CN1357528A - Caproleic acid extracting process from royal jelly - Google Patents
Caproleic acid extracting process from royal jelly Download PDFInfo
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- CN1357528A CN1357528A CN 00132077 CN00132077A CN1357528A CN 1357528 A CN1357528 A CN 1357528A CN 00132077 CN00132077 CN 00132077 CN 00132077 A CN00132077 A CN 00132077A CN 1357528 A CN1357528 A CN 1357528A
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Abstract
The present invention discloses the process of extracting caproleic acid from royal jelly and maintaining its original activity and functions. The process includes the steps of: diluting raw royal jelly, filtering to eliminate impurity, dissolving raw royal jelly, heating to reflux, extracting to separate, regualting pH value, storing under low temperature, mixing through stirring, depositing to extract, and vacuum freeze drying. The product of the present invention is spongy dry powder with water content of 0.5-2.0% and caproleic acid content of 70.0-90.0%. The present invention is stable in product quality, simple in technology and easy to control cost.
Description
The present invention relates to a kind of method of extracting decylenic acid, especially a kind of extracting method that from royal jelly, extracts decylenic acid and make it to keep under field conditions (factors) original activeconstituents and effect.
Decylenic acid full name is 10-hydroxyl olefin(e) acid (10-HAD), it is the important component of royal jelly, it only is present in the royal jelly under field conditions (factors), study for a long time and experimental results show that by us, decylenic acid extract the back use separately have anticancer, anti-cancer, unique functions such as anti-inflammatory, sterilization, toxin expelling, and can strengthen body immunity, improve microcirculation in human body, promote tissue anti-ageing, special efficacy such as promote longevity is arranged.More than these researchs also early by expert's experiment and clinical proof the both at home and abroad.But how can extract the high decylenic acid that also can keep its activeconstituents of content from royal jelly, the interaction energy of decylenic acid is given full play to, be a difficult problem always.As application number is 86107034, and the authorization day for announcing is that the patent of invention on March 2nd, 1988 discloses a kind of method of extracting 10-hydroxy-from royal jelly with physical method, and the decylenic acid content that is extracted is 25%, and content is low, and purity is not high.
The purpose of this invention is to provide a kind of method of from royal jelly, extracting decylenic acid, and make it to keep original activeconstituents and effect under field conditions (factors), and the content height.
The object of the present invention is achieved like this: technical process of the present invention is: the magma dilution, and filtering and impurity removing, dissolving magma, reflux, extracting and separating, pH value is regulated, low-temperature storage, the mixed stirring, precipitation is extracted, vacuum lyophilization.
Specific embodiment of the present invention is:
A, magma dilution: before producing utensil is carried out ultraviolet disinfection, get the royal jelly magma distilled water diluting that meets " GB9697-88 royal jelly standard " salable product, magma and distilled water weight ratio are 1: 1～2.
B, filtering and impurity removing: the magma after the dilution is filtered through the above screen of 50 orders, removes impurity.
C, dissolving magma: the magma that will remove impurity is poured in the basic solution for preparing in advance, through agitator 5～10 minutes stirring and dissolving of rotating speed uniform rotation with 5～20 rev/mins, the preparation of basic solution is to add an amount of NaOH with distilled water to regulate, making pH value is 7.0～7.8, and the weight ratio of magma and distilled water is 1: 1～5.
D, reflux: the apparatus,Soxhlet's of packing into of the magma solution after will dissolving, with ethanol be solvent in 60～75 ℃ of refluxing extraction after 60～180 minutes, it is an amount of to add ethanol again, continues reflux 100～150 minutes, puts cold.
E, extracting and separating: the magma solution after the reflux is moved in the extractor, upper strata oily matter is separated.
F, pH value regulate: when oily matter was heated to 50～80 ℃, the Hcl that adds 0.2～0.5mol/L was an amount of, and making pH value is 2.0～4.5, put coldly, filtered.
G, low-temperature storage: filtrate is packed in the appropriate containers, airtight, under-5 ℃～-10 ℃ temperature condition, deposited 30～120 minutes.
H, the mixed stirring: take out filtrate after the low-temp storage, add ethanol mixing under 35～65 ℃ and stir, the weight proportion of ethanol and filtrate is (70～80): 100.
I, precipitation are extracted: natural sedimentation behind the mixing, extract.
