CN104530168B - A kind of industrialized process for preparing of mogroside Ⅴ - Google Patents
A kind of industrialized process for preparing of mogroside Ⅴ Download PDFInfo
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- CN104530168B CN104530168B CN201410763087.8A CN201410763087A CN104530168B CN 104530168 B CN104530168 B CN 104530168B CN 201410763087 A CN201410763087 A CN 201410763087A CN 104530168 B CN104530168 B CN 104530168B
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- C07—ORGANIC CHEMISTRY
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- C07J17/00—Normal steroids containing carbon, hydrogen, halogen or oxygen, having an oxygen-containing hetero ring not condensed with the cyclopenta(a)hydrophenanthrene skeleton
- C07J17/005—Glycosides
Abstract
Present invention is disclosed the industrialized process for preparing of a kind of mogroside Ⅴ, including step: I, with extraction, evaporation prepare Momordia grosvenori aglycone crude product；II, with water, Momordia grosvenori aglycone crude product is configured to solution, filters insoluble matter；III, Momordia grosvenori aglycone solution is pumped into dynamic axial compression column preparing chromatography system, in post, filler is anti-phase spherical silica gel, applied sample amount is 0.1%～3%, in post, flowing is aqueous solutions of organic solvent mutually, the Initial Gradient first controlling aqueous solutions of organic solvent is 2: 8～4: 6, flow velocity is 100ml/min, eluting 30min～50min；Adjust gradient >=1, continue to be eluted to 50min～60min, the detection wavelength adjusting New UV Spectrophotometric detector is 203nm, from flowing start mutually to inject dynamic axial compression column preparing chromatography system carry out liquid chromatographic detection, the online eluent collecting corresponding chromatographic peak, obtains the purity mogroside Ⅴ more than 95%.Apply preparation method of the present invention, simplify process technique and can on-line real time monitoring, improve safety, saved cost, mogroside Ⅴ purity is preferable.
Description
Technical field
The present invention relates to the extraction field of Lo Han Guo fruit effective ingredient, technology of preparing is extracted in the industrialization particularly relating to a kind of mogroside Ⅴ.
Background technology
Fructus Momordicae [Siraitiagrosuenorii] is the fruit of cucurbitaceous plant Fructus Momordicae, it it is the natural product resource of a kind of great exploitation potential, mogroside is principle active component in Fructus Momordicae, and it is a kind of triterpene glucoside, has biological nature widely.Content and the highest composition of sugariness during wherein mogroside Ⅴ is Lo Han Guo fruit, its content is about 1%, and sugariness is equivalent to 300 times of sucrose, is main sweet ingredient.Mogroside has safety, and taste matter is good, and sugariness is high, and Heat stability is good is of light color, is affected characteristics such as little (pH value between 2～10) by external environment pH.China in this product of official approval in July, 1996 as food additive.
Fructus Momordicae commercial production generally uses crystallization recrystallization, chromatography or the two method for combined use.But no matter which kind of preparation method, its technique is the most loaded down with trivial details, the longest, and production efficiency is the lowest, and purity is the highest, it is impossible to obtain the product of more than 90% purity.Chinese patent (application number: 201210167052.9, denomination of invention: a kind of extraction mogroside Ⅴ and method of farnesol from Fructus Momordicae) describe the method used chromatography and crystallize the method extraction mogroside Ⅴ that recrystallization combines, process steps is lengthy and jumbled, and it is the highest to extract the product purity obtained.Owing to using flammable organic solvent in a large number in producing, such as ethyl acetate, petroleum ether, acetone etc. are as crystallization or solvent system, poor stability.
Chinese patent (application number: 200810073876.3) is separately had to describe a kind of method separating-purifying mogroside Ⅴ using two steps chromatography (using unformed purification on normal-phase silica gel and C18 reverse phase silica gel respectively).The method simplifies and more existing raisings in terms of product purity in step compared to conventional crystallization recrystallization method, but solvent for use such as dichloromethane, big to environment and safety hazard, separating rate is slow, and the shortcoming being difficult to on-line real time monitoring separation process.
Summary of the invention
Loaded down with trivial details for technique existing during tradition mogroside Ⅴ crude product refining, the problems such as purity is the highest, the purpose of the present invention aims to provide the industrialized process for preparing of a kind of mogroside Ⅴ, simplifies preparation method and has the characteristic of ON-LINE SEPARATION.
