CN1357370A - Extraction process of effective component in Maka - Google Patents
Extraction process of effective component in Maka Download PDFInfo
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- CN1357370A CN1357370A CN 01138330 CN01138330A CN1357370A CN 1357370 A CN1357370 A CN 1357370A CN 01138330 CN01138330 CN 01138330 CN 01138330 A CN01138330 A CN 01138330A CN 1357370 A CN1357370 A CN 1357370A
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- meyenii walp
- lepidinm meyenii
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Abstract
The present invention relates to the field of natural product chemistry and medicine chemistry and provides a method of extracting effective component from plant root and stem. Fresh maka root after being wvacuum drying and ground into powder is supercritical CO2 extracted with CO2 and entrainer to obtain extraction liquid and the extraction liquid is produced into granule through vacuum evaporation to concentrate, mixing with water and emulsifier, homogenization to emulsify and spray to dry. It has high material utilization and effective component extracting rate, and the product has stable pharmacological effect and is easy to dissolve, eat, transport and store.
Description
Technical field
The invention belongs to natural product chemistry and pharmaceutical chemistry field, particularly from plant roots and stems, extract, concentrate the method for active ingredient.
Background technology
Natural medicine-food dual purpose plant Lepidinm meyenii Walp (Lepidium meyenii walp, be commonly called as Maca) in mountain area, Andean, South America the cultivation history in thousands of years has been arranged, and are one of indispensable crops in those areas, the Lepidinm meyenii Walp root is used to strengthen energy as food and medical herbs traditionally, resisting fatigue, the treatment female dimacteric syndrome, sexual function improving etc., and these effects have obtained the proof of modern medicine study, as the aminoacid in the Lepidinm meyenii Walp root, sterols etc. have significant antifatigue effect, alkaloid, saponins etc. have good regulating action to the endocrine of climacteric women, make Lepidinm meyenii Walp have the effect that substitutes synthetic estradiol, Lepidinm meyenii Walp alkene, the effect that materials such as Lepidinm meyenii Walp amide and benzyl isothiocyanate can play sexual function improving and improve fertility.
The Lepidinm meyenii Walp health promoting product great majority of selling on the international market are to be raw material with Lepidinm meyenii Walp root dry powder directly at present, its preparation method is: the Lepidinm meyenii Walp root is dried naturally or dries in drying baker, be ground into powder then, load into capsule or tabletting is made tablet, even just directly with the box-packed finished product that promptly obtains of powder." the VITA-MYR MACA " of the such product such as the U.S., " the Maca Andina " of Peru etc. are to be used for food or food supplement, and health-care effect is not obvious, and range of application is extremely limited to.
Natural plant extracts is the important trend of international health product exploitation, the people that deeply make of medical research recognize that most of disease has multiple cause, the Lepidinm meyenii Walp concentrated extract is the extracted form natural plant elite that contains the various active composition, without any side effects, it sets out from different perspectives to preventing multiple disease that original effect is arranged.Existing Lepidinm meyenii Walp root extracts the concentrate preparation method: with the Lepidinm meyenii Walp root is raw material, at first with containing alcoholic acid aqueous solution lixiviate raw material, separation and Extraction liquid, raw material water and organic solvent mixed liquor again extracts one time as 90% ethanol etc. again, carry out gradient elution by reversed-phase liquid chromatography, substep is collected, and concentrates thereby make in the Lepidinm meyenii Walp active ingredient obtain initial gross separation, and concentrated solution obtains the Lepidinm meyenii Walp root by drying and extracts the concentrate powder.See U.S. Pat 6267995, " Extract of Lepidium Meyenii roots for pharmaceutical applications " its date of application is on March 3rd, 1999, July 31 calendar year 2001 Shen Qing Publication day.Though said method has carried out certain concentrating and separating to active ingredient with health role in the Lepidinm meyenii Walp root, but still having deficiencies such as the effective constituent extraction ratio is low, separating step is loaded down with trivial details, active ingredient less stable, incompatibility large-scale production, these problems have had a strong impact on application and the popularization of Lepidinm meyenii Walp in fields such as food, health product.
Summary of the invention
The invention provides a kind of Lepidinm meyenii Walp active ingredient extracting method, adopt supercritical CO
2Abstraction technique replaces traditional extraction and separation technology, and control vacuum drying temperature and thickening temperature, thereby to preserve the raw material active ingredient, to improve its extraction ratio raising raw material availability.