J, vacuum lyophilization: the extract Stainless Steel Disc of packing into is entered the vacuum freeze drier evaporator room and carries out slow hardening knot from room temperature with-24 ℃/hour cooling rate, when the extract temperature is reduced to-25～-30 ℃, kept constant temperature 30～120 minutes, meanwhile water vapour coagulator is vacuumized, the pressure that makes evaporator room is at 30～60Pa, carry out warming temperature after finishing said process, the kiln vacuum is evacuated to 10～30Pa, after 4～6 hours, make extract temperature liter reach 40～53 ℃, promptly get and be the former powder of spongiform drying.
The decylenic acid finished product that the present invention extracted is for being the former powder of spongiform drying, and its moisture content is 0.5～2.0%, and decylenic acid content is 70.0～90.0%.
The decylenic acid that the present invention extracted can keep original activeconstituents and effect under field conditions (factors), content and purity height, and constant product quality, technology is simple, and cost is easy to control.
Below by embodiment the present invention is further elaborated.
Embodiment one
Before producing utensil is carried out ultraviolet disinfection, get the royal jelly magma distilled water diluting that meets " GB9697-88 royal jelly standard " salable product, magma and distilled water weight ratio are 1: 2.Filter through the above screen of 50 orders, remove impurity, the magma of removing impurity is poured in the basic solution for preparing in advance, the preparation of basic solution is with DH20 distilled water and adds an amount of NaOH adjusting, making pH value is 7.0, the weight ratio of magma and distilled water is 1: 5, through centrifugal stirrer 5 minutes stirring and dissolving of rotating speed uniform rotation with 5 rev/mins.With the magma solution apparatus,Soxhlet's of packing into, with ethanol is solvent, and after 60 minutes, it is an amount of to add ethanol again in 60 ℃ of refluxing extraction, continued reflux 100 minutes, put coldly, move into then in the extractor upper strata oily matter is isolated, when oily matter is heated to 50 ℃, the Hcl that adds 0.2mol/L is an amount of, making pH value is 2.0, puts coldly, filters.Filtrate is packed in the appropriate containers, airtight, under-5 ℃ temperature condition, deposited 30 minutes.Take out filtrate and mix under 35 ℃ of temperature condition with ethanol and stir evenly, the weight ratio of ethanol and filtrate is 70%, natural sedimentation, extraction throw out.
Finish as stated above and extract is put into Stainless Steel Disc after the extraction and go into DT-735 vacuum freeze drier evaporator room, carry out the slow hardening knot with-24 ℃/hour cooling rate from room temperature.When the extract temperature is reduced to-25 ℃, kept constant temperature 30 minutes, make the thorough deep colling of extract.Meanwhile, water vapour coagulator is vacuumized, the pressure that makes evaporator room is in 30Pa (absolute pressure).After finishing said process, carry out warming temperature, the kiln vacuum is evacuated to 10Pa (absolute pressure), after 4 hours, make extract temperature liter reach 40 ℃, get final product to such an extent that be the former powder of spongiform drying, moisture content is 0.5～2.0%, and decylenic acid content is 70.0～90.0%
Embodiment two
Before producing utensil is carried out ultraviolet disinfection, get the royal jelly magma distilled water diluting that meets " GB9697-88 royal jelly standard " salable product, magma and distilled water weight ratio are 1: 1.Filter through the above screen of 50 orders, remove impurity, the magma of removing impurity is poured in the basic solution for preparing in advance, the preparation of basic solution is with DH20 distilled water and adds an amount of NaOH adjusting, making pH value is 7.8, the weight ratio of magma and distilled water is 1: 1, through centrifugal stirrer 10 minutes stirring and dissolving of rotating speed uniform rotation with 20 rev/mins.With the magma solution apparatus,Soxhlet's of packing into, with ethanol is solvent, and after 180 minutes, it is an amount of to add ethanol again in 75 ℃ of refluxing extraction, continued reflux 150 minutes, put coldly, move into then in the extractor upper strata oily matter is isolated, when oily matter is heated to 80 ℃, the Hcl that adds 0.5mol/L is an amount of, making pH value is 4.5, puts coldly, filters.Filtrate is packed in the appropriate containers, airtight, under-10 ℃ temperature condition, deposited 120 minutes.Taking out filtrate mixes under 65 ℃ of temperature condition with ethanol and stirs evenly the weight ratio 80% of ethanol and filtrate, natural sedimentation, extraction throw out.
