CN109824509A - The extracting method of radix achyranthis bidentatae leaf Linoleic acid - Google Patents
The extracting method of radix achyranthis bidentatae leaf Linoleic acid Download PDFInfo
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Abstract
The invention discloses a kind of extracting methods of radix achyranthis bidentatae leaf Linoleic acid, belong to linoleic extractive technique field.Technical solution of the present invention main points are as follows: by radix achyranthis bidentatae leaf dried and crushed, after n-hexane extraction, through saponification process, carry out urea clathrate at low temperature to get linoleic acid is arrived.The extracting method of radix achyranthis bidentatae leaf Linoleic acid provided by the present invention, easy to operate, linoleic acid recovery rate is good, and agents useful for same is cheap, from a wealth of sources, is easily obtained, and the development and utilization for linoleic process study and radix achyranthis bidentatae leaf provide new approaches.
Description
Technical field
The invention belongs to linoleic extractive technique fields, and in particular to a kind of extracting method of radix achyranthis bidentatae leaf Linoleic acid.
Background technique
Multinomial data shows, linoleic acid can be significantly reduced that blood fat is horizontal, thin vessels in softening, mitigates blood
Pressure increases blood circulation, restores the effects of nervous function indirectly, the sufferer rate of cardiovascular and cerebrovascular disease can be reduced, especially to hat
The prevention and treatment of the diseases such as heart trouble, atherosclerosis, senile obesity has positive meaning.
Numerous studies find radix achyranthis bidentatae rich in the ingredients such as triterpene saponin, polysaccharide, alkaloids, recently again some researches show that
Wherein it is rich in lubricant component.Achyranthes Amaranthaceae is herbaceos perennial, is China's commonly one of large Chinese medicine, mainly
In Henan, Sichuan one with plantation.In order to further excavate the practical value of radix achyranthis bidentatae leaf, need to provide a kind of easy to operate and efficiency compared with
High linoleic extracting method.
Linoleic acid is a kind of unsaturated fatty acid, and extracting method is more, and wherein urea inclusion is legal because of required equipment
Simply, it is easy to operate it is easy to learn, cost is relatively low and gained unsaturated fatty acid purity is higher and is widely applied.In addition, urine
Plain inclusion method is operated at low temperature, can utmostly save linoleic bioactivity, will not be because isomerization occurs
Linoleic nutrition and physiological activity are lost with polymerization reaction.Therefore, urea adduct method is pure for linoleic acid large-scale separation
The ideal method of change.
Summary of the invention
The present invention has extracted linoleic acid using urea adduct method from radix achyranthis bidentatae leaf for the first time, and has easy to operate, extraction
The advantages that rate is good, with high purity, has widened the research range of radix achyranthis bidentatae leaf, deeply develops for it and provides new thinking.
Linoleic purpose is extracted to realize, the present invention adopts the following technical solutions: the extraction side of radix achyranthis bidentatae leaf Linoleic acid
Method, it is characterised in that specific steps are as follows:
Step S1: it by radix achyranthis bidentatae leaf dried and crushed at radix achyranthis bidentatae leaf powder, is added just by radix achyranthis bidentatae Ye Fenyu n-hexane solid-liquid ratio 1g:3~8mL
Hexane extraction, extraction temperature are 40~60 DEG C, and extraction time is 1~5h, repeat to extract 1~3 time, filtrate removes through vacuum distillation
Solvent hexane obtains the compound lard of radix achyranthis bidentatae leaf；
Step S2: the compound lard for taking step S1 to extract, by compound lard and NaOH-C2H5OH solvent feed ratio 1g:2~4mL
NaOH-C is added2H5OH solution, in 75~85 DEG C of water-baths react 1.5~3h, with hydrochloric acid solution adjust mixed system pH value to
1~3, it stirs evenly, separates oil reservoir, the n-hexane extraction of 10 times of volume oil reservoir sample amounts is added, and be washed to neutrality, be evaporated under reduced pressure
Solvent hexane is removed, desiccant water removal is added and is dried to obtain fatty acid mixed；
Step S3: taking ethyl alcohol to be heated to 70 DEG C, urea be added while stirring, is completely dissolved in urea in ethyl alcohol and obtains urea-second
Alcoholic solution；
Step S4: the fatty acid mixed for taking step S2 to obtain is added to step by urea and 1~3:1 of fatty acid mixed mass ratio
In urea-ethanol solution that S3 is obtained, 75~85 DEG C of temperature are maintained, 30~70min of return stirring, object to be mixed becomes clear
Stop heating afterwards, continues stirring and be cooled to room temperature；
Step S5: 5~25h is included at -10~5 DEG C, gained urea clathrate mixture is separated by filtration, with petroleum ether knot
Brilliant object obtains filtrate；
Step S6: being added petroleum ether and sig water in the filtrate obtained to step S5, extraction obtains organic phase, by organic phase water
It is washed till neutrality, then with desiccant dryness, rotary evaporation removal petroleum ether obtains linoleic acid.
