CN106380501B - A kind of method that stigmasterol is extracted in the stem from Job's tears - Google Patents
A kind of method that stigmasterol is extracted in the stem from Job's tears Download PDFInfo
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- C07—ORGANIC CHEMISTRY
- C07J—STEROIDS
- C07J9/00—Normal steroids containing carbon, hydrogen, halogen or oxygen substituted in position 17 beta by a chain of more than two carbon atoms, e.g. cholane, cholestane, coprostane
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Abstract
The method that the present invention discloses extraction stigmasterol in a kind of stem from Job's tears, including enzymolysis, ultrasonic wave extraction, saponification, urea column chromatography and crystallization and etc..The method of the present invention can keep the natural characteristic of product, and processing step is few, and operating condition is gentle, and solvent toxicity is low, and production technology safety, extraction efficiency is high, and product purity is up to 99%.
Description
Technical field
The present invention relates to the production preparation field of phytosterol, and in particular to the side of stigmasterol is extracted in a kind of stem from Job's tears
Method.
Background technology
Stigmasterol (stigmaster01), C29H450.Molecular weight is 412, also known as one 5,22 1 diene of beans steroid, one 3B, mono- alcohol or
Mono- one 5,22 1 diene of ethyl cholesteric, one 3 B of 24R, mono- alcohol, is a plant sterols, is widely present in various plants.Stigmasterol
With a variety of pharmacological activity such as significant anti-oxidant, antitumor, cardiovascular disease resistants, and the starting material of steroid medicine is synthesized,
There is application in industries such as medicine, food and chemical industry.In recent years, as the discovery of new steroid drugs, the development of production, production are advised
The expansion of mould, raw material requirement also gradually increase；On the other hand due to unreasonable digging, shortage of resources is caused, soap in plant
Salidroside content declines, and international market supply and demand contradiction is occurred, and how to obtain the stigmasterol of more higher purity is stigmasterol research
One important directions.
Job's tears (Coix lachryma-jobiL. it is) grass family (Gramineae) Coix, slightly sweet flavor, cold nature,
There is invigorating the spleen, tonifying lung, heat-clearing, dampness removing, be known as the good reputation of " king of tonic ".The chemical composition of Job's tears is ground at present
Study carefully it is fewer, and it is more concentrate on coix seed, the document report in terms of its pharmacology activity research is also few, biological action thing
Matter basis is indefinite, causes its application clinically to be limited to.Research has shown that Job's tears stem contains steroidal, polysaccharide, flavones, has
The chemical composition such as machine acid, sheath matter, triterpene, therefore how research extracts stigmasterol from Job's tears and more Job's tears can be made full use of to provide
Source.
The Chinese patent of Publication No. CN1374319A discloses a kind of side that stigmasterol is extracted from mixed phytosterin
Method, this method are enriched with stigmasterol with solvent method, and master operation is filtered including water-bath dissolving, cooling growing the grain, insulation, the use of its solvent
Normal heptane and dichloroethanes mixed solvent, normal heptane：Dichloroethanes=l ﹕ 1~2, l ﹕ 1.5~1.8 are optimal.Wherein mixed plant steroid
The mass volume ratio of alcohol and solvent (m/V) is optimal for 3~5,1 ﹕ 3.5~4.5 of l ﹕.Water-bath solution temperature is 70~75 DEG C.Water-bath
20~25 DEG C are down to, when keeping constant temperature growing the grain 12~24 small.After every time, last extract is pressed into same process
Recrystallized, repeated 2-6 times next time, number of repetition determines the content of extraction stigmasterol.Filtrate is through low-temperature treatment, temperature
For -10 DEG C, steroid alcohol and solvent is recycled.This method solvent consumption is big, and production waste material is more, and energy expenditure is big, and sterol yield is low.
The content of the invention
To solve the above-mentioned problems, the present invention provides a kind of method that stigmasterol is extracted in stem from Job's tears, side of the invention
Method can keep the natural characteristic of product, and processing step is few, and operating condition is gentle, and solvent toxicity is low, production technology safety, extraction
Efficient, product purity is up to 99%.