Lepidinm meyenii Walp active ingredient extracting method of the present invention, comprise drying, pulverizing, extraction successively, concentrate and the drying and granulating program, it is characterized in that: (1) fresh Lepidinm meyenii Walp is behind vacuum drying, and it is standby to be ground into powder, and (2) adopt supercritical CO with the Lepidinm meyenii Walp root powder in (1)
2The abstraction technique extraction, it is standby to obtain extracting solution, and (3) extracting solution vacuum evaporation concentrates, and (4) concentrated solution adds entry and emulsifying agent, spray-drying process after the emulsifying.
In the described Lepidinm meyenii Walp active ingredient extracting method, supercritical CO
2Abstraction technique can be used CO
2+ entrainer extracts, and entrainer is one or both the mixed organic solvents in ethanol, acetone, ethyl acetate, the normal hexane, and entrainer accounts for 5～30% of total extractant volume content.
Described Lepidinm meyenii Walp active ingredient extracting method, it is further characterized in that: vacuum is 45～60 ℃ of 0.02～0.08Mpa, temperature during (1) vacuum drying, and (2) extracting pressure is 25～32Mpa, 35～45 ℃ of extraction temperature, 2～4 hours extraction time, CO
2Flow velocity is 10～15Kg/Kg raw material h, (3) vacuum evaporation concentrates vacuum 0.70～0.85Mpa, 41～57 ℃ of temperature, (4) emulsifying agent of spray-drying process is a kind of or its mixture in arabic gum, maltodextrin, modified starch, monoglyceride, the corn syrup, emulsifier aqueous solution concentration is 1～4%, and emulsifier aqueous solution and concentrated extracting solution weight ratio are 1.0～2.0: 1.
In the described Lepidinm meyenii Walp active ingredient extracting method, vacuum evaporation concentrates system and places falling film type vacuum evaporator to carry out extracting solution, emulsifying is undertaken by the equal stock pump of high pressure, homogenization pressure 25～40Mpa, import the hig h-speed centrifugal spray drying device then, 80～90 ℃ of feeding temperatures, 180～190 ℃ of inlet temperature, 70～90 ℃ of leaving air temps.
The present invention adopts vacuum drying, supercritical extraction technique and spray drying technology, has improved extraction concentration technique in the past greatly:
The first, improved raw material availability, the active ingredient extraction ratio has also improved over half, and efficacy stability extracts concentrate and has more remarkable health care;
Second, dry, uniform fine-powdered that the extraction concentrate of preparation is, be easy to dissolving, instant edible, transportation and storage, and be fit to continue to be processed into dosage forms such as various capsules, tablet, electuary, wherein continue to process the tablet that obtains and have matrix type controlled release effect, active ingredient is easier to be absorbed by the body;
The 3rd, technology advanced person makes preparation process standardization, standardization, easy, and solvent is saved greatly, and the production cycle shortens greatly, thereby can carry out large-scale production;
The 4th, by spray drying technology, avoided deficiencies such as pueraria root powder and common Lepidinm meyenii Walp extracting solution product mouthfeel, abnormal smells from the patient be not good, make purposes and suitable crowd more extensive.
Adopt method of the present invention, obtain the concentrated extract powder of active ingredient in the Lepidinm meyenii Walp root at last.Detect effective component content in this concentrated powder, wherein fatty acid total amount is 20～40%, benzyl isothiocyanate content is 10～15%, Lepidinm meyenii Walp amide (macamides) and Lepidinm meyenii Walp alkene (macaenes) total content are 7～14%, sterol content is 2～8%, VC content is 0.1～0.4%, VB1 content is 0.003～0.008%, VB2 content is 0.002～0.006%.