Preferably, the solid-liquid ratio of radix achyranthis bidentatae Ye Fenyu n-hexane described in step S1 is 1g:6mL.
Preferably, extraction temperature described in step S1 is 50 DEG C, extraction time 2h, repeats to extract 2 times.
Preferably, urea-ethanol solution concentration described in step S3 is 50~300g/L.
Preferably, urea-ethanol solution concentration described in step S3 is 100g/L.
Preferably, the mass ratio of urea and fatty acid mixed is 2:1 in urea-ethanol solution described in step S4.
Preferably, urea clathrate process is included for 24 hours at -5 DEG C in step S5.
Preferably, desiccant described in step S2 and S6 is anhydrous sodium sulfate.
Preferably, the volume ratio 1:1:1 of filtrate described in step S6, petroleum ether and sig water, wherein sig water is hydrogen-oxygen
Change sodium solution.
The invention has the following advantages:
1, radix achyranthis bidentatae leaf is the traditional advantage product in China, and the more ground in the whole nation have plantation and cost is not high is widely used, and the present invention is first
Secondary provide extracts linoleic technique from radix achyranthis bidentatae leaf, and radix achyranthis bidentatae leaf is enable sufficiently to be recycled, and is the research of radix achyranthis bidentatae leaf
Provide new approaches；
2, the extracting method of radix achyranthis bidentatae leaf Linoleic acid provided by the invention, easy to operate, linoleic recovery rate is high and required sets
Standby simple economy, reagent price is cheap, from a wealth of sources, is easily obtained.
Specific embodiment
The present invention is further specifically described below with reference to embodiment, it should which explanation, following the description are only
In order to explain the present invention, its content is not defined.
Embodiment 1
Step S1: being ground into radix achyranthis bidentatae leaf powder for radix achyranthis bidentatae leaf, and precision weighs 50g, and 300mL is being added just by solid-liquid ratio (w/v) 1g:6mL
Hexane solution extracts 4h in 50 DEG C of water-baths, repeats to extract 2 times, obtains radix achyranthis bidentatae leaf after vacuum distillation recovered solvent n-hexane
Compound lard；
Step S2: NaOH-C is added by solid-liquid ratio (w/v) 1g:4mL in the compound lard for taking step S1 to extract2H5OH solution, 75
3h is reacted in~85 DEG C of water-baths, is taken out, appropriate 50~70 DEG C of warm water is added to dissolve, 20min is stirred, hydrochloric acid solution is added to be adjusted to pH value
For 2 acid solution, 15min is stirred, separates oil reservoir, the n-hexane extraction of about 10 times of volume oil reservoir sample amounts is added, and is washed to
Neutrality, vacuum distillation remove solvent hexane, and anhydrous sodium sulfate is added and is dried to obtain fatty acid mixed；
Step S3: taking 500mL ethyl alcohol to be heated to 70 DEG C, and urea 50g is added while stirring, is completely dissolved in urea in ethyl alcohol and obtains
Urea-ethanol solution；
Step S4: urea-ethanol solution that step S3 is obtained is added in the fatty acid mixed that step S2 is obtained, and maintains temperature
70 DEG C, return stirring 1h, object to be mixed stops heating after becoming clear, continues stirring to being cooled to room temperature；
Step S5: it is included at -5 DEG C for 24 hours, gained urea clathrate mixture is separated by filtration, with petroleum ether crystal, is washed
2~3 times are washed, merging filtrate；
Step S6: petroleum ether and sig water are added in the filtrate obtained to step S5, wherein the body of filtrate, petroleum ether and sig water
Product uses sig water that can further remove the impurity component in extracting solution as aqueous phase extracted, sig water is hydrogen than being 1:1:1
Sodium hydroxide solution extracts 2~3 times, collects organic phase, and organic phase is washed to neutrality, and the drying of 100g anhydrous sodium sulfate, rotation is added
Turn evaporative removal petroleum ether and obtain linoleic acid, the linoleic acid after taking revolving repeats weighing 2 times, its average value is taken to obtain linoleic acid
Quality；The quality of fatty acid mixed can be obtained by step S2, and linoleic acid yield=(linoleic acid quality/fatty acid mixed quality) ×
100%, it is 18.6% that linoleic yield, which is calculated, through detection.
