CN109289242A - Method for preparing mogroside V by combined subcritical and molecular distillation - Google Patents
Method for preparing mogroside V by combined subcritical and molecular distillation Download PDFInfo
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- CN109289242A CN109289242A CN201811085219.0A CN201811085219A CN109289242A CN 109289242 A CN109289242 A CN 109289242A CN 201811085219 A CN201811085219 A CN 201811085219A CN 109289242 A CN109289242 A CN 109289242A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/12—Molecular distillation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07J—STEROIDS
- C07J17/00—Normal steroids containing carbon, hydrogen, halogen or oxygen, having an oxygen-containing hetero ring not condensed with the cyclopenta(a)hydrophenanthrene skeleton
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Abstract
本发明涉及一种利用亚临界和分子蒸馏联合制备罗汉果糖苷V的方法，其包括如下步骤：1）将罗汉果粉末进行亚临界萃取，获得罗汉果萃取物；2）将罗汉果萃取物进行分子蒸馏，得到含罗汉果糖苷V的轻组分。步骤1）中亚临界萃取时，温度为10－50℃，压力为0.5－2.0 MPa，时间为3－5 h。本发明方法包括原料粉碎预处理、亚临界萃取和分子蒸馏三个步骤，操作步骤简单便捷，耗时较短，适合规模化生产和应用；整个工艺过程中温度较低不会对香味物质进行破坏，对目标化合物影响较小，并且原料来自于自然界，在制备过程中并无引入有害物质，不存在有毒溶剂残留问题；采用本发明方法制备所得的罗汉果糖苷V纯度较高，纯度在94.6%以上。The present invention relates to a method for preparing Mogroside V by combining subcritical and molecular distillation, which comprises the following steps: 1) performing subcritical extraction on Luo Han Guo powder to obtain a Luo Han Guo extract; 2) performing molecular distillation on the Luo Han Guo extract to obtain Mogroside V-containing light fraction. Step 1) During mid-subcritical extraction, the temperature is 10-50 °C, the pressure is 0.5-2.0 MPa, and the time is 3-5 h. The method of the invention includes three steps of raw material pulverization pretreatment, subcritical extraction and molecular distillation, the operation steps are simple and convenient, the time consumption is short, and it is suitable for large-scale production and application; the temperature in the whole process is low and will not destroy the aroma substances , the impact on the target compound is small, and the raw materials come from nature, no harmful substances are introduced in the preparation process, and there is no problem of toxic solvent residue; the mogroside V prepared by the method of the present invention has a higher purity, and the purity is above 94.6% .
Description
Technical field
This patent belongs to active ingredients in natural plants extractive technique field, and in particular to a kind of to utilize subcritical and molecule
The method for preparing natural sweetener Fructus Momordicae fructoside V is combined in distillation.
Background technique
Siraitia grosvenorii is the perennial liana of Curcurbitaceae, and leaf is heart-shaped, dioecism, summer-flowering, seed in autumn.Chinese medicine
Lung heat phlegm-fire cough, pharynx are cured mainly containing medicinal ingredients such as Fructus Momordicae fructoside, a variety of amino acid and vitamins with its fruit medicine
Laryngitis, tonsillitis, acute gastritis, constipation etc. are the famous specialties in Guangxi China Guilin City.
Glucosides rich in Siraitia grosvenorii, total content is 3.78-3.86% in dry fruit, and content is most in glucosides
It is glucosides V, content is 22% or so of total glucosides.The sugariness of glucosides V is 256 times of sucrose, and sweet and pure, free from extraneous odour returns
Sense of taste is strong, and thermal stability is good, can be used as the sweetener of food, dish, and heat is lower is adiposis patient and is unsuitable for using confectionery
The ideal sugar substitute of diabetes patient, and have effects that eliminating phlegm and relieving cough is relievingd asthma.