The above-mentioned purpose of the present invention is achieved through the following technical solutions, a kind of industrialized process for preparing of mogroside Ⅴ, including step: I, Fructus Momordicae raw material is extracted under heating, microwave or any one assosting effect ultrasonic with water, organic solvent or both mixed solvents, Fructus Momordicae extracting solution is obtained after solid-liquid separation, the method then using at least spraying, rotation to steam removes liquid, it is thus achieved that the Momordia grosvenori aglycone crude product of mogroside Ⅴ mass content 1%～20%；II, with water Momordia grosvenori aglycone crude product is configured to solution, filters and remove insoluble matter；nullIII、Momordia grosvenori aglycone solution is pumped into dynamic axial compression column preparing chromatography system，In post, filler is the anti-phase spherical silica gel of 10 μm～50 μm，Applied sample amount is corresponding with Momordia grosvenori aglycone crude product quality，Flowing is mutually for mass concentration 10%～90% and have the aqueous solutions of organic solvent of adjustable gradient in post，The Initial Gradient first controlling aqueous solutions of organic solvent is 2: 8～4: 6，Flow velocity is 100ml/min，Eluting 30min～50min，The gradient then adjusting aqueous solutions of organic solvent is 1: 1～9: 1，Continue to be eluted to 50min～60min，The detection wavelength adjusting New UV Spectrophotometric detector is 203nm，From flowing and starting flowing mutually, dynamic axial compression column preparing chromatography system is carried out liquid chromatographic detection，The online eluent collecting corresponding chromatographic peak，Obtain the purity mogroside Ⅴ more than 95%.
Further, organic solvent described in step I and step III is at least methanol, ethanol, acetonitrile.
Further, described anti-phase spherical silica gel is the n-octadecane base reverse phase silica gel grain of particle diameter 10 μm.
Further, described anti-phase spherical silica gel is the n-octadecane base reverse phase silica gel grain of particle diameter 22 μm.
Further, described anti-phase spherical silica gel is the n-octadecane base reverse phase silica gel grain of particle diameter 50 μm.
Further, in described post, flowing is ethanol and water mutually, and Initial Gradient is 2: 8～3: 7.
Further, in described post, flowing is acetonitrile and water mutually, and Initial Gradient is 2: 8～3: 7.
Further, in described post, flowing is methanol and water mutually, and Initial Gradient is 2: 8～4: 6.
The enforcement of technology of preparing scheme of the present invention, it compares to the remarkable advantage that conventional preparation techniques had: directly use the Momordia grosvenori aglycone crude product after thick extraction to prepare mogroside Ⅴ, the pre-treatment loaded down with trivial details without large amount of complex and last handling process, solvent for use is cheap, safety, and isolated and purified process can on-line real time monitoring, substantially increase safety, saved cost, it is adaptable to large-scale industrial production.High performance liquid chromatography finally measures display, and mogroside Ⅴ purity is more than 95%, the most miscellaneous is less than 5%.
Accompanying drawing explanation
Fig. 1 is the high-performance liquid chromatogram determination collection of illustrative plates of original Momordia grosvenori aglycone crude product.
Fig. 2 is the high-performance liquid chromatogram determination collection of illustrative plates with the isolated and purified mogroside Ⅴ of dynamic axial compression column being filled with 10 μm n-octadecane base reverse phase silica gel filler (applied sample amount 600mg).
Fig. 3 is the high-performance liquid chromatogram determination collection of illustrative plates with the isolated and purified mogroside Ⅴ of dynamic axial compression column being filled with 10 μm n-octadecane base reverse phase silica gel filler (applied sample amount 1g).
Fig. 4 is the high-performance liquid chromatogram determination collection of illustrative plates with the isolated and purified mogroside Ⅴ of dynamic axial compression column being filled with 10 μm n-octadecane base reverse phase silica gel filler (applied sample amount 3g).
Fig. 5 be be filled with 10 μm n-octadecane base reverse phase silica gel filler (applied sample amount 3g) the isolated and purified mogroside Ⅴ of dynamic axial compression column prepare collection of illustrative plates.
