CN104987954A - Method for extracting volatile oil and magnolol from mangnolia officinalis leaves - Google Patents

Abstract

The invention discloses a method for extracting volatile oil and magnolol from mangnolia officinalis leaves. First, mangnolia officinalis leaf powder is placed in a distilling tank for steam distillation, the mangnolia officinalis volatile oil is extracted, then the magnolol is extracted by the following steps that 1. water and solid residues in the distilling tank are stirred, slaked lime is added, pH is adjusted to 9-10, stirring is carried out continuously for 30-40 min, and filtering is carried out; 2. filter residues are subjected to normal-temperature digestion by two times with lime water with pH of 9-10, the extracting liquid is combined, concentrated hydrochloric acid is used for adjusting pH of the extracting liquid to be 3-4, standing and settling are carried out, water is used for washing until neutral is achieved, constant temperature drying is carried out under the temperature of 45 DEG C, and crude extract is obtained; and 3. the crude extract and silica gel with four-time amount are mixed, petroleum ether is used for reflux extraction, extracting liquid is concentrated, cooling is carried out, after complete precipitation crystallization, filtering is carried out, and then an ethyl acetate and petroleum ether mixed solution is used for recrystallization. Comprehensive extracting of two effective components in the mangnolia officinalis leaves is achieved, the process is simple, cost is low, the extracting rate is high, and environment-protecting industrialized production can be achieved.

Description

The method of volatile oil and magnolol is extracted from bark of official magnolia leaf

Technical field

The present invention relates to the extracting method of effective ingredients in plant, what be specifically related to is a kind of method extracting volatile oil and magnolol from bark of official magnolia leaf.

Background technology

Magnolol is the significant medicine of a kind of physiologically active, have anti-inflammatory, antibacterial, resisting pathogenic microbes, antiulcer agent, anti-oxidant, antitumor, the effect such as morphine withdrawal syndrome and anticoagulant can be suppressed, mainly clinically be used as to eliminate that full vexed, the calm nervus centralis of chest abdomen, sportsmen are of flaccid muscles, antimycotic, in the medicine of antiulcer agent etc., apply wide model, consumption is large.For a long time, magnolol mainly extracts from the dry hide of the magnolia bark of official magnolia (Magnolia officinalis Rehd et Wils) drying, Gen Pi and branch skin, Magnolia bark is important Chinese medicinal materials, also Cortex Magnoliae Officinalis is, Magnolia bark will grow and just meet pharmaceutical quality requirement in about 20 years, bark of official magnolia tree poor growth, the production of crude drugs cycle is very long.The resource of Magnolia bark is very limited now, and the source of magnolol also receives the restriction of scarcity of resources.

Research finds, containing the biologically active substance that magnolia obovata bark is identical in bark of official magnolia leaf, as magnolol, Honokiol, volatilization wet goods, and find that Cortex Magnoliae Officinalis volatile oil has anti-microbial activity, just in bark of official magnolia leaf, the content of magnolol is lower, only having 0.29%-0.36%, is the 1/8-1/10 of Magnolia bark content.Bark of official magnolia leaf resource is abundanter, and its leaf is long and roomy, and annual autumn withers and falls naturally, and the weight of the bark of official magnolia leaf magnolia obovata bark of annual growth is suitable, and therefore, people just start the research of extracting magnolol from bark of official magnolia leaf.Initial, people extract the magnolol in bark of official magnolia leaf by the existing method extracting magnolol from Magnolia bark, facts have proved, this approach is unworkable, because the method extracting magnolol from Magnolia bark carries or alcohol extracting with alkali, and the high temperature reflux in basic solvent or alcohol extracting process all can cause the deterioration by oxidation of magnolol, magnolol loss is comparatively large, consequently substantially can not get magnolol product.Until 2012, China Patent Publication No. CN 102304027 B discloses a kind of methyl alcohol and soaks the method that bark of official magnolia leaf extracts magnolol, and the extraction yield of the method can reach 98.1%-98.6%, and content is up to 99.1%.But the main Extraction medium methyl alcohol used in the method causes poisonous and hazardous Working environment, but also there is the deficiency that leaching process is loaded down with trivial details, factorial praluction cost is higher.