The present invention is achieved through the following technical solutions：
A kind of method that stigmasterol is extracted in stem from Job's tears, comprises the following steps：
（1）Enzymolysis：Job's tears stem is put into pulverizer and crushes to obtain Job's tears stem coarse powder, cellulose is added in Job's tears stem coarse powder
Enzyme and pectase, are then dissolved in the water of 1~3 times of coarse powder weight, and 5~8h is digested at 30~50 DEG C, filter, dry, obtain enzyme
Solve Job's tears stem powder；
（2）Ultrasonic wave extraction：Enzymolysis Job's tears stem powder and absolute ethyl alcohol are added in ultrasonic equipment and carry out ultrasonic wave extraction,
Filtering, obtains extracting solution, extracting solution is put into Rotary Evaporators and is concentrated under reduced pressure, obtain extractum A；
（3）Saponification：Extractum A is dissolved in the ethanol solution of the sodium hydroxide of 10~50wt%, be sufficiently stirred, 40~70
1~3h of saponification at DEG C, reaction solution are neutralized with hydrochloric acid to neutrality, then with saturated salt solution and petroleum ether extraction, aqueous phase discarded, stone
Oily ether is mutually concentrated under reduced pressure with Rotary Evaporators, obtains medicinal extract B；
（4）Urea column chromatography：Urea is dissolved in loaded solvent, then adds silica gel, urea is supported on silica gel, is removed
Unload solvent, and stationary phase is made；Stationary phase is filled into column, then by medicinal extract B upper props, is eluted with eluant, eluent injection chromatographic column
Flowed out to no stigmasterol, collect eluent, by thin-layer chromatography tracing detection, merged and stigmasterol standard items Rf values are identical washes
De- liquid, is concentrated to give stigmasterol crude product；
（5）Crystallization：Stigmasterol crude product is dissolved in methanol, is crystallized, filtering, obtains stigmasterol sterling.
Preferably, the weight that cellulase and pectase described above add is the 0.1~1% of Job's tears stem coarse powder weight, fine
The plain enzyme of dimension and pectase are mixed with arbitrary proportion.
Preferably, the solid-liquid ratio 1 of enzymolysis Job's tears stem powder and absolute ethyl alcohol described above:10~15.
Preferably, multi-frequency ultrasonic described above is extracted as double frequency or Three-frequency ultrasonic extraction, is carried using dual-frequency ultrasonic wave
When taking, the frequencies of two kinds of ultrasonic waves is 20~40kHz and 20~60kHz, and power is 50~200W, 100~500W, extraction time
For 20~40min；When being extracted using Three-frequency ultrasonic, the frequencies of three kinds of ultrasonic waves is 20~40kHz, 20~60kHz, 500~
1000kHz, power is 50~200W, 100~500W, 500~2000W, and extraction time is 10~25min.
Preferably, the ethanol solution of the sodium hydroxide of 10~50wt% of the above and the solid-liquid ratio of extractum A are 3~10:
1。
Preferably, loaded solvent described above is absolute ethyl alcohol or 75~95% ethanol-water solution.
Preferably, the mass ratio of urea and silica gel described above is 1~10:3.
Preferably, eluant, eluent described above is that volume ratio is 10:1~2:1 benzene-ethyl acetate solution.
Compared with prior art, advantages of the present invention and have the beneficial effect that：
1st, the present invention adds pectase in Job's tears stem coarse powder and cellulase is digested, and can destroy the thin of Job's tears stem
Cell wall, makes stigmasterol be easier to be suggested out, after filtering, moreover it is possible to removes the water-solubility impurities such as par-tial polysaccharide, improves beans steroid
The recovery rate of alcohol.
2nd, the present invention is extracted using multi-frequency ultrasonic, can significantly shorten extraction time, is reduced solvent dosage, is improved
Rate, and obtained extracting solution quality is good, it is easily refined.
3rd, the present invention is isolated and purified using urea column chromatography, and easy to operate, cost is low, and urea chromatographic column can repeat
Utilize.
4th, method of the invention can keep the natural characteristic of product, and processing step is few, and operating condition is gentle, solvent toxicity
Low, production technology safety, extraction efficiency is high, and product purity is up to 99%.
5th, the present invention extracts stigmasterol by the use of agricultural wastes Job's tears stem as raw material, can reduce the row of agricultural wastes
Put, increase the utilization rate of coix plant, improve farmers' income, preserve the ecological environment.