Detailed description of the invention
Loaded down with trivial details for the technique in the presence of the existing subtractive process of mogroside Ⅴ crude product in view of disclosed in background technology of the present invention, the problems such as purity is the highest, innovation proposes the industrialized process for preparing of a kind of mogroside Ⅴ.The method can directly use thick Momordia grosvenori aglycone crude product after extracting to prepare mogroside Ⅴ, the pre-treatment loaded down with trivial details without large amount of complex and last handling process, solvent for use is cheap, safety, and isolated and purified process can on-line real time monitoring from the point of view of the general introduction of preparation method of the present invention, it includes the preparation of Momordia grosvenori aglycone crude product, utilize Momordia grosvenori aglycone crude product configuration solution and use high performance liquid chromatography (HPLC) method optimization and judge the optimal separation purification condition of mogroside Ⅴ, it is achieved high efficiency extraction.
From the point of view of step by step, step I: under heating, microwave, any one assosting effect such as ultrasonic, Fructus Momordicae raw material is extracted with water or organic solvent or both mixed solvents, Fructus Momordicae extracting solution is obtained after solid-liquid separation, the method then using at least spraying, rotation to steam removes liquid, obtaining the Momordia grosvenori aglycone crude product of mogroside Ⅴ mass content 1%～20%, its high-performance liquid chromatogram determination collection of illustrative plates is as shown in Figure 1.
Step II, with water Momordia grosvenori aglycone crude product is configured to solution, filters and remove insoluble matter.
nullStep III、Momordia grosvenori aglycone solution is pumped into dynamic axial compression column preparing chromatography system，In post, filler is the anti-phase spherical silica gel of 10 μm～50 μm，Applied sample amount is corresponding with Momordia grosvenori aglycone crude product quality，Flowing is mutually for mass concentration 10%～90% and have the aqueous solutions of organic solvent of adjustable gradient in post，The Initial Gradient first controlling aqueous solutions of organic solvent is 2: 8～4: 6，Flow velocity is 100ml/min，Eluting 30min～50min，The gradient then adjusting aqueous solutions of organic solvent is 1: 1～9: 1，Continue to be eluted to 50min～60min，The detection wavelength adjusting New UV Spectrophotometric detector is 203nm，From flowing and starting flowing mutually, dynamic axial compression column preparing chromatography system is carried out liquid chromatographic detection，The online eluent collecting corresponding chromatographic peak，Obtain the purity mogroside Ⅴ more than 95%.
Under above-mentioned general principle technical scheme instructs, process that what it was the most concrete or real be preferable to carry out may is that and is prepared as ordinary skill in the art means due to the dry crude product of Fructus Momordicae, almost without difference in the subsequent process steps of the present invention, therefore in the preferred embodiment and some embodiments described later, the description of step I will be omitted.After the preparation completing Momordia grosvenori aglycone crude product, take 600mg Momordia grosvenori aglycone crude product water and be configured to the solution of mass concentration 0.3%, and be filtered to remove insoluble matter.Then this Momordia grosvenori aglycone solution is pumped in dynamic axial compression column preparing chromatography system.Here column dimension is Φ 50mm × 250mm, and in post, filler is the n-octadecane base reverse phase silica gel grain of 10 μm, and applied sample amount is also 600mg, and in post, flowing is the mixed solution of food-grade ethanol and water mutually, and Initial Gradient scope is 2: 8～3: 7.Consider for food safety, therefore preferably food-grade ethanol.Coutroi velocity is 100ml/min, elution time 30min；Afterwards the gradient of above-mentioned aqueous solutions of organic solvent is adjusted to 9: 1, continues to be eluted to 50min, terminate a separation cycle with this.During eluting, the detection wavelength adjusting New UV Spectrophotometric detector is 203nm, dynamic axial compression column preparing chromatography system is carried out liquid chromatographic detection, the online eluent collecting corresponding chromatographic peak, occur that the corresponding time is collected in the eluent of 12min～14min according to chromatographic peak, as in figure 2 it is shown, the distillate obtained analyzes mogroside Ⅴ purity through HPLC reaches 99%.
For showing the variable embodiment of preparation method of the present invention and the efficient suitability more fully, below by way of more embodiments, the present invention will be described in more detail.