The extraction of existing Fructus Momordicae fructoside V, preparation method are more, but resulting Fructus Momordicae fructoside V purity is not high or operates
Process is complicated, takes a long time.Such as, Chinese patent CN200810073876.3 discloses the preparation method of Fructus Momordicae fructoside V, is
Separating-purifying, obtained final products are carried out to the thick glycosides containing Fructus Momordicae fructoside V by silica gel column chromatography and C18 reversed phase chromatography
Purity only 70% or more, this method prepare Fructus Momordicae fructoside V there are complex steps, product purity is lower the defects of.In in addition,
State patent CN200910044558.9 discloses a kind of production method of fructus of the Mogroside V content greater than 60%,
Mainly using saccharification enzymatic hydrolysis, water are mentioned, are concentrated, ion-exchange resin decolorization, macroporous absorbent resin separate and alumina column chromatography
Purification, and finished product is obtained through last concentrate drying.Chromatography of this method Jing Guo multistep, equally exist operating process it is cumbersome, consumption
When it is longer the defects of.
Summary of the invention
Present invention aims to overcome that prior art defect, provide it is a kind of combined using subcritical and molecular distillation prepare sieve
The method of Chinese fructoside V, this method step is easy, and the purity of preparation gained Fructus Momordicae fructoside V is higher.
To achieve the above object, the present invention adopts the following technical scheme:
A method of combined using subcritical and molecular distillation and prepare Fructus Momordicae fructoside V comprising following steps:
1) Grosvenor Momordica Fruit is subjected to subcritical abstraction, obtains Siraitia grosvenorii extract；
2) Siraitia grosvenorii extract is subjected to molecular distillation, obtains the light component of the V containing Fructus Momordicae fructoside.
Specifically, when step 1) Subcritical extracts, temperature is 10-50 DEG C, pressure in order to obtain preferable effect of extracting
Power is 0.5-2.0 MPa, and the time is 3-5 h.
Further, when step 1) Subcritical extracts, extractant is one of normal butane, propane, dimethyl ether, ether
Or the mixture of two or more arbitrary proportions, Grosvenor Momordica Fruit and extractant is added by solid-liquid ratio 1g:6-15mL when extraction.
Specifically, in order to obtain preferable molecular distillation effect, when carrying out molecular distillation in step 2, vapo(u)rizing temperature 50
± 5 DEG C, distillation pressure is 0.01-0.1 Pa.Further in order to obtain higher product purity, preferably molecule steaming is being carried out
Before evaporating, Siraitia grosvenorii extract is concentrated under reduced pressure in advance to remove part extractant, the partial extraction agent of removing is to account for extraction
The 50-70% of agent totality accumulated amount is advisable.
Further, when carrying out molecular distillation in step 2, the revolving speed of scraper plate is 50-70 rad/min, charging rate
0.1-1.0mL/min.
It is further preferred that Grosvenor Momordica Fruit is preparatory in step 1) crosses 40-60 mesh screen.Specifically, Siraitia grosvenorii is ground
Alms bowl is pulverized, is sieved (aperture of sieve is 40-60 mesh), and Grosvenor Momordica Fruit is obtained.
Subcritical fluid extraction technology is the special nature using subcritical fluids, and material injects subcritical in extractor
Fluid impregnates, the extraction process carried out under the conditions of certain solid-liquid ratio, extraction temperature, extraction time, extracting pressure.Extraction is mixed
It closes liquid and enters vapo(u)rization system after being separated by solid-liquid separation, it, will according to the principle of reduction vaporization under the action of compressor and vacuum pump
Extractant switchs to gaseous state by liquid to obtain Objective extraction object.
Molecular distillation is also known as short-path distillation, is a kind of new and high technology of liquid-liquid separation, it is different from Conventional espresso by boiling
The poor separation principle of point, but separation is realized by the difference of different material molecular tools, molecular distillation technique is in spy
Enrichment, the isolation technics of flavor component etc. application are levied than wide.