The specific embodiment
Embodiment one:
Gather fresh Lepidinm meyenii Walp, clean, remove stem and leaf, the Lepidinm meyenii Walp root places vacuum drying cabinet to dry under 0.05Mpa, 60 ℃ to moisture to reach 8%, pulverizes and by 20 eye mesh screens, obtains dry Lepidinm meyenii Walp root powder with pulverizer; Powder is put into the container type extractor, adopt supercritical CO
2Abstraction technique is used CO
2The extraction of+entrainer, entrainer is selected 95% ethanol, and content is 20% of total extractant volume content, and extracting pressure is 29.5Mpa, and extraction temperature is 40 ℃, the extraction time is 4 hours, CO
2Flow velocity is 15kg/kg raw material h, CO
2Can through separate reenter in the extractor after freezing recycling, the ethanol extract that obtains places falling film type vacuum evaporator, in vacuum is 0.82Mpa, and temperature is a concentrated extracting solution and reclaim ethanol under 43 ℃ of states, thereby obtains the concentrated extracting solution of active ingredient in the Lepidinm meyenii Walp root; In concentrated extracting solution, add suitable water and emulsifying agent, the emulsifying agent that uses is pressed the blended emulsifier of 1: 1.5 mass ratio as arabic gum, maltodextrin, emulsifier aqueous solution concentration is 1.5%, emulsion and concentrated extracting solution mass ratio are 1.3: 1, and by the equal stock pump emulsifying of high pressure, homogenization pressure is 30Mpa, import the hig h-speed centrifugal spray drying device then, 80 ℃ of feeding temperatures, 180 ℃ of inlet temperature, 90 ℃ of leaving air temps.Through cooling gained water content 4.1%, weight is that the powder of MAKA dry powder 3.2% is exactly an active ingredient concentrated extract in the final Lepidinm meyenii Walp root.Detect effective component content in this concentrated extract powder, wherein fatty acid total amount is 32.4%, benzyl isothiocyanate content is 10.5%, Lepidinm meyenii Walp amide (macamides) and Lepidinm meyenii Walp alkene (macaenes) total content are 13.2%, sterol content is 7.5%, VC content is 0.15%, VB1 content is 0.007%, VB2 content is 0.004%.
Embodiment two:
The basic step of preparation method is with embodiment one, partial parameters and condition can change as follows: the Lepidinm meyenii Walp root places vacuum drying cabinet to dry under 0.08Mpa, 45 ℃ to moisture to reach 7%, entrainer is 95% ethanol and the ethyl acetate mixed organic solvents by 2: 1 volume ratios during supercritical extraction, content is 7% of total extractant volume content, extracting pressure is 25Mpa, extraction temperature is 35 ℃, and the extraction time is 2 hours, CO
2Flow velocity is 10kg/kg raw material h, and the organic solvent extraction liquid that obtains is 0.7Mpa in vacuum, and temperature is vacuum concentration and recovery under 57 ℃ of states; Concentrated extracting solution carries out emulsifying with maltodextrin and corn syrup by the blended emulsifier of 2: 3 mass ratioes, and homogenization pressure is 25Mpa, and the feeding temperature during centrifugal spray drying is 82 ℃, 185 ℃ of inlet temperature, 87 ℃ of leaving air temps.Through cooling gained water content 4.0%, weight is that the powder of MAKA dry powder 3.0% is exactly an active ingredient concentrated extract in the final Lepidinm meyenii Walp root.Wherein effective component content is: fatty acid total amount 27.8%, benzyl isothiocyanate content 14.7%, Lepidinm meyenii Walp amide (macamides) and Lepidinm meyenii Walp alkene (macaenes) total content 10.1%, sterol content 7.9%, VC content 0.2%, VB1 content 0.004%, VB2 content 0.003%.
Embodiment three:
The basic step of preparation method is with embodiment one, partial parameters and condition can change as follows: the Lepidinm meyenii Walp root places vacuum drying cabinet to dry under 0.02Mpa, 60 ℃ to moisture to reach 9%, entrainer is acetone and the normal hexane mixed organic solvents by 3: 1 volume ratios during supercritical extraction, account for 30% of total extractant volume content, extracting pressure is 32Mpa, extraction temperature is 45 ℃, and the extraction time is 3 hours, CO
2Flow velocity is 12kg/kg raw material h, and the organic solvent extraction liquid that obtains is 0.85Mpa in vacuum, and temperature is vacuum concentration and recovery under 50 ℃ of states; Concentrated extracting solution carries out emulsifying with monoglyceride and maltodextrin by the blended emulsifier of 1: 3 mass ratio, the emulsifying agent water concentration is 2.0%, emulsion and concentrated extracting solution weight ratio are 1.1: 1, homogenization pressure is 40Mpa, feeding temperature during centrifugal spray drying is 84 ℃, 188 ℃ of air intakes, 80 ℃ of leaving air temps.Through cooling gained water content 4.2%, weight is that the powder of MAKA dry powder 3.3% is exactly an active ingredient concentrated extract in the final Lepidinm meyenii Walp root.The concentrated extract powder weight that obtains at last is 3.4% of a MAKA dry powder, and effective component content is: fatty acid total amount 35.3%, benzyl isothiocyanate content 10.5%, Lepidinm meyenii Walp amide (macamides) and Lepidinm meyenii Walp alkene (macaenes) total content 14.0%, sterol content 6.5%, VC content 0.2%, VB1 content 0.004%, VB2 content 0.003%.