Embodiment 2
Step S1: being ground into radix achyranthis bidentatae leaf powder for radix achyranthis bidentatae leaf, and precision weighs 50g, and 150mL is being added just by solid-liquid ratio (w/v) 1g:3mL
Hexane solution extracts 2h in 50 DEG C of water-baths, repeats to extract 1 time, obtains radix achyranthis bidentatae leaf after vacuum distillation recovered solvent n-hexane
Compound lard；
Step S2: NaOH-C is added by solid-liquid ratio (w/v) 1g:4mL in the compound lard for taking step S1 to extract2H5OH solution, 75
3h is reacted in~85 DEG C of water-baths, is taken out, appropriate 50~70 DEG C of warm water is added to dissolve, 20min is stirred, hydrochloric acid solution is added to be adjusted to pH value
For 2 acid solution, 15min is stirred, separates oil reservoir, the n-hexane extraction of about 10 times of volume oil reservoir sample amounts is added, and is washed to
Neutrality, vacuum distillation remove solvent hexane, and anhydrous sodium sulfate is added and is dried to obtain fatty acid mixed；
Step S3: taking 500mL ethyl alcohol to be heated to 70 DEG C, and urea 50g is added while stirring, is completely dissolved in urea in ethyl alcohol and obtains
Urea-ethanol solution；
Step S4: urea-ethanol solution that step S3 is obtained is added in the fatty acid mixed that step S2 is obtained, and maintains temperature
70 DEG C, return stirring 1h, object to be mixed stops heating after becoming clear, continues stirring to being cooled to room temperature；
Step S5: it is included at -5 DEG C for 24 hours, gained urea clathrate mixture is separated by filtration, with petroleum ether crystal, is washed
2~3 times are washed, merging filtrate；
Step S6: petroleum ether and sig water are added in the filtrate obtained to step S5, wherein the body of filtrate, petroleum ether and sig water
Product uses sig water that can further remove the impurity component in extracting solution as aqueous phase extracted, sig water is hydrogen than being 1:1:1
Sodium hydroxide solution extracts 2~3 times, collects organic phase, and organic phase is washed to neutrality, and the drying of 100g anhydrous sodium sulfate, rotation is added
Turn evaporative removal petroleum ether and obtains linoleic acid；With embodiment 1, calculate yield is linoleic yield calculation method
17.3%。
Embodiment 3
Step S1: being ground into radix achyranthis bidentatae leaf powder for radix achyranthis bidentatae leaf, and precision weighs 50g, and 300mL is being added just by solid-liquid ratio (w/v) 1g:6mL
Hexane solution extracts 4h in 50 DEG C of water-baths, repeats to extract 2 times, obtains radix achyranthis bidentatae leaf after vacuum distillation recovered solvent n-hexane
Compound lard；
Step S2: NaOH-C is added by solid-liquid ratio (w/v) 1g:2mL in the compound lard for taking step S1 to extract2H5OH solution, 75
3h is reacted in~85 DEG C of water-baths, is taken out, appropriate 50~70 DEG C of warm water is added to dissolve, 20min is stirred, hydrochloric acid solution is added to be adjusted to pH value
For 2 acid solution, 15min is stirred, separates oil reservoir, the n-hexane extraction of about 10 times of volume oil reservoir sample amounts is added, and is washed to
Neutrality, vacuum distillation remove solvent hexane, and anhydrous sodium sulfate is added and is dried to obtain fatty acid mixed；
Step S3: taking 500mL ethyl alcohol to be heated to 70 DEG C, and urea 50g is added while stirring, is completely dissolved in urea in ethyl alcohol and obtains
Urea-ethanol solution；
Step S4: urea-ethanol solution that step S3 is obtained is added in the fatty acid mixed that step S2 is obtained, and maintains temperature
70 DEG C, return stirring 1h, object to be mixed stops heating after becoming clear, continues stirring to being cooled to room temperature；
Step S5: it is included at -5 DEG C for 24 hours, gained urea clathrate mixture is separated by filtration, with petroleum ether crystal, is washed
2~3 times are washed, merging filtrate；
