CN106565795A - Method for extracting alkaloid from bitter gourds - Google Patents
Method for extracting alkaloid from bitter gourds Download PDFInfo
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- CN106565795A CN106565795A CN201610922364.4A CN201610922364A CN106565795A CN 106565795 A CN106565795 A CN 106565795A CN 201610922364 A CN201610922364 A CN 201610922364A CN 106565795 A CN106565795 A CN 106565795A
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- fructus momordicae
- momordicae charantiae
- alkaloid
- filtration
- extracted
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07G—COMPOUNDS OF UNKNOWN CONSTITUTION
- C07G5/00—Alkaloids
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- Organic Chemistry (AREA)
- Medicines Containing Plant Substances (AREA)
- Extraction Or Liquid Replacement (AREA)
Abstract
The invention belongs to the field of natural organic chemistry, and relates to a novel method for extracting bitter gourd alkaloid from bitter gourds. The method is characterized by comprising the following steps of (1), rapidly and uniformly heating tissue cells of the bitter gourds by utilizing a microwave technology, so that liquid in the cells is rapidly vaporized to burst cell walls and effective components are released as soon as possible; and (2), performing gradient elution of the bitter gourd alkaloid by utilizing a macro-porous adsorption resin technology, and performing enrichment and purification, so that the purity of the bitter gourd alkaloid is above 90%. Compared with the traditional process, the method disclosed by the invention has the advantages of being rapid, high-efficiency, safe, energy-saving and the like; the time for an extraction time is greatly shortened while the relatively high extraction rate is kept; furthermore, the content of impurities in extracting solution is reduced; raw material sources are abundant; therefore, the production cost is reduced; and the method is applicable to industrial production.
Description
Technical field
The invention belongs to field of natural organic chemistry, is related to a kind of method that alkaloid is extracted from Fructus Momordicae charantiae.
Background technology
The bright and beautiful Fructus Litchi of Fructus Momordicae charantiae (Momordica Charantia L.) another name, toad, leprosy Fructus Vitis viniferae, balsam pear, red sheep, are calabash
Section's Fructus Momordicae charantiae platymiscium, is a kind of Common Vegetables widely planted in the whole world.《Compendium of Materia Medica》Record Fructus Momordicae charantiae, bitter in the mouth, sweet, nothing
Poison, except pathogenic heat, solves tired, and clear away heart-fire improving eyesight, QI invigorating tonifying YANG.The effect of heat, improving eyesight, removing toxic substances is washed with clearing away summer-heat, in being usually used in treatment
The diseases such as summer-heat, dysentery, cute conjunctivitis pain, carbuncle erysipelas.Subtropical and tropical zones are distributed mainly on, have cultivation in China each department
Training, originates in the ground such as Guangxi, Guangdong, Yunnan, Fujian.
The chemical composition of Fructus Momordicae charantiae mainly has glycoside, lipid, saccharide, flavonoid, saccharide and alkaloidss etc..Life in Fructus Momordicae charantiae
Alkaloids are a class organic compounds containing nitrogens, are bioactive substances critically important in natural medicinal ingredients, with special medicinal valency
Value.
The content of the invention
It is an object of the invention to provide a kind of method that alkaloid is extracted from Fructus Momordicae charantiae, the method is to utilize microwave extracting
The complex technique of technology assisted extraction Fructus Momordicae charantiae alkaloid and enriching and purifying macroporous resin, medicinal material extract is complete, target chemical combination
Thing extraction efficiency is high, and abundant raw material source is easy to get, convenient and simple, and low cost is easy to industrialized production.