Summary of the invention

The object of the invention is to propose a kind of method of volatile oil Honokiol being carried out comprehensive extraction from bark of official magnolia leaf, the method operation is simpler, and cost is lower, and the purity of magnolol is high, and extraction yield is stablized, and can realize gueen factoryization and produce.

The technical scheme realizing above-mentioned purpose is: a kind of method extracting volatile oil and magnolol from bark of official magnolia leaf, it is characterized in that completing in the steps below:

1) bark of official magnolia leaf powder is placed in retort, passes into water vapour and distill under stirring, distillation time is 1h-1.2h, receives whole process and slip out liquid from prolong,

2) slip out liquid 30 DEG C-60 DEG C model petroleum ether extractions three times, during each extraction, the consumption of sherwood oil is 0.7-1 times that slips out liquid accumulated amount, combining extraction liquid,

3) use anhydrous sodium sulfate drying extraction liquid, then Distillation recovery sherwood oil, obtains Cortex Magnoliae Officinalis volatile oil;

4) step 1 is completed) after, stir the water in retort and solid slag, Temperature fall, to normal temperature, adds white lime, regulates pH=9-10, continues to stir 30min-40min, releases material, filter,

5) by step 4) the liming normal temperature lixiviate twice of filter residue pH=9-10, the consumption of each liming be the 23-25 of filter residue weight doubly, continuously stirring 30min-40min in each leaching process, filters, filtrate and step 4) filtrate merging,

6) filtrate regulates its pH=3-4 with concentrated hydrochloric acid, leaves standstill precipitation, collecting precipitation thing,

7) with distilled water, throw out washing is extremely neutral, freeze-day with constant temperature at 45 DEG C, obtains crude extract,

8) the silica gel mix of crude extract and 4 times amount is even, mixture 30 DEG C-60 DEG C model sherwood oils refluxing extraction in circulation extractor of 30-32 times amount, be back to and slip out liquid without till during magnolol, then concentrated extracting solution reclaim sherwood oil, cooling, after separating out flaxen crystallization completely, filter

9) pale yellow crystals ethyl acetate and sherwood oil volume ratio be 8: 2 solution carry out recrystallization, obtain the magnolol that purity is not less than 99.2%.

The invention has the advantages that: the comprehensive extraction 1, achieving two kinds of effective constituents, both obtained Cortex Magnoliae Officinalis volatile oil, magnolol of having got back, bark of official magnolia leaf is fully utilized.2, bark of official magnolia leaf powder extracts magnolol again after wet distillation process, significantly can reduce the dark thick jelly in leaching process in the past, easy purification process, and the extraction yield of magnolol significantly improves.3, regulate the pH=3-4 of filtrate that aldehydes matter can be made to maximize precipitation with concentrated hydrochloric acid, decrease the precipitation of other acidic substance.4, operation is simpler, and the used time is short, mainly using lime aqueous solution as Extraction medium in the leaching process of magnolol, avoids the use of poisonous and harmful solvent, achieves gueen factoryization and produces.5, cost is lower, and in the leaching process of magnolol, waste water is capable of circulation to be applied mechanically, and reduces production cost by a relatively large margin.6, extraction yield is stablized, and the purity of magnolol is high.7, according to the inventive method, the industrial scale of batch production can make the oil mass that obtains of bark of official magnolia leaf volatile oil reach 1.5%-2.0%; The extraction rate reached of magnolol is to 98.5%-99.1%, and purity reaches 99.2%-99.5%; The method is also applicable to extracting magnolol from Magnolia bark, and can increase substantially extraction yield and the purity of magnolol.

Embodiment

Below in conjunction with embodiment, the invention will be further described.