Step S6: petroleum ether and sig water are added in the filtrate obtained to step S5, wherein the body of filtrate, petroleum ether and sig water
Product uses sig water that can further remove the impurity component in extracting solution as aqueous phase extracted, sig water is hydrogen than being 1:1:1
Sodium hydroxide solution extracts 2~3 times, collects organic phase, and organic phase is washed to neutrality, and the drying of 100g anhydrous sodium sulfate, rotation is added
Turn evaporative removal petroleum ether and obtains linoleic acid；With embodiment 1, calculate yield is linoleic yield calculation method
15.6%。
Embodiment 4
Step S1: being ground into radix achyranthis bidentatae leaf powder for radix achyranthis bidentatae leaf, and precision weighs 50g, and 300mL is being added just by solid-liquid ratio (w/v) 1g:6mL
Hexane solution extracts 4h in 50 DEG C of water-baths, repeats to extract 2 times, obtains radix achyranthis bidentatae leaf after vacuum distillation recovered solvent n-hexane
Compound lard；
Step S2: NaOH-C is added by solid-liquid ratio (w/v) 1g:4mL in the compound lard for taking step S1 to extract2H5OH solution, 75
3h is reacted in~85 DEG C of water-baths, is taken out, appropriate 50~70 DEG C of warm water is added to dissolve, 20min is stirred, hydrochloric acid solution is added to be adjusted to pH value
For 2 acid solution, 15min is stirred, separates oil reservoir, the n-hexane extraction of about 10 times of volume oil reservoir sample amounts is added, and is washed to
Neutrality, vacuum distillation remove solvent hexane, and anhydrous sodium sulfate is added and is dried to obtain fatty acid mixed；
Step S3: taking 500mL ethyl alcohol to be heated to 70 DEG C, and urea 5g is added while stirring, is completely dissolved in urea in ethyl alcohol and obtains
Urea-ethanol solution；
Step S4: urea-ethanol solution that step S3 is obtained is added in the fatty acid mixed that step S2 is obtained, and maintains temperature
70 DEG C, return stirring 1h, object to be mixed stops heating after becoming clear, continues stirring to being cooled to room temperature；
Step S5: it is included at -5 DEG C for 24 hours, gained urea clathrate mixture is separated by filtration, with petroleum ether crystal, is washed
2~3 times are washed, merging filtrate；
Step S6: petroleum ether and sig water are added in the filtrate obtained to step S5, wherein the body of filtrate, petroleum ether and sig water
Product uses sig water that can further remove the impurity component in extracting solution as aqueous phase extracted, sig water is hydrogen than being 1:1:1
Sodium hydroxide solution extracts 2~3 times, collects organic phase, and organic phase is washed to neutrality, and the drying of 100g anhydrous sodium sulfate, rotation is added
Turn evaporative removal petroleum ether and obtains linoleic acid；With embodiment 1, calculate yield is linoleic yield calculation method
14.4%。
Embodiment 5
Step S1: being ground into radix achyranthis bidentatae leaf powder for radix achyranthis bidentatae leaf, and precision weighs 50g, and 300mL is being added just by solid-liquid ratio (w/v) 1g:6mL
Hexane solution extracts 4h in 50 DEG C of water-baths, repeats to extract 2 times, the miscella of radix achyranthis bidentatae leaf is obtained after vacuum distillation recovered solvent
Rouge；
Step S2: NaOH-C is added by solid-liquid ratio (w/v) 1g:4mL in the compound lard for taking step S1 to extract2H5OH solution, 75
3h is reacted in~85 DEG C of water-baths, is taken out, appropriate 50~70 DEG C of warm water is added to dissolve, 20min is stirred, hydrochloric acid solution is added to be adjusted to pH value
For 2 acid solution, 15min is stirred, separates oil reservoir, the n-hexane extraction of about 10 times of volume oil reservoir sample amounts is added, and is washed to
Neutrality, vacuum distillation remove solvent hexane, and anhydrous sodium sulfate is added and is dried to obtain fatty acid mixed；