For achieving the above object, the technical solution used in the present invention is：
A kind of method that Fructus Momordicae charantiae alkaloid is extracted from Fructus Momordicae charantiae, its step is as follows：
(1) by Fructus Momordicae charantiae cleaning, drying, 40～80 mesh sieves were crushed；
(2) at ambient temperature, the Fructus Momordicae charantiae of crushing is immersed in 60～80% acetone (makes material and extracting liquid volume ratio
For 1: 5～1: 20), soak 30～60min；
(3) by Fructus Momordicae charantiae mixed liquor, in 300～600W, 25～40 DEG C, 30～60min of microwave extraction is recovered by filtration extraction
Liquid；
(4) said extracted liquid is put in the pillar equipped with macroporous adsorbent resin, adds eluant to carry out gradient elution；
(5) potentiometric titrimeter tracing detection is used, each stepwise elution liquid of Fructus Momordicae charantiae alkaloid is collected；
(6) concentrating under reduced pressure, dry Fructus Momordicae charantiae alkaloid.
The inventive method has carried out following optimizations to above-mentioned technical proposal：
Step (3) is carried out that extracting solution is recovered by filtration by following processes：
The first step is filtered：By the mixed liquor after microwave treatment, centrifugal filtration, filtrate, filtration residue are collected respectively.
Second step is filtered：By first step filtration residue 60～80% washing with acetones, centrifugal filtration, collect filter respectively
Liquid, filtration residue.
Macroreticular resin can select D101, HPD700, H-60 or AB-8 type macroporous adsorbent resin in step (4).
Resin first soaks 24h with 95% ethanol, then is 0.5mol/L hydrochloric acid solutions immersion 6h with concentration, and distilled water flushing connects to neutrality
It is 0.5mol/L sodium hydroxide solutions immersion 6h with concentration, and distilled water flushing is to neutrality.Step (3) filtrate is put into
In pillar equipped with macroporous adsorbent resin, respectively with water, 30%, 50% and 80% isopropanol eluant carries out gradient elution.
The inventive method has following technique effect：
(1) rapid, homogeneous heating is carried out to the histiocyte of Fructus Momordicae charantiae using microwave technology, makes the rapid vapour of intracellular fluid
Change, burst cell wall, effective ingredient is discharged as soon as possible, the method has the advantages that fast, efficient, safe, energy-conservation, should
Method substantially reduces the time used by extraction process while higher extraction ratio is kept, and reduces in extracting solution
The content of impurity.
(2) macroporous absorbent resin technology is utilized, gradient elution is carried out to Fructus Momordicae charantiae alkaloid, enriching and purifying makes Fructus Momordicae charantiae alkaloid
Purity reaches more than 90%.Process is simple is easy to operate, and extraction rate is fast.
Specific embodiment
Embodiment 1
(1) by Fructus Momordicae charantiae cleaning, drying, 40 mesh sieves were crushed, weighed 100g；
(2) at ambient temperature, the Fructus Momordicae charantiae of crushing is immersed in 60% acetone (make material be 1: 5 with water volume ratio),
Immersion 30min；
(3) by Fructus Momordicae charantiae mixed liquor, in 300W, 25 DEG C, filtrate, mistake are collected respectively in microwave extraction 30min, centrifugal filtration
Filter residue, by 60% washing with acetone of filtration residue, centrifugal filtration, collects filtrate；
(4) above-mentioned filtrate is put in the pillar equipped with D101 type macroporous adsorbent resins, respectively with water, 10%, 50%
Gradient elution is carried out with 80% acetone eluant；
(5) potentiometric titrimeter tracing detection is used, each stepwise elution liquid of Fructus Momordicae charantiae alkaloid is collected；
(6) concentrating under reduced pressure, dry Fructus Momordicae charantiae alkaloid, the detection of Jing potentiometric titrimeters, alkaloid 90.85%.
