Fritillary flower powder, loads in supercritical extraction reactor;
B, in supercritical extraction reactor, extraction temperature is 30 ~ 50 DEG C, CO
2fluid pressure is 20 ~ 40MPa, entrainer ethanol flow velocity 0.2 ~ 0.5ml/min, extraction time 1 ~ 3h, obtains absorbing liquid after extract methanol absorption, wherein needs with 20 ~ 30ml methanol absorption after the extraction of 100g Fritillary flower powder;
C, absorbing liquid D101 type macroporous resin chromatographic column chromatography, Tomography Velocity is two bed volume flow velocitys per hour, first with distillation washing chromatographic column after chromatography, be washed till effluent colourless, then chromatographic column is washed with mass percentage concentration 50% ethanol of 2 bed volumes, use mass percentage concentration 95% ethanol elution of 8 bed volumes again, the eluent collecting 95% ethanol elution obtains Fritillary flower eluent, Fritillary flower eluent is evaporated near dry under 450 ~ 500Pa condition, dry 24h under 105 DEG C of conditions again, obtain the light yellow Fritillary flower extract that Main Ingredients and Appearance is fritillaria total alkaloids.
2. supercritical fluid as claimed in claim 1 extracts the method for fritillaria total alkaloids from Fritillary flower, it is characterized in that in step b, and extraction temperature is 38 DEG C, CO
2fluid pressure is 33MPa, entrainer ethanol flow velocity 0.25ml/min, extraction time 2h.
3. supercritical fluid as claimed in claim 1 extracts the method for fritillaria total alkaloids from Fritillary flower, it is characterized in that in step b, and extraction temperature is 30 DEG C, CO
2fluid pressure is 20MPa, entrainer ethanol flow velocity 0.20ml/min, extraction time 3h.
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| CN201510676691.1A CN105213755A (en) | 2015-10-20 | 2015-10-20 | From Fritillary flower, the method for fritillaria total alkaloids is extracted with supercritical fluid |
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| CN201510676691.1A CN105213755A (en) | 2015-10-20 | 2015-10-20 | From Fritillary flower, the method for fritillaria total alkaloids is extracted with supercritical fluid |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2017185281A1 (en) * | 2016-04-28 | 2017-11-02 | 朱小涛 | Fritillary flower extractive preparation method |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01238582A (en) * | 1988-03-18 | 1989-09-22 | Hikari Kaneko | Steroid alkaloid compound |
| CN102210803A (en) * | 2011-05-18 | 2011-10-12 | 北京中医药大学 | Extraction and enrichment method of fritillaria total alkaloids |
-
2015
- 2015-10-20 CN CN201510676691.1A patent/CN105213755A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01238582A (en) * | 1988-03-18 | 1989-09-22 | Hikari Kaneko | Steroid alkaloid compound |
| CN102210803A (en) * | 2011-05-18 | 2011-10-12 | 北京中医药大学 | Extraction and enrichment method of fritillaria total alkaloids |
Non-Patent Citations (1)
| Title |
|---|
| 张良等: "CO2超临界萃取川贝母游离生物碱工艺研究", 《西华大学学报自然科学版》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2017185281A1 (en) * | 2016-04-28 | 2017-11-02 | 朱小涛 | Fritillary flower extractive preparation method |
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