The method of the present invention passes through raw material comminution pretreatment, subcritical abstraction and molecular distillation three using Siraitia grosvenorii as raw material
Fructus Momordicae fructoside V is prepared in step.It is detected through efficient liquid phase, Fructus Momordicae fructoside V in molecular distillation light component obtained
Purity reaches 94.6% or more.Compared to the prior art, the method for the present invention has the beneficial effect that:
1) the method for the present invention includes three raw material comminution pretreatment, subcritical abstraction and molecular distillation steps, and operating procedure is simple
It is convenient, it is time-consuming shorter, it is suitble to large-scale production and application；Temperature is lower in entire technical process to carry out brokenly fragrance matter
It is bad, it is smaller on target compound influence, and raw material has no introducing harmful substance, no from nature during the preparation process
There are toxic problem of solvent residual；
2) prepare that resulting Fructus Momordicae fructoside V purity is higher, and purity is 94.6% or more using the method for the present invention.
Detailed description of the invention
Fig. 1 is the HPLC spectrogram that embodiment 1 prepares gained Fructus Momordicae fructoside V finished product.
Specific embodiment
Technical solution of the present invention is further discussed in detail with reference to embodiments, but protection scope of the present invention
It is not limited thereto.
Embodiment 1
A method of combined using subcritical and molecular distillation and prepare Fructus Momordicae fructoside V comprising following steps:
1) Siraitia grosvenorii is pulverized with stone roller alms bowl, crosses 40-60 mesh screen, obtain Grosvenor Momordica Fruit；
2) it takes 200 g of Grosvenor Momordica Fruit to be placed in subcritical abstraction kettle, the positive fourth of volume ratio 1:1 is added into subcritical abstraction kettle
Alkane and 1200 mL of dimethyl ether extract 3 under conditions of extraction temperature is 10 DEG C, extracting pressure is 2.0 MPa as extractant
H obtains Siraitia grosvenorii extract；
3) Siraitia grosvenorii extract is concentrated under reduced pressure to remove 60% extractant, then vapo(u)rizing temperature is 50 DEG C, distillation pressure is
0.01 Pa, scraper plate revolving speed are 50 rad/min, charging rate carries out molecular distillation under conditions of being 0.1 mL/min, are contained
The light component of Fructus Momordicae fructoside V, then freeze-dried machine are freeze-dried 24 h, obtain white powder crystal, as Siraitia grosvenorii
Glucosides V finished product, yield 13.65%.
Fructus Momordicae fructoside V finished product obtained by above-mentioned preparation is carried out efficient liquid phase detection, testing result discovery: purity is
96.95%, the result is shown in Figure 1.
The actual conditions of efficient liquid phase detection are as follows:
Chromatographic condition: chromatographic column Agilent ZORBAX SB-C18(4.6mm × 250nm, 5 μm)；Mobile phase water: (A) and second
Nitrile (B), using gradient elution, 0-40 min, 5%-68% B；30 DEG C of column temperature；203 nm of Detection wavelength；Volume flow 1mL/
min。
Embodiment 2
A method of combined using subcritical and molecular distillation and prepare Fructus Momordicae fructoside V comprising following steps:
1) Siraitia grosvenorii is pulverized with stone roller alms bowl, crosses 40-60 mesh screen, obtain Grosvenor Momordica Fruit；
2) it takes 200 g of Grosvenor Momordica Fruit to be placed in subcritical abstraction kettle, 2400 mL conduct of propane is added into subcritical abstraction kettle
Extractant extracts 4 h under conditions of extraction temperature is 30 DEG C, extracting pressure is 1.5 MPa, obtains Siraitia grosvenorii extract；
3) Siraitia grosvenorii extract is concentrated under reduced pressure to remove 60% extractant, then vapo(u)rizing temperature is 50 DEG C, distillation pressure is
0.03 Pa, scraper plate revolving speed are 60 rad/min, charging rate carries out molecular distillation under conditions of being 0.3 mL/min, are contained
The light component of Fructus Momordicae fructoside V, then freeze-dried machine are freeze-dried 24 h, obtain white powder crystal, as Siraitia grosvenorii
Glucosides V finished product, yield 12.37%.