Embodiment 2
(1) by Fructus Momordicae charantiae cleaning, drying, 60 mesh sieves were crushed, weighed 100g；
(2) at ambient temperature, the Fructus Momordicae charantiae of crushing is immersed in into 70% acetone (making material be 1: 10 with water volume ratio), leaching
Bubble 45min；
(3) by Fructus Momordicae charantiae mixed liquor, in 400W, 30 DEG C, filtrate, mistake are collected respectively in microwave extraction 40min, centrifugal filtration
Filter residue, by 70% washing with acetone of filtration residue, centrifugal filtration, collects filtrate；
(4) said extracted liquid is put in the pillar equipped with HPD700 type macroporous adsorbent resins, respectively with water, 10%,
50% and 80% acetone eluant carries out gradient elution；
(5) potentiometric titrimeter tracing detection is used, each stepwise elution liquid of Fructus Momordicae charantiae alkaloid is collected；
(6) concentrating under reduced pressure, dry Fructus Momordicae charantiae alkaloid, the detection of Jing potentiometric titrimeters, alkaloid 92.46%.
Embodiment 3
(1) by Fructus Momordicae charantiae cleaning, drying, 70 mesh sieves were crushed, weighed 100g；
(2) at ambient temperature, the Fructus Momordicae charantiae of crushing is immersed in 75% acetone (make material be 1: 15 with water volume ratio),
Immersion 60min；
(3) by Fructus Momordicae charantiae mixed liquor, in 500W, 35 DEG C, filtrate, mistake are collected respectively in microwave extraction 50min, centrifugal filtration
Filter residue, by 75% washing with acetone of filtration residue, centrifugal filtration, collects filtrate；
(4) said extracted liquid is put in the pillar equipped with AB-8 type macroporous adsorbent resins, respectively with water, 10%, 50%
Gradient elution is carried out with 80% acetone eluant；
(5) potentiometric titrimeter tracing detection is used, each stepwise elution liquid of Fructus Momordicae charantiae alkaloid is collected；
(6) concentrating under reduced pressure, dry Fructus Momordicae charantiae alkaloid, the detection of Jing potentiometric titrimeters, alkaloid 92.63%.
Embodiment 4
(1) by Fructus Momordicae charantiae cleaning, drying, 80 mesh sieves were crushed, weighed 100g；
(2) at ambient temperature, the Fructus Momordicae charantiae of crushing is immersed in 80% acetone (make material be 1: 20 with water volume ratio),
Immersion 60min；
(3) by Fructus Momordicae charantiae mixed liquor, in 600W, 40 DEG C, filtrate, mistake are collected respectively in microwave extraction 60min, centrifugal filtration
Filter residue, by 80% washing with acetone of filtration residue, centrifugal filtration, collects filtrate；
(4) said extracted liquid is put in the pillar equipped with H-60 type macroporous adsorbent resins, respectively with water, 10%, 50%
Gradient elution is carried out with 80% acetone eluant；
(5) potentiometric titrimeter tracing detection is used, each stepwise elution liquid of Fructus Momordicae charantiae alkaloid is collected；
(6) concentrating under reduced pressure, dry Fructus Momordicae charantiae alkaloid, the detection of Jing potentiometric titrimeters, alkaloid 93.15%.
Claims (6)
1. it is a kind of from Fructus Momordicae charantiae extract Fructus Momordicae charantiae alkaloid new method, it is characterised in that its step is as follows：
(1) by Fructus Momordicae charantiae cleaning, drying, 40～80 mesh sieves were crushed；
(2) at ambient temperature, the Fructus Momordicae charantiae of crushing is immersed in 60～80% acetone (make material be 1 with extracting liquid volume ratio:
5～1: 20), soak 30～60min；
(3) by Fructus Momordicae charantiae mixed liquor, in 300～600W, 25～40 DEG C, 30～60min of microwave extraction is recovered by filtration extracting solution；
(4) said extracted liquid is put in the pillar equipped with macroporous adsorbent resin, adds eluant to carry out gradient elution；
(5) potentiometric titrimeter tracing detection is used, each stepwise elution liquid of Fructus Momordicae charantiae alkaloid is collected；
(6) concentrating under reduced pressure, dry Fructus Momordicae charantiae alkaloid.