Embodiment
Embodiment 1
A kind of method that stigmasterol is extracted in stem from Job's tears, comprises the following steps：
（1）Enzymolysis：Job's tears stem is put into pulverizer and crushes to obtain Job's tears stem coarse powder, cellulose is added in Job's tears stem coarse powder
Enzyme and pectase, are then dissolved in the water of 1 times of coarse powder weight, and 8h is digested at 50 DEG C, filter, dry, obtain enzymolysis Job's tears stem powder；
The weight that its cellulase and pectase add is the 0.1% of Job's tears stem coarse powder weight, the weight ratio of cellulase and pectase
For 2:1；
（2）Ultrasonic wave extraction：Enzymolysis Job's tears stem powder and absolute ethyl alcohol are added the double ultrasonic waves of progress in ultrasonic equipment to carry
Take, digest the solid-liquid ratio 1 of Job's tears stem powder and absolute ethyl alcohol:10, the frequency of two kinds of ultrasonic waves is 20kHz and 40kHz, and power is
50W, 100W, extraction time 20min；Filtering, obtains extracting solution, extracting solution is put into Rotary Evaporators and is concentrated under reduced pressure,
Obtain extractum A；
（3）Saponification：Extractum A is dissolved in the ethanol solution of the sodium hydroxide of 10wt%, the second of the sodium hydroxide of 10wt%
Alcoholic solution and the solid-liquid ratio of extractum A are 3:1, it is sufficiently stirred, saponification 1h, reaction solution are neutralized with hydrochloric acid at 40~50 DEG C
Property, then mutually it is concentrated under reduced pressure, is obtained with Rotary Evaporators with saturated salt solution and petroleum ether extraction, aqueous phase discarded, petroleum ether
Medicinal extract B；
（4）Urea column chromatography：Urea is dissolved in absolute ethyl alcohol, then adds silica gel, urea is supported on silica gel, is urinated
The mass ratio of element and silica gel is 1:3, absolute ethyl alcohol is removed, stationary phase is made；Stationary phase is filled into column, then by medicinal extract B upper props, is used
Volume ratio is 10:1 benzene-ethyl acetate solution injection chromatographic column is eluted to no stigmasterol outflow, is collected eluent, is passed through
Thin-layer chromatography tracing detection, merges the eluent identical with stigmasterol standard items Rf values, is concentrated to give stigmasterol crude product；
（5）Crystallization：Stigmasterol crude product is dissolved in methanol, is crystallized, filtering, obtains stigmasterol sterling.
The stigmasterol sterling that the present embodiment obtains is detected using HPLC, purity 99.0%.
Embodiment 2
A kind of method that stigmasterol is extracted in stem from Job's tears, comprises the following steps：
（1）Enzymolysis：Job's tears stem is put into pulverizer and crushes to obtain Job's tears stem coarse powder, cellulose is added in Job's tears stem coarse powder
Enzyme and pectase, are then dissolved in the water of 3 times of coarse powder weight, and 5h is digested at 30 DEG C, filter, dry, obtain enzymolysis Job's tears stem powder；
The weight that its cellulase and pectase add is the 1% of Job's tears stem coarse powder weight, and the weight ratio of cellulase and pectase is
2:1；
（2）Ultrasonic wave extraction：Enzymolysis Job's tears stem powder and absolute ethyl alcohol are added in ultrasonic equipment and carry out Three-frequency ultrasonic
Extraction, digests the solid-liquid ratio 1 of Job's tears stem powder and absolute ethyl alcohol:15, the frequencies of three kinds of ultrasonic waves is 40kHz, 60kHz,
1000kHz, power 200W, 500W, 2000W, extraction time 10min；Filtering, obtains extracting solution, extracting solution is put into rotation
It is concentrated under reduced pressure in evaporimeter, obtains extractum A；
（3）Saponification：Extractum A is dissolved in the ethanol solution of the sodium hydroxide of 50wt%, the second of the sodium hydroxide of 50wt%
Alcoholic solution and the solid-liquid ratio of extractum A are 10:1, it is sufficiently stirred, saponification 3h, reaction solution are neutralized with hydrochloric acid at 50~70 DEG C
Property, then mutually it is concentrated under reduced pressure, is obtained with Rotary Evaporators with saturated salt solution and petroleum ether extraction, aqueous phase discarded, petroleum ether
Medicinal extract B；
（4）Urea column chromatography：Urea is dissolved in 75% ethanol-water solution, then adds silica gel, is supported on urea
On silica gel, the mass ratio of urea and silica gel is 10:3,75% ethanol-water solution is removed, stationary phase is made；Stationary phase is filled into column,
Then it is 2 with volume ratio by medicinal extract B upper props:1 benzene-ethyl acetate solution injection chromatographic column is eluted to no stigmasterol stream
Go out, collect eluent, by thin-layer chromatography tracing detection, merge the eluent identical with stigmasterol standard items Rf values, be concentrated to give
Stigmasterol crude product；
（5）Crystallization：Stigmasterol crude product is dissolved in methanol, is crystallized, filtering, obtains stigmasterol sterling.