Step S3: taking 500mL ethyl alcohol to be heated to 70 DEG C, and urea 5g is added while stirring, is completely dissolved in urea in ethyl alcohol and obtains
Urea-ethanol solution；
Step S4: urea-ethanol solution that step S3 is obtained is added in the fatty acid mixed that step S2 is obtained, and maintains temperature
70 DEG C, return stirring 1h, object to be mixed stops heating after becoming clear, continues stirring to being cooled to room temperature；
Step S5: it includes at 5 DEG C for 24 hours, gained urea clathrate mixture is separated by filtration, with petroleum ether crystal, is washed
2~3 times are washed, merging filtrate；
Step S6: petroleum ether and sig water are added in the filtrate obtained to step S5, wherein the body of filtrate, petroleum ether and sig water
Product uses sig water that can further remove the impurity component in extracting solution as aqueous phase extracted, sig water is hydrogen than being 1:1:1
Sodium hydroxide solution extracts 2~3 times, collects organic phase, and organic phase is washed to neutrality, and the drying of 100g anhydrous sodium sulfate, rotation is added
Turn evaporative removal petroleum ether and obtains linoleic acid；With embodiment 1, calculate yield is linoleic yield calculation method
15.1%。
Embodiment 6
Step S1: being ground into radix achyranthis bidentatae leaf powder for radix achyranthis bidentatae leaf, and precision weighs 50g, and 300mL is being added just by solid-liquid ratio (w/v) 1g:6mL
Hexane solution extracts 4h in 50 DEG C of water-baths, repeats to extract 2 times, obtains radix achyranthis bidentatae leaf after vacuum distillation recovered solvent n-hexane
Compound lard；
Step S2: NaOH-C is added by solid-liquid ratio (w/v) 1g:4mL in the compound lard for taking step S1 to extract2H5OH solution, 75
3h is reacted in~85 DEG C of water-baths, is taken out, appropriate 50~70 DEG C of warm water is added to dissolve, 20min is stirred, hydrochloric acid solution is added to be adjusted to pH value
For 2 acid solution, 15min is stirred, separates oil reservoir, the n-hexane extraction of about 10 times of volume oil reservoir sample amounts is added, and is washed to
Neutrality, vacuum distillation remove solvent hexane, and anhydrous sodium sulfate is added and is dried to obtain fatty acid mixed；
Step S3: taking 500mL ethyl alcohol to be heated to 70 DEG C, and urea 5g is added while stirring, is completely dissolved in urea in ethyl alcohol and obtains
Urea-ethanol solution；
Step S4: urea-ethanol solution that step S3 is obtained is added in the fatty acid mixed that step S2 is obtained, and maintains temperature
70 DEG C, return stirring 1h, mixture stops heating after becoming clear, continues stirring to being cooled to room temperature；
Step S5: including 10h at -5 DEG C, and gained urea clathrate mixture is separated by filtration, with petroleum ether crystal, is washed
2~3 times are washed, merging filtrate；
Step S6: petroleum ether and sig water are added in the filtrate obtained to step S5, wherein the body of filtrate, petroleum ether and sig water
Product uses sig water that can further remove the impurity component in extracting solution as aqueous phase extracted, sig water is hydrogen than being 1:1:1
Sodium hydroxide solution extracts 2~3 times, collects organic phase, and organic phase is washed to neutrality, and the drying of 100g anhydrous sodium sulfate, rotation is added
Turn evaporative removal petroleum ether and obtains linoleic acid；With embodiment 1, calculate yield is linoleic yield calculation method
13.2%。
Above-mentioned, although specific embodiments of the present invention have been described, not to the limit of the scope of the present invention
System, based on the technical solutions of the present invention, those skilled in the art do not need to make the creative labor can make it is each
Kind modification or deformation are still within protection scope of the present invention.