Embodiment 1, after the preparation completing Momordia grosvenori aglycone crude product, takes 1g Momordia grosvenori aglycone crude product water and is configured to the solution of mass concentration 0.3%, and be filtered to remove insoluble matter.Then this Momordia grosvenori aglycone solution is pumped in dynamic axial compression column preparing chromatography system.Same column dimension is Φ 50mm × 250mm, and in post, filler is the n-octadecane base reverse phase silica gel grain of 10 μm, and applied sample amount is also 1g, in post, flowing is the mixed solution of ethanol and water mutually, Initial Gradient scope is 2: 8～3: 7, and coutroi velocity is 100ml/min, elution time 30min；Afterwards the gradient of above-mentioned aqueous solutions of organic solvent is adjusted to 9: 1, continues to be eluted to 50min, terminate a separation cycle with this.During eluting, the detection wavelength adjusting New UV Spectrophotometric detector is 203nm, dynamic axial compression column preparing chromatography system is carried out liquid chromatographic detection, the online eluent collecting corresponding chromatographic peak, occur that the corresponding time is collected in the eluent of 12min～14min according to chromatographic peak, as it is shown on figure 3, it is 98.5% that the distillate obtained analyzes mogroside Ⅴ purity through HPLC.
Embodiment 2, after the preparation completing Momordia grosvenori aglycone crude product, takes 3g Momordia grosvenori aglycone crude product water and is configured to the solution of mass concentration 1%, and be filtered to remove insoluble matter.Then this Momordia grosvenori aglycone solution is pumped in dynamic axial compression column preparing chromatography system.Same column dimension is Φ 50mm × 250mm, and in post, filler is the n-octadecane base reverse phase silica gel grain of 10 μm, and applied sample amount is also 3g, in post, flowing is the mixed solution of ethanol and water mutually, Initial Gradient scope is 2: 8～3: 7, and coutroi velocity is 100ml/min, elution time 50min；Afterwards the gradient of above-mentioned aqueous solutions of organic solvent is adjusted to 9: 1, continues to be eluted to 60min, terminate a separation cycle with this.During eluting, the detection wavelength adjusting New UV Spectrophotometric detector is 203nm, dynamic axial compression column preparing chromatography system is carried out liquid chromatographic detection, the online eluent collecting corresponding chromatographic peak, occur that the corresponding time is collected in the eluent of 10min～15min according to chromatographic peak, as shown in Figure 4 with shown in Fig. 5, it is 97.4% that the distillate obtained analyzes mogroside Ⅴ purity through HPLC.
Embodiment 3 the present embodiment uses the n-octadecane base reverse phase silica gel grain of 22 μm, and remaining technique is all with embodiment 2, and gained mogroside Ⅴ purity is 97.0%
Embodiment 4 uses flowing to be methanol and water mutually, and gradient scope is 2: 8～4: 6, and coutroi velocity is 100ml/min, elution time 50min；Afterwards the gradient of above-mentioned aqueous solutions of organic solvent being adjusted to 9: 1, continue to be eluted to 60min, remaining technique is all with embodiment 2, and gained mogroside Ⅴ purity is 97.5%.
Embodiment 5 uses flowing to be acetonitrile and water mutually, and gradient scope is 2: 8～3: 7, and coutroi velocity is 100ml/min, elution time 30min；Afterwards the gradient of above-mentioned aqueous solutions of organic solvent being adjusted to 5: 5, continue to be eluted to 60min, remaining technique is all with embodiment 2, and gained mogroside Ⅴ purity is 98.1%.
The most many embodiments are introduced visible, by the preparation method of the present invention, can directly use the Momordia grosvenori aglycone crude product after thick extraction to prepare mogroside Ⅴ, the pre-treatment loaded down with trivial details without large amount of complex and last handling process, solvent for use is cheap, safety, and isolated and purified process can on-line real time monitoring, substantially increase safety, save cost, it is adaptable to large-scale industrial production.High performance liquid chromatography finally measures display, and mogroside Ⅴ purity is more than 95%, the most miscellaneous is less than 5%.
The above, it it is only presently preferred embodiments of the present invention, not the present invention is made any pro forma restriction, although the present invention is disclosed above with preferred embodiment, but it is not limited to the present invention, any those skilled in the art, in the range of without departing from technical solution of the present invention, when the technology contents of available the disclosure above makes a little variation or is modified to the Equivalent embodiments of equivalent variations, in every case it is the content without departing from technical solution of the present invention, any simple modification above example made according to the technical spirit of the present invention, equivalent variations and modification, all still fall within the range of technical solution of the present invention.