Embodiment 1

Bark of official magnolia leaf is dried in the shade, pulverizes, cross 100 mesh sieves, then complete the extraction of Cortex Magnoliae Officinalis volatile oil and magnolol in the steps below:

1) take bark of official magnolia leaf powder 40kg and put into retort, pass into wet distillation 1.2h under stirring, from prolong, receive whole process slip out liquid,

2) slip out liquid 30 DEG C-60 DEG C model petroleum ether extractions three times, during each extraction, the consumption of sherwood oil is 0.7 times that slips out liquid accumulated amount, combining extraction liquid,

3) use anhydrous sodium sulfate drying extraction liquid, then Distillation recovery sherwood oil, obtain 0.72kg Cortex Magnoliae Officinalis volatile oil;

4) step 1 is completed) after, continue to stir the water in retort and solid slag, Temperature fall, to normal temperature, adds white lime, regulates pH=10, stirs 30min-40min, releases material, filters,

5) by step 4) the liming normal temperature lixiviate twice of filter residue pH=10, the consumption of each liming is 25 times of filter residue weight, continuously stirring 40min in each leaching process, filters, filtrate and step 4) filtrate merging,

6) filtrate regulates its pH=3 with concentrated hydrochloric acid, leaves standstill precipitation, collecting precipitation thing,

7) with distilled water, throw out washing is extremely neutral, freeze-day with constant temperature at 45 DEG C, obtains crude extract 2.45kg,

8) the silica gel mix of crude extract and 4 times amount is even, mixture 30 DEG C-60 DEG C model sherwood oils refluxing extraction in circulation extractor of 30 times amount, be back to and slip out liquid without till during magnolol, then concentrated extracting solution reclaim sherwood oil, cooling, after separating out flaxen crystallization completely, filter

9) pale yellow crystals ethyl acetate and sherwood oil volume ratio be 8: 2 solution carry out recrystallization, obtain highly purified magnolol and other aldehydes matter, wherein magnolol is 0.141kg, and purity is 99.5%, and extraction yield is 99.1%.

Embodiment 2

Take bark of official magnolia leaf 100 order powder 60kg, put into retort, then complete the extraction of Cortex Magnoliae Officinalis volatile oil and magnolol in the steps below:

1) pass into wet distillation 1h under stirring, from prolong, receive whole process slip out liquid,

2) slip out liquid 30 DEG C-60 DEG C model petroleum ether extractions three times, during each extraction, the consumption of sherwood oil is 1 times that slips out liquid accumulated amount, combining extraction liquid,

3) use anhydrous sodium sulfate drying extraction liquid, then Distillation recovery sherwood oil, obtain 0.96kg Cortex Magnoliae Officinalis volatile oil;

4) step 1 is completed) after, continue to stir the water in retort and solid slag, Temperature fall, to normal temperature, adds white lime, regulates pH=9, stirs 40min, releases material, filters,

5) by step 4) the liming normal temperature lixiviate twice of filter residue pH=9, the consumption of each liming is 24 times of filter residue weight, continuously stirring 40min in each leaching process, filters, filtrate and step 4) filtrate merging,

6) filtrate regulates its pH=3 with concentrated hydrochloric acid, leaves standstill precipitation, collecting precipitation thing,

7) with distilled water, throw out washing is extremely neutral, freeze-day with constant temperature at 45 DEG C, obtains crude extract 3.48kg,

8) the silica gel mix of crude extract and 4 times amount is even, mixture 30 DEG C-60 DEG C model sherwood oils refluxing extraction in circulation extractor of 31 times amount, be back to and slip out liquid without till during magnolol, then concentrated extracting solution reclaim sherwood oil, cooling, after separating out flaxen crystallization completely, filter

9) pale yellow crystals ethyl acetate and sherwood oil volume ratio be 8: 2 solution carry out recrystallization, obtain highly purified magnolol and other aldehydes matter, wherein magnolol is 0.216kg, and purity is 99.3%, and extraction yield is 98.8%.