Finish as stated above and extract is put into Stainless Steel Disc after the extraction and go into DT-735 vacuum freeze drier evaporator room, carry out the slow hardening knot with-24 ℃/hour cooling rate from room temperature.When the extract temperature is reduced to-30 ℃, kept constant temperature 120 minutes, make the thorough deep colling of extract.Meanwhile, water vapour coagulator is vacuumized, the pressure that makes evaporator room is in 60Pa (absolute pressure).After finishing said process, carry out warming temperature, the kiln vacuum is evacuated to 30Pa (absolute pressure), after 6 hours, make extract temperature liter reach 53 ℃, get final product to such an extent that be the former powder of spongiform drying, moisture content is 0.5～2.0%, and decylenic acid content is 70.0～90.0%
Embodiment three
Before producing utensil is carried out ultraviolet disinfection, get the royal jelly magma distilled water diluting that meets " GB9697-88 royal jelly standard " salable product, magma and distilled water weight ratio are 1: 1.5.Filter through the above screen of 50 orders, remove impurity, the magma of removing impurity is poured in the basic solution for preparing in advance, the preparation of basic solution is with DH20 distilled water and adds an amount of NaOH adjusting, making pH value is 7.4, magma and distilled water weight ratio are 1: 2.5, through centrifugal stirrer 7 minutes stirring and dissolving of rotating speed uniform rotation with 10 rev/mins.With the magma solution apparatus,Soxhlet's of packing into, with ethanol is solvent, and after 120 minutes, it is an amount of to add ethanol again in 70 ℃ of refluxing extraction, continued reflux 125 minutes, put coldly, move into then in the extractor upper strata oily matter is isolated, when oily matter is heated to 65 ℃, the Hcl that adds 0.35mol/L is an amount of, making pH value is 3.2, puts coldly, filters.Filtrate is packed in the appropriate containers, airtight, deposited 90 minutes at storing chamber at-8 ℃ temperature condition.Take out filtrate and mix under 50 ℃ with ethanol and stir evenly, the weight proportion of ethanol and filtrate is 75%, natural sedimentation, extraction throw out.
Finish as stated above and extract is put into Stainless Steel Disc after the extraction and go into DT-735 vacuum freeze drier evaporator room, carry out the slow hardening knot with-24 ℃/hour cooling rate from room temperature.When the extract temperature is reduced to-27 ℃, kept constant temperature 80 minutes, make the thorough deep colling of extract.Meanwhile, water vapour coagulator is vacuumized, the pressure that makes evaporator room is in 45Pa (absolute pressure).After finishing said process, carry out warming temperature, the kiln vacuum is evacuated to 20Pa (absolute pressure), after 5 hours, make extract temperature liter reach 46 ℃, get final product to such an extent that be the former powder of spongiform drying, moisture content is 0.5～2.0%, and decylenic acid content is 70.0～90.0%.
The decylenic acid that the present invention extracted can keep original activeconstituents and effect under field conditions (factors), content and purity height, and constant product quality, technology is simple, and cost is easy to control.
Claims (6)
1, a kind of method of extracting decylenic acid from royal jelly is characterized in that: technical process is the magma dilution, filtering and impurity removing, and dissolving magma, reflux, extracting and separating, pH value is regulated, low-temperature storage, the mixed stirring, precipitation is extracted, vacuum lyophilization.
2, a kind of method of from royal jelly, extracting decylenic acid according to claim 1, it is characterized in that: specific embodiment is:
A, magma dilution: before producing utensil is carried out ultraviolet disinfection, get the royal jelly magma distilled water diluting that meets " GB9697-88 royal jelly standard " salable product;
B, filtering and impurity removing: the magma after the dilution is filtered through the above screen of 50 orders, removes impurity;
C, dissolving magma: the magma that will remove impurity is poured in the basic solution for preparing in advance, through agitator 5～10 minutes stirring and dissolving of rotating speed uniform rotation with 5～20 rev/mins, the preparation of basic solution is to add an amount of NaOH with distilled water to regulate, and making pH value is 7.0～7.8;
D, reflux: the apparatus,Soxhlet's of packing into of the magma solution after will dissolving, with ethanol be solvent in 60～75 ℃ of refluxing extraction after 60～180 minutes, it is an amount of to add ethanol again, continues reflux 100～150 minutes, puts cold;
E, extracting and separating: the magma solution after the reflux is moved in the extractor, upper strata oily matter is separated;
F, pH value regulate: when oily matter is heated to 50～80 ℃, add an amount of Hcl, making pH value is 2.0～4.5, puts coldly, filters;
G, low-temperature storage: filtrate is packed in the appropriate containers, airtight, under-5 ℃～-10 ℃ temperature condition, deposited 30～120 minutes;
H, the mixed stirring: take out filtrate after the low-temp storage, add ethanol mixing under 35～65 ℃ and stir, the weight proportion of ethanol and filtrate is (70～80): 100;
I, precipitation are extracted: natural sedimentation behind the mixing, extract;
J, vacuum lyophilization: the extract Stainless Steel Disc of packing into is entered the vacuum freeze drier evaporator room and carries out slow hardening knot from room temperature with-24 ℃/hour cooling rate, when the extract temperature is reduced to-25 ℃～-30 ℃, kept constant temperature 30～120 minutes, meanwhile water vapour coagulator is vacuumized, the pressure that makes evaporator room is at 30～60Pa, carry out warming temperature after finishing said process, the kiln vacuum is evacuated to 10～30Pa, after 4～6 hours, make extract temperature liter reach 40～53 ℃.