Claims (8)
1. the industrialized process for preparing of a mogroside Ⅴ, it is characterised in that include step:
I, Fructus Momordicae raw material is extracted under heating, microwave or any one assosting effect ultrasonic with water, organic solvent or both mixed solvents, Fructus Momordicae extracting solution is obtained after solid-liquid separation, the method then using at least spraying, rotation to steam removes liquid, it is thus achieved that the Momordia grosvenori aglycone crude product of mogroside Ⅴ mass content 1%～20%；
II, with water Momordia grosvenori aglycone crude product is configured to solution, filters and remove insoluble matter；
nullIII、Momordia grosvenori aglycone solution is pumped into dynamic axial compression column preparing chromatography system，In post, filler is the anti-phase spherical silica gel of 10 μm～50 μm，Applied sample amount is 0.1%～3%，Flowing is mutually for mass concentration 10%～90% and have the aqueous solutions of organic solvent of adjustable gradient in post，The Initial Gradient first controlling aqueous solutions of organic solvent is 2: 8～4: 6，Flow velocity is 100ml/min，Eluting 30min～50min，The gradient then adjusting aqueous solutions of organic solvent is 1: 1～9: 1，Continue to be eluted to 50min～60min，The detection wavelength adjusting New UV Spectrophotometric detector is 203nm，From flowing and starting flowing mutually, dynamic axial compression column preparing chromatography system is carried out liquid chromatographic detection，The online eluent collecting corresponding chromatographic peak，Obtain the purity mogroside Ⅴ more than 95%.
The industrialized process for preparing of mogroside Ⅴ the most according to claim 1, it is characterised in that: described in step I and step III, organic solvent is at least methanol, ethanol, acetonitrile.
The industrialized process for preparing of mogroside Ⅴ the most according to claim 1, it is characterised in that: described anti-phase spherical silica gel is the n-octadecane base reverse phase silica gel grain of particle diameter 10 μm.
The industrialized process for preparing of mogroside Ⅴ the most according to claim 1, it is characterised in that: described anti-phase spherical silica gel is the n-octadecane base reverse phase silica gel grain of particle diameter 22 μm.
The industrialized process for preparing of mogroside Ⅴ the most according to claim 1, it is characterised in that: described anti-phase spherical silica gel is the n-octadecane base reverse phase silica gel grain of particle diameter 50 μm.
The industrialized process for preparing of mogroside Ⅴ the most according to claim 1, it is characterised in that: in described post, flowing is ethanol and water mutually, and Initial Gradient is 2: 8～3: 7.
The industrialized process for preparing of mogroside Ⅴ the most according to claim 1, it is characterised in that: in described post, flowing is acetonitrile and water mutually, and Initial Gradient is 2: 8～3: 7.
The industrialized process for preparing of mogroside Ⅴ the most according to claim 1, it is characterised in that: in described post, flowing is methanol and water mutually, and Initial Gradient is 2: 8～4: 6.
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| NZ549739A (en) | 2006-09-07 | 2009-01-31 | Biovittoria Ltd | Sweetening compositions and processes for preparing them |
| CN104892717B (en) * | 2015-06-18 | 2017-05-31 | 湖南华诚生物资源股份有限公司 | A kind of technical grade preparative liquid chromatography separation method of momordica glycoside V |
| TWI729232B (en) * | 2016-10-24 | 2021-06-01 | 大陸商桂林吉福思羅漢果有限公司 | Extracts from fruits of the cucurbitaceae family, and methods of preparing thereof |
| CN110343141B (en) * | 2019-07-22 | 2021-09-07 | 湖南艾达伦科技有限公司 | Preparation method and application of high-content mogroside monomer product |
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| CN103570789A (en) * | 2013-11-14 | 2014-02-12 | 南宁麦斯威生物科技有限公司 | Preparation method of high-purity momordica glycosides |
| CN104059122B (en) * | 2014-05-06 | 2016-04-27 | 义乌章舸生物工程有限公司 | A kind of preparation method of high-purity Momordica grosvenori saponin(e V |
| CN103923152B (en) * | 2014-05-08 | 2015-11-04 | 青岛润德生物科技有限公司 | A kind of extracting method of mogroside V |
| CN104086614B (en) * | 2014-07-25 | 2016-01-20 | 湖南华诚生物资源股份有限公司 | A kind of preparation method being applicable to industrial Fructus Monordicae extract |
| CN104086615B (en) * | 2014-07-29 | 2015-12-09 | 桂林实力科技有限公司 | A kind of method preparing mogroside V from Grosvenor Momordica |
| CN104098641B (en) * | 2014-07-29 | 2016-03-02 | 桂林实力科技有限公司 | A kind of method extracting mogroside V from Grosvenor Momordica |
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