Claims (4)
1. Lepidinm meyenii Walp active ingredient extracting method comprises drying, pulverizing, extraction successively, concentrates and the drying and granulating program, it is characterized in that:
(1) fresh Lepidinm meyenii Walp is behind vacuum drying, and it is standby to be ground into powder,
(2) the Lepidinm meyenii Walp root powder in (1) is adopted the extraction of supercritical CO 2 abstraction technique, it is standby to obtain extracting solution,
(3) extracting solution vacuum evaporation concentrates,
(4) concentrated solution adds entry and emulsifying agent, spray-drying process after the emulsifying.
2. Lepidinm meyenii Walp active ingredient extracting method as claimed in claim 1 is characterized in that: supercritical CO
2Abstraction technique is for using CO
2+ entrainer extracts, and entrainer is one or both the mixed organic solvents in ethanol, acetone, ethyl acetate, the normal hexane, and entrainer accounts for 5～30% of total extractant volume content.
3. Lepidinm meyenii Walp active ingredient extracting method as claimed in claim 2 is characterized in that:
(1) vacuum is 45～60 ℃ of 0.02～0.08Mpa, temperature during vacuum drying,
(2) extracting pressure is 25～32Mpa, 35～45 ℃ of extraction temperature, and 2～4 hours extraction time,
CO
2Flow velocity is 10～15Kg/Kg raw material h,
(3) vacuum evaporation concentrates vacuum 0.70～0.85Mpa, 41～57 ℃ of temperature,
(4) emulsifying agent of spray-drying process is a kind of or its mixture in arabic gum, maltodextrin, modified starch, monoglyceride, the corn syrup, and emulsifier aqueous solution concentration is 1～4%, emulsifying agent
Aqueous solution and concentrated extracting solution weight ratio are 1.0～2.0: 1.
4. Lepidinm meyenii Walp active ingredient extracting method as claimed in claim 3 is characterized in that:
Vacuum evaporation concentrates system and places falling film type vacuum evaporator to carry out extracting solution, and emulsifying is undertaken by the equal stock pump of high pressure, homogenization pressure 25～40Mpa, import the hig h-speed centrifugal spray drying device then, 80～90 ℃ of feeding temperatures, 180～190 ℃ of inlet temperature, 70～90 ℃ of leaving air temps.
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| Application Number | Priority Date | Filing Date | Title |
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| CNB011383305A CN1166387C (en) | 2001-12-20 | 2001-12-20 | Extraction process of effective component in Maka |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB011383305A CN1166387C (en) | 2001-12-20 | 2001-12-20 | Extraction process of effective component in Maka |
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| CN1357370A true CN1357370A (en) | 2002-07-10 |
| CN1166387C CN1166387C (en) | 2004-09-15 |
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Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CZ297984B6 (en) * | 2004-08-26 | 2007-05-16 | Naturprodukt Cz Spol. S R. O. | Foodstuff supplement based on silymarin |
| CN102524465A (en) * | 2012-02-22 | 2012-07-04 | 红云红河烟草(集团)有限责任公司 | Method for preparing maca health-care Puer tea cream |
| CN102579547A (en) * | 2012-03-26 | 2012-07-18 | 张丽琴 | Method for extracting active ingredients of maca |
| CN102626171A (en) * | 2012-03-30 | 2012-08-08 | 云南省农业科学院高山经济植物研究所 | Health care food containing maca and production process thereof |
| CN102697039A (en) * | 2012-05-31 | 2012-10-03 | 昆明理工大学 | Preparation method of Maca active extracts |
| CN102742840A (en) * | 2012-07-16 | 2012-10-24 | 西藏然康科技有限公司 | Maca Cordyceps buccal tablet and preparation method thereof |
| CN102895281A (en) * | 2012-11-05 | 2013-01-30 | 江苏江大源生态生物科技有限公司 | Method for extracting active ingredient from maca |
| CN102987366A (en) * | 2012-10-29 | 2013-03-27 | 李俊霖 | Fine maca tablets and preparation method thereof |