Claims (9)
1. the extracting method of radix achyranthis bidentatae leaf Linoleic acid, it is characterised in that specific steps are as follows:
Step S1: it by radix achyranthis bidentatae leaf dried and crushed at radix achyranthis bidentatae leaf powder, is added just by radix achyranthis bidentatae Ye Fenyu n-hexane solid-liquid ratio 1g:3~8mL
Hexane extraction, extraction temperature are 40~60 DEG C, and extraction time is 1~5h, repeat to extract 1~3 time, filtrate removes through vacuum distillation
Solvent hexane obtains the compound lard of radix achyranthis bidentatae leaf；
Step S2: the compound lard for taking step S1 to extract, by compound lard and NaOH-C2H5OH solvent feed ratio 1g:2~4mL adds
Enter NaOH-C2H5OH solution reacts 1.5~3h in 75~85 DEG C of water-baths, adjusts the pH value of mixed system to 1 with hydrochloric acid solution
~3, it stirs evenly, separates oil reservoir, the n-hexane extraction of 10 times of volume oil reservoir sample amounts is added, and be washed to neutrality, be evaporated under reduced pressure
Solvent hexane is removed, desiccant water removal is added and is dried to obtain fatty acid mixed；
Step S3: taking ethyl alcohol to be heated to 70 DEG C, urea be added while stirring, is completely dissolved in urea in ethyl alcohol and obtains urea-second
Alcoholic solution；
Step S4: the fatty acid mixed for taking step S2 to obtain is added to step by urea and 1~3:1 of fatty acid mixed mass ratio
In urea-ethanol solution that S3 is obtained, 75~85 DEG C of temperature are maintained, 30~70min of return stirring, object to be mixed becomes clear
Stop heating afterwards, continues stirring and be cooled to room temperature；
Step S5: 5~25h is included at -10~5 DEG C, gained urea clathrate mixture is separated by filtration, with petroleum ether knot
Brilliant object obtains filtrate；
Step S6: being added petroleum ether and sig water in the filtrate obtained to step S5, extraction obtains organic phase, by organic phase water
It is washed till neutrality, then with desiccant dryness, rotary evaporation removal petroleum ether obtains linoleic acid.
2. the extracting method of radix achyranthis bidentatae leaf Linoleic acid according to claim 1, it is characterised in that: radix achyranthis bidentatae described in step S1
The solid-liquid ratio of Ye Fenyu n-hexane is 1g:6mL.
3. the extracting method of radix achyranthis bidentatae leaf Linoleic acid according to claim 1, it is characterised in that: extracted described in step S1
Temperature is 50 DEG C, extraction time 2h, repeats to extract 2 times.
4. the extracting method of radix achyranthis bidentatae leaf Linoleic acid according to claim 1, it is characterised in that: urinated described in step S3
Element-ethanol solution concentration is 50~300g/L.
5. the extracting method of radix achyranthis bidentatae leaf Linoleic acid according to claim 1, it is characterised in that: urinated described in step S3
Element-ethanol solution concentration is 100g/L.
6. the extracting method of radix achyranthis bidentatae leaf Linoleic acid according to claim 1, it is characterised in that: urinated described in step S4
The mass ratio of urea and fatty acid mixed is 2:1 in element-ethanol solution.
7. the extracting method of radix achyranthis bidentatae leaf Linoleic acid according to claim 1, it is characterised in that: urea clathrate in step S5
Process is included for 24 hours at -5 DEG C.
8. the extracting method of radix achyranthis bidentatae leaf Linoleic acid according to claim 1, it is characterised in that: described in step S2 and S6
Desiccant is anhydrous sodium sulfate.
9. the extracting method of radix achyranthis bidentatae leaf Linoleic acid according to claim 1, it is characterised in that: filtered described in step S6
The volume ratio 1:1:1 of liquid, petroleum ether and sig water, wherein sig water is sodium hydroxide solution.
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| 董琴琴: "牛膝化学成分的研究", 《中国优秀硕士学位论文全文数据库农业科技辑》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110257175A (en) * | 2019-06-20 | 2019-09-20 | 深圳市仙迪化妆品有限公司 | It is a kind of to prepare linoleic method and linoleic application using rose hip oil |
| CN110835298A (en) * | 2019-10-30 | 2020-02-25 | 南宁学院 | Method for extracting linoleic acid from sirloin |
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| CN109824509B (en) | 2021-10-22 |
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