The stigmasterol sterling that the present embodiment obtains is detected using HPLC, purity 99.2%.
Embodiment 3
A kind of method that stigmasterol is extracted in stem from Job's tears, comprises the following steps：
（1）Enzymolysis：Job's tears stem is put into pulverizer and crushes to obtain Job's tears stem coarse powder, cellulose is added in Job's tears stem coarse powder
Enzyme and pectase, are then dissolved in the water of 2 times of coarse powder weight, and 6h is digested at 40 DEG C, filter, dry, obtain enzymolysis Job's tears stem powder；
The weight that its cellulase and pectase add is the 0.5% of Job's tears stem coarse powder weight, the weight ratio of cellulase and pectase
For 1:1；
（2）Ultrasonic wave extraction：Enzymolysis Job's tears stem powder and absolute ethyl alcohol are added in ultrasonic equipment and carry out dual-frequency ultrasonic wave
Extraction, digests the solid-liquid ratio 1 of Job's tears stem powder and absolute ethyl alcohol:12, the frequency of two kinds of ultrasonic waves is 35kHz and 55kHz, and power is
100W, 200W, extraction time 30min；Filtering, obtains extracting solution, extracting solution is put into Rotary Evaporators and is concentrated under reduced pressure,
Obtain extractum A；
（3）Saponification：Extractum A is dissolved in the ethanol solution of the sodium hydroxide of 30wt%, the second of the sodium hydroxide of 30wt%
Alcoholic solution and the solid-liquid ratio of extractum A are 6:1, it is sufficiently stirred, saponification 2h, reaction solution are neutralized with hydrochloric acid at 50~60 DEG C
Property, then mutually it is concentrated under reduced pressure, is obtained with Rotary Evaporators with saturated salt solution and petroleum ether extraction, aqueous phase discarded, petroleum ether
Medicinal extract B；
（4）Urea column chromatography：Urea is dissolved in 95% ethanol-water solution, then adds silica gel, is supported on urea
On silica gel, the mass ratio of urea and silica gel is 5:3,95% ethanol-water solution is removed, stationary phase is made；Stationary phase is filled into column,
Then it is 5 with volume ratio by medicinal extract B upper props:1 benzene-ethyl acetate solution injection chromatographic column is eluted to no stigmasterol stream
Go out, collect eluent, by thin-layer chromatography tracing detection, merge the eluent identical with stigmasterol standard items Rf values, be concentrated to give
Stigmasterol crude product；
（5）Crystallization：Stigmasterol crude product is dissolved in methanol, is crystallized, filtering, obtains stigmasterol sterling.
The stigmasterol sterling that the present embodiment obtains is detected using HPLC, purity 99.1%.