Embodiment 3

Take bark of official magnolia leaf 100 order powder 80kg, put into retort, then complete the extraction of Cortex Magnoliae Officinalis volatile oil and magnolol in the steps below:

1) pass into wet distillation 1h under stirring, from prolong, receive whole process slip out liquid,

2) slip out liquid 30 DEG C-60 DEG C model petroleum ether extractions three times, during each extraction, the consumption of sherwood oil is 0.7 times that slips out liquid accumulated amount, combining extraction liquid,

3) use anhydrous sodium sulfate drying extraction liquid, then Distillation recovery sherwood oil, obtain 1.36kg Cortex Magnoliae Officinalis volatile oil;

4) step 1 is completed) after, stir the water in retort and solid slag, Temperature fall, to normal temperature, adds white lime, regulates pH=10, continues to stir 30min, releases material, filter,

5) by step 4) the liming normal temperature lixiviate twice of filter residue pH=9, the consumption of each liming is 23 times of filter residue weight, continuously stirring 35min in each leaching process, filters, filtrate and step 4) filtrate merging,

6) filtrate regulates its pH=4 with concentrated hydrochloric acid, leaves standstill precipitation, collecting precipitation thing,

7) with distilled water, throw out washing is extremely neutral, freeze-day with constant temperature at 45 DEG C, obtains crude extract 4.96kg,

8) the silica gel mix of crude extract and 4 times amount is even, mixture 30 DEG C-60 DEG C model sherwood oils refluxing extraction in circulation extractor of 32 times amount, be back to and slip out liquid without till during magnolol, then concentrated extracting solution reclaim sherwood oil, cooling, after separating out flaxen crystallization completely, filter

9) pale yellow crystals ethyl acetate and sherwood oil volume ratio be 8: 2 solution carry out recrystallization, obtain highly purified magnolol and other aldehydes matter, wherein magnolol is 0.286kg, and purity is 99.2%, and extraction yield is 98.5%.

Claims (1)

1. from bark of official magnolia leaf, extract a method for volatile oil and magnolol, it is characterized in that completing in the steps below:

1) bark of official magnolia leaf powder is placed in retort, passes into water vapour and distill under stirring, distillation time is 1h-1.2h, receives whole process and slip out liquid from prolong,

2) slip out liquid 30 DEG C-60 DEG C model petroleum ether extractions three times, during each extraction, the consumption of sherwood oil is 0.7-1 times that slips out liquid accumulated amount, combining extraction liquid,

3) use anhydrous sodium sulfate drying extraction liquid, then Distillation recovery sherwood oil, obtains Cortex Magnoliae Officinalis volatile oil;

4) step 1 is completed) after, continue to stir the water in retort and solid slag, Temperature fall, to normal temperature, adds white lime, regulates pH=9-10, continues to stir 30min-40min, releases material, filter,

5) by step 4) the liming normal temperature lixiviate twice of filter residue pH=9-10, the consumption of each liming be the 23-25 of filter residue weight doubly, continuously stirring 30min-40min in each leaching process, filters, filtrate and step 4) filtrate merging,

6) filtrate regulates its pH=3-4 with concentrated hydrochloric acid, leaves standstill precipitation, collecting precipitation thing,

7) with distilled water, throw out washing is extremely neutral, freeze-day with constant temperature at 45 DEG C, obtains crude extract,

8) the silica gel mix of crude extract and 4 times amount is even, mixture 30 DEG C-60 DEG C model sherwood oils refluxing extraction in circulation extractor of 30-32 times amount, be back to and slip out liquid without till during magnolol, then concentrated extracting solution reclaim sherwood oil, cooling, after separating out flaxen crystallization completely, filter

9) pale yellow crystals ethyl acetate and sherwood oil volume ratio be 8: 2 solution carry out recrystallization, obtain the magnolol that purity is not less than 99.2%.