2. the new method that Fructus Momordicae charantiae alkaloid is extracted from Fructus Momordicae charantiae according to claim 1 is characterized in that：Described step (2)
In, Extraction solvent used is 60～80% acetone.
3. the new method that Fructus Momordicae charantiae alkaloid is extracted from Fructus Momordicae charantiae according to claim 1 is characterized in that：Described step (3)
In, it is recovered by filtration as secondary centrifuging filtration, first step filtration：By the mixed liquor after microwave treatment, centrifugal filtration, collected respectively
Filtrate, filtration residue, second step is filtered：By first step filtration residue 60～80% washing with acetones, centrifugal filtration, collect and filter
Liquid.
4. the new method that Fructus Momordicae charantiae alkaloid is extracted from Fructus Momordicae charantiae according to claim 1 is characterized in that：Described step (4)
In, macroreticular resin can select Di01, HPD700, H-60 or AB-8 type macroporous resin.Resin is first soaked with 95% ethanol
Bubble 24h, then be 0.5mol/L hydrochloric acid solutions immersion 6h with concentration, distilled water flushing to neutrality is then 0.5mol/L with concentration
Sodium hydroxide solution soaks 6h, and distilled water flushing is to neutrality.
5. the new method that Fructus Momordicae charantiae alkaloid is extracted from Fructus Momordicae charantiae according to claim 1 is characterized in that：Described step (4)
In, gradient elution is put into filtrate in the pillar equipped with macroporous adsorbent resin, respectively with water, 10%, 50% and 80% acetone
Eluant carries out gradient elution.
6. the new method that Fructus Momordicae charantiae alkaloid is extracted from Fructus Momordicae charantiae according to claim 1 is characterized in that：Described step (5)
In, potentiometric titrimeter tracing detection, it is also possible to thin layer chromatograph.
Priority Applications (1)
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| CN201610922364.4A CN106565795A (en) | 2016-10-17 | 2016-10-17 | Method for extracting alkaloid from bitter gourds |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107050161A (en) * | 2017-05-04 | 2017-08-18 | 中南林业科技大学 | A kind of extraction of one side pin total alkaloid and isolation and purification method |
| CN107970285A (en) * | 2017-12-12 | 2018-05-01 | 长沙理工大学 | A kind of method of total alkaloid in high rhizome of Chinese monkshood of microwave radiation exaraction |
| CN108042620A (en) * | 2017-12-12 | 2018-05-18 | 长沙理工大学 | The extracting method of total alkaloid in a kind of high rhizome of Chinese monkshood |
| CN108851076A (en) * | 2018-06-06 | 2018-11-23 | 李云逸 | A kind of preparation method and application of Bitter Melon P.E |
-
2016
- 2016-10-17 CN CN201610922364.4A patent/CN106565795A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107050161A (en) * | 2017-05-04 | 2017-08-18 | 中南林业科技大学 | A kind of extraction of one side pin total alkaloid and isolation and purification method |
| CN107050161B (en) * | 2017-05-04 | 2020-02-07 | 中南林业科技大学 | Method for extracting, separating and purifying total alkaloids of zanthoxylum dissitum Hemsl |
| CN107970285A (en) * | 2017-12-12 | 2018-05-01 | 长沙理工大学 | A kind of method of total alkaloid in high rhizome of Chinese monkshood of microwave radiation exaraction |
| CN108042620A (en) * | 2017-12-12 | 2018-05-18 | 长沙理工大学 | The extracting method of total alkaloid in a kind of high rhizome of Chinese monkshood |
| CN108042620B (en) * | 2017-12-12 | 2020-04-07 | 长沙理工大学 | Method for extracting total alkaloids in aconitum sinomontanum nakai |
| CN108851076A (en) * | 2018-06-06 | 2018-11-23 | 李云逸 | A kind of preparation method and application of Bitter Melon P.E |
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