3, the method from royal jelly extraction decylenic acid as claimed in claim 1 or 2, it is characterized in that: during the magma dilution, magma and distilled water weight proportion are 1: 1～2.
4, the method from royal jelly extraction decylenic acid as claimed in claim 1 or 2, it is characterized in that: during dissolving magma, the weight proportion of magma and distilled water is 1: 1～5.
5, the method from royal jelly extraction decylenic acid as claimed in claim 1 or 2, it is characterized in that: when pH value was regulated, the volumetric molar concentration of the Hcl of adding was 0.2～0.5mol/L.
6, the method from royal jelly extraction decylenic acid as claimed in claim 1 or 2, it is characterized in that: the decylenic acid finished product that is extracted is for being the former powder of spongiform drying.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 00132077 CN1241893C (en) | 2000-12-14 | 2000-12-14 | Caproleic acid extracting process from royal jelly |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 00132077 CN1241893C (en) | 2000-12-14 | 2000-12-14 | Caproleic acid extracting process from royal jelly |
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| CN1357528A true CN1357528A (en) | 2002-07-10 |
| CN1241893C CN1241893C (en) | 2006-02-15 |
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| CN 00132077 Expired - Fee Related CN1241893C (en) | 2000-12-14 | 2000-12-14 | Caproleic acid extracting process from royal jelly |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103044240A (en) * | 2011-10-15 | 2013-04-17 | 山东华康蜂业有限公司 | Process for extracting 10-oxhydryl-2-caproleic acid from royal jelly |
| CN107641077A (en) * | 2017-11-22 | 2018-01-30 | 刘峰 | A kind of method that the decylenic acid of 10 hydroxyl 2 is extracted from royal jelly freeze-dried powder |
| CN108066272A (en) * | 2018-01-03 | 2018-05-25 | 杭州蜂情科技有限公司 | It is a kind of that there is the royal jelly extract for promoting collagen synthesis and its extracting method and its purposes |
| CN109105842A (en) * | 2018-07-24 | 2019-01-01 | 湖南省明园蜂业有限公司 | 10- hydroxyl-alpha-decene acid content processing method in a kind of raising royal jelly |
| CN113575898A (en) * | 2021-08-11 | 2021-11-02 | 杭州碧于天保健品有限公司 | Method for removing foreign matters in royal jelly slurry residue based on crystallization technology |
-
2000
- 2000-12-14 CN CN 00132077 patent/CN1241893C/en not_active Expired - Fee Related
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103044240A (en) * | 2011-10-15 | 2013-04-17 | 山东华康蜂业有限公司 | Process for extracting 10-oxhydryl-2-caproleic acid from royal jelly |
| CN107641077A (en) * | 2017-11-22 | 2018-01-30 | 刘峰 | A kind of method that the decylenic acid of 10 hydroxyl 2 is extracted from royal jelly freeze-dried powder |
| CN108066272A (en) * | 2018-01-03 | 2018-05-25 | 杭州蜂情科技有限公司 | It is a kind of that there is the royal jelly extract for promoting collagen synthesis and its extracting method and its purposes |
| CN109105842A (en) * | 2018-07-24 | 2019-01-01 | 湖南省明园蜂业有限公司 | 10- hydroxyl-alpha-decene acid content processing method in a kind of raising royal jelly |
| CN113575898A (en) * | 2021-08-11 | 2021-11-02 | 杭州碧于天保健品有限公司 | Method for removing foreign matters in royal jelly slurry residue based on crystallization technology |
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| Publication number | Publication date |
|---|---|
| CN1241893C (en) | 2006-02-15 |
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