Embodiment 4
A kind of method that stigmasterol is extracted in stem from Job's tears, comprises the following steps：
（1）Enzymolysis：Job's tears stem is put into pulverizer and crushes to obtain Job's tears stem coarse powder, cellulose is added in Job's tears stem coarse powder
Enzyme and pectase, are then dissolved in the water of 2 times of coarse powder weight, and 6h is digested at 50 DEG C, filter, dry, obtain enzymolysis Job's tears stem powder；
The weight that its cellulase and pectase add is the 0.8% of Job's tears stem coarse powder weight, the weight ratio of cellulase and pectase
For 1:3；
（2）Ultrasonic wave extraction：Enzymolysis Job's tears stem powder and absolute ethyl alcohol are added in ultrasonic equipment and carry out Three-frequency ultrasonic
Extraction, digests the solid-liquid ratio 1 of Job's tears stem powder and absolute ethyl alcohol:12, the frequencies of three kinds of ultrasonic waves is 20kHz, 40kHz, 500kHz,
Power is 50,100W, 500W, extraction time 25min.Filtering, obtains extracting solution, extracting solution is put into Rotary Evaporators and is carried out
It is concentrated under reduced pressure, obtains extractum A；
（3）Saponification：Extractum A is dissolved in the ethanol solution of the sodium hydroxide of 20wt%, the second of the sodium hydroxide of 20wt%
Alcoholic solution and the solid-liquid ratio of extractum A are 6:1, it is sufficiently stirred, saponification 1h, reaction solution are neutralized with hydrochloric acid at 50~60 DEG C
Property, then mutually it is concentrated under reduced pressure, is obtained with Rotary Evaporators with saturated salt solution and petroleum ether extraction, aqueous phase discarded, petroleum ether
Medicinal extract B；
（4）Urea column chromatography：Urea is dissolved in 80% ethanol-water solution, then adds silica gel, urea is supported on silicon
On glue, the mass ratio of urea and silica gel is 6:3,80% ethanol-water solution is removed, stationary phase is made；Stationary phase is filled into column, so
It is 3 with volume ratio afterwards by medicinal extract B upper props:1 benzene-ethyl acetate solution injection chromatographic column is eluted to no stigmasterol outflow,
Eluent is collected, by thin-layer chromatography tracing detection, merges the eluent identical with stigmasterol standard items Rf values, is concentrated to give beans steroid
Alcohol crude product；
（5）Crystallization：Stigmasterol crude product is dissolved in methanol, is crystallized, filtering, obtains stigmasterol sterling.
The stigmasterol sterling that the present embodiment obtains is detected using HPLC, purity 99.2%.
Embodiment 5
A kind of method that stigmasterol is extracted in stem from Job's tears, comprises the following steps：
（1）Enzymolysis：Job's tears stem is put into pulverizer and crushes to obtain Job's tears stem coarse powder, cellulose is added in Job's tears stem coarse powder
Enzyme and pectase, are then dissolved in the water of 3 times of coarse powder weight, and 8h is digested at 40 DEG C, filter, dry, obtain enzymolysis Job's tears stem powder；
The weight that its cellulase and pectase add is the 0.6% of Job's tears stem coarse powder weight, the weight ratio of cellulase and pectase
For 1:1；
（2）Ultrasonic wave extraction：Enzymolysis Job's tears stem powder and absolute ethyl alcohol are added in ultrasonic equipment and carry out dual-frequency ultrasonic wave
Extraction, digests the solid-liquid ratio 1 of Job's tears stem powder and absolute ethyl alcohol:12, the frequency of two kinds of ultrasonic waves is 40kHz and 20kHz, and power is
200W, 500W, extraction time 25min；Filtering, obtains extracting solution, extracting solution is put into Rotary Evaporators and is concentrated under reduced pressure,
Obtain extractum A；
（3）Saponification：Extractum A is dissolved in the ethanol solution of the sodium hydroxide of 20wt%, the second of the sodium hydroxide of 20wt%
Alcoholic solution and the solid-liquid ratio of extractum A are 8:1, it is sufficiently stirred, saponification 2h, reaction solution are neutralized with hydrochloric acid at 50~60 DEG C
Property, then mutually it is concentrated under reduced pressure, is obtained with Rotary Evaporators with saturated salt solution and petroleum ether extraction, aqueous phase discarded, petroleum ether
Medicinal extract B；
（4）Urea column chromatography：Urea is dissolved in absolute ethyl alcohol, then adds silica gel, urea is supported on silica gel, is urinated
The mass ratio of element and silica gel is 5:3, absolute ethyl alcohol is removed, stationary phase is made；Stationary phase is filled into column, then by medicinal extract B upper props, is used
Volume ratio is 5:1 benzene-ethyl acetate solution injection chromatographic column is eluted to no stigmasterol outflow, is collected eluent, is passed through
Thin-layer chromatography tracing detection, merges the eluent identical with stigmasterol standard items Rf values, is concentrated to give stigmasterol crude product；
（5）Crystallization：Stigmasterol crude product is dissolved in methanol, is crystallized, filtering, obtains stigmasterol sterling.
The stigmasterol sterling that the present embodiment obtains is detected using HPLC, purity 99.3%.