| CN103622123A (en) * | 2013-11-26 | 2014-03-12 | 江苏江大源生态生物科技有限公司 | Maca function beverage and preparation method thereof |
| CN104207016A (en) * | 2014-07-30 | 2014-12-17 | 理想科技集团有限公司 | Rice noodles with MACA and preparation method thereof |
| CN104356178A (en) * | 2014-12-02 | 2015-02-18 | 丽江百岁坊生物科技开发有限公司 | Preparation method of glucosinolate and benzyl isothiocyanate as metabolite of glucosinolate |
| CN104523803A (en) * | 2015-01-14 | 2015-04-22 | 昆明博尚生物技术有限公司 | Preparation method of extract preserving natural flavor of maca |
| CN105348357A (en) * | 2015-12-03 | 2016-02-24 | 中国科学院过程工程研究所 | Lepidium meyenii saponin as well as preparation method and application thereof |
| CN105361183A (en) * | 2015-11-06 | 2016-03-02 | 孟令刚 | Process for preparing maca particle powder |
| CN105524807A (en) * | 2016-02-02 | 2016-04-27 | 贵州茅台酒厂集团技术开发公司 | Maca extracting and maca wine producing process |
| CN105712896A (en) * | 2016-01-22 | 2016-06-29 | 中山优诺生物科技发展有限公司 | Method for efficiently preparing macamides monomers from Lepidium meyenii |
-
2001
- 2001-12-20 CN CNB011383305A patent/CN1166387C/en not_active Expired - Fee Related
Cited By (20)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CZ297984B6 (en) * | 2004-08-26 | 2007-05-16 | Naturprodukt Cz Spol. S R. O. | Foodstuff supplement based on silymarin |
| CN102524465A (en) * | 2012-02-22 | 2012-07-04 | 红云红河烟草(集团)有限责任公司 | Method for preparing maca health-care Puer tea cream |
| CN102579547A (en) * | 2012-03-26 | 2012-07-18 | 张丽琴 | Method for extracting active ingredients of maca |
| CN102626171B (en) * | 2012-03-30 | 2015-08-05 | 云南省农业科学院高山经济植物研究所 | A kind of health food and production technology thereof containing agate coffee |
| CN102626171A (en) * | 2012-03-30 | 2012-08-08 | 云南省农业科学院高山经济植物研究所 | Health care food containing maca and production process thereof |
| CN102697039A (en) * | 2012-05-31 | 2012-10-03 | 昆明理工大学 | Preparation method of Maca active extracts |
| CN102742840A (en) * | 2012-07-16 | 2012-10-24 | 西藏然康科技有限公司 | Maca Cordyceps buccal tablet and preparation method thereof |
| CN102742840B (en) * | 2012-07-16 | 2013-10-23 | 西藏然康科技有限公司 | Maca Cordyceps buccal tablet and preparation method thereof |
| CN102987366A (en) * | 2012-10-29 | 2013-03-27 | 李俊霖 | Fine maca tablets and preparation method thereof |
| CN102895281A (en) * | 2012-11-05 | 2013-01-30 | 江苏江大源生态生物科技有限公司 | Method for extracting active ingredient from maca |
| CN103622123A (en) * | 2013-11-26 | 2014-03-12 | 江苏江大源生态生物科技有限公司 | Maca function beverage and preparation method thereof |
| CN104207016A (en) * | 2014-07-30 | 2014-12-17 | 理想科技集团有限公司 | Rice noodles with MACA and preparation method thereof |
| CN104356178A (en) * | 2014-12-02 | 2015-02-18 | 丽江百岁坊生物科技开发有限公司 | Preparation method of glucosinolate and benzyl isothiocyanate as metabolite of glucosinolate |
| CN104356178B (en) * | 2014-12-02 | 2017-04-19 | 丽江百岁坊生物科技开发有限公司 | Preparation method of glucosinolate and benzyl isothiocyanate as metabolite of glucosinolate |
| CN104523803A (en) * | 2015-01-14 | 2015-04-22 | 昆明博尚生物技术有限公司 | Preparation method of extract preserving natural flavor of maca |
| CN104523803B (en) * | 2015-01-14 | 2018-06-19 | 云南良旺生物技术有限公司 | A kind of preparation method for retaining the natural flavour mountaineous extract of maca |
| CN105361183A (en) * | 2015-11-06 | 2016-03-02 | 孟令刚 | Process for preparing maca particle powder |
| CN105348357A (en) * | 2015-12-03 | 2016-02-24 | 中国科学院过程工程研究所 | Lepidium meyenii saponin as well as preparation method and application thereof |
| CN105712896A (en) * | 2016-01-22 | 2016-06-29 | 中山优诺生物科技发展有限公司 | Method for efficiently preparing macamides monomers from Lepidium meyenii |
| CN105524807A (en) * | 2016-02-02 | 2016-04-27 | 贵州茅台酒厂集团技术开发公司 | Maca extracting and maca wine producing process |
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