Claims (5)
1. the method for stigmasterol is extracted in a kind of stem from Job's tears, it is characterised in that comprise the following steps：
（1）Enzymolysis：Job's tears stem is put into pulverizer and crushes to obtain Job's tears stem coarse powder, in Job's tears stem coarse powder add cellulase and
Pectase, is then dissolved in the water of 1~3 times of coarse powder weight, and 5~8h is digested at 30~50 DEG C, filters, dry, obtains the enzymolysis heart of a lotus seed
Job's tears stem powder；
（2）Ultrasonic wave extraction：Enzymolysis Job's tears stem powder and absolute ethyl alcohol are added in ultrasonic equipment and carry out ultrasonic wave extraction, mistake
Filter, obtains extracting solution, extracting solution is put into Rotary Evaporators and is concentrated under reduced pressure, obtain extractum A；
（3）Saponification：Extractum A is dissolved in the ethanol solution of the sodium hydroxide of 10~50wt%, be sufficiently stirred, at 40~70 DEG C
1~3h of saponification, reaction solution are neutralized with hydrochloric acid to neutrality, then with saturated salt solution and petroleum ether extraction, aqueous phase discarded, petroleum ether
Mutually it is concentrated under reduced pressure with Rotary Evaporators, obtains medicinal extract B；The ethanol solution and extractum A of the sodium hydroxide of the 10~50wt%
Solid-liquid ratio be 3~10:1；
（4）Urea column chromatography：Urea is dissolved in loaded solvent, then adds silica gel, urea is supported on silica gel, is removed negative
Solvent is carried, stationary phase is made；Stationary phase is filled into column, then by medicinal extract B upper props, carries out being eluted to nothing with eluant, eluent injection chromatographic column
Stigmasterol flows out, and collects eluent, by thin-layer chromatography tracing detection, merges the elution identical with stigmasterol standard items Rf values
Liquid, is concentrated to give stigmasterol crude product；The mass ratio of the urea and silica gel is 1~10:3；The eluant, eluent is that volume ratio is 10:1
~2:1 benzene-ethyl acetate solution；
（5）Crystallization：Stigmasterol crude product is dissolved in methanol, is crystallized, filtering, obtains stigmasterol sterling.
2. in the stem according to claim 1 from Job's tears extract stigmasterol method, it is characterised in that the cellulase and
The weight that pectase adds is the 0.1~1% of Job's tears stem coarse powder weight, and cellulase and pectase are mixed with arbitrary proportion.
3. the method for stigmasterol is extracted in the stem according to claim 1 from Job's tears, it is characterised in that the enzymolysis Job's tears stem
The solid-liquid ratio 1 of powder and absolute ethyl alcohol:10~15.
4. the method for stigmasterol is extracted in the stem according to claim 1 from Job's tears, it is characterised in that the ultrasonic wave extraction
Extracted for double frequency or Three-frequency ultrasonic, when being extracted using dual-frequency ultrasonic wave, the frequencies of two kinds of ultrasonic waves for 20~40kHz and 20~
60kHz, power are 50~200W, 100~500W, and extraction time is 20~40min；When being extracted using Three-frequency ultrasonic, three kinds
The frequency of ultrasonic wave for 20~40kHz, 20~60kHz, 500~1000kHz, power for 50~200W, 100~500W, 500~
2000W, extraction time are 10~25min.
5. the method for stigmasterol is extracted in the stem according to claim 1 from Job's tears, it is characterised in that the loaded solvent is
Absolute ethyl alcohol or 75~95% ethanol-water solution.
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| CN107625774A (en) * | 2017-08-30 | 2018-01-26 | 右江民族医学院 | Application and its extracting method of the cycloartenol in antineoplastic in Job's tears cauline leaf |
| CN107383141A (en) * | 2017-08-30 | 2017-11-24 | 右江民族医学院 | The method that the ketone of 24 ethyl cholestane of (20R) 22E, 4,22 diene 3 is extracted in Job's tears cauline leaf |
| CN107652349A (en) * | 2017-08-30 | 2018-02-02 | 右江民族医学院 | A kind of method that cycloartenol is isolated and purified in the cauline leaf from Job's tears |
| CN107513091A (en) * | 2017-08-30 | 2017-12-26 | 右江民族医学院 | There is the compound and its extracting method of antitumor activity in Job's tears cauline leaf |
| CN110642962B (en) * | 2019-09-03 | 2022-03-22 | 南昌大学 | Separation and purification method of hybrid bean pectin polysaccharide |
| CN113512084B (en) * | 2021-03-26 | 2023-09-26 | 右江民族医学院 | Method for extracting stigmasterol from coix seed stems and leaves by combining ultrasonic countercurrent with biological enzyme |
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