Fructus Momordicae fructoside V finished product obtained by above-mentioned preparation is carried out efficient liquid phase detection, testing result discovery: purity is
95.81%。
Embodiment 3
A method of combined using subcritical and molecular distillation and prepare Fructus Momordicae fructoside V comprising following steps:
1) Siraitia grosvenorii is pulverized with stone roller alms bowl, crosses 40-60 mesh screen, obtain Grosvenor Momordica Fruit；
2) it takes 200 g of Grosvenor Momordica Fruit to be placed in subcritical abstraction kettle, the propane of volume ratio 1:1 is added into subcritical abstraction kettle
With 2000 mL of ether as extractant, 3 h are extracted under conditions of extraction temperature is 40 DEG C, extracting pressure is 1.0 MPa, are obtained
To Siraitia grosvenorii extract；
3) Siraitia grosvenorii extract is concentrated under reduced pressure to remove 60% extractant, then vapo(u)rizing temperature is 50 DEG C, distillation pressure is
0.06 Pa, scraper plate revolving speed are 55 rad/min, charging rate carries out molecular distillation under conditions of being 0.6 mL/min, are contained
The light component of Fructus Momordicae fructoside V, then freeze-dried machine are freeze-dried 24 h, obtain white powder crystal, as Siraitia grosvenorii
Glucosides V finished product, yield 14.46%.
Fructus Momordicae fructoside V finished product obtained by above-mentioned preparation is carried out efficient liquid phase detection, testing result discovery: purity is
94.62%。
Embodiment 4
A method of combined using subcritical and molecular distillation and prepare Fructus Momordicae fructoside V comprising following steps:
1) Siraitia grosvenorii is pulverized with stone roller alms bowl, crosses 40-60 mesh screen, obtain Grosvenor Momordica Fruit；
2) it takes 200 g of Grosvenor Momordica Fruit to be placed in subcritical abstraction kettle, normal butane and ether (body is added into subcritical abstraction kettle
Product is than 1:1) 3000 mL as extractant, extract 5 h under conditions of extraction temperature is 50 DEG C, extracting pressure is 2.0 MPa,
Obtain Siraitia grosvenorii extract；
3) Siraitia grosvenorii extract is concentrated under reduced pressure to remove 60% extractant, then vapo(u)rizing temperature is 50 DEG C, distillation pressure is
0.1 Pa, scraper plate revolving speed are 70 rad/min, charging rate carries out molecular distillation under conditions of being 1.0 mL/min, are contained
The light component of Fructus Momordicae fructoside V, then freeze-dried machine are freeze-dried 24 h, obtain white powder crystal, as Siraitia grosvenorii
Glucosides V finished product, yield 12.98%.
Fructus Momordicae fructoside V finished product obtained by above-mentioned preparation is carried out efficient liquid phase detection, testing result discovery: purity is
97.82%。
Embodiment 5
A method of combined using subcritical and molecular distillation and prepare Fructus Momordicae fructoside V comprising following steps:
1) Siraitia grosvenorii is pulverized with stone roller alms bowl, crosses 40-60 mesh screen, obtain Grosvenor Momordica Fruit；
2) it takes 200 g of Grosvenor Momordica Fruit to be placed in subcritical abstraction kettle, ether and dimethyl ether (body is added into subcritical abstraction kettle
Product is than 1:1) 2800 mL as extractant, extract 4 h under conditions of extraction temperature is 35 DEG C, extracting pressure is 1.5 MPa,
Obtain Siraitia grosvenorii extract；
3) Siraitia grosvenorii extract is concentrated under reduced pressure to remove 60% extractant, then vapo(u)rizing temperature is 50 DEG C, distillation pressure is
0.07 Pa, scraper plate revolving speed are 60 rad/min, charging rate carries out molecular distillation under conditions of being 0.04 mL/min, are obtained
The light component of the V containing Fructus Momordicae fructoside, then freeze-dried machine are freeze-dried 24 h, obtain white powder crystal, as arhat
Fructoside V finished product, yield 14.41%.
Fructus Momordicae fructoside V finished product obtained by above-mentioned preparation is carried out efficient liquid phase detection, testing result discovery: purity is
95.89%。
Embodiment 6
A method of combined using subcritical and molecular distillation and prepare Fructus Momordicae fructoside V comprising following steps:
1) Siraitia grosvenorii is pulverized with stone roller alms bowl, crosses 40-60 mesh screen, obtain Grosvenor Momordica Fruit；
2) Grosvenor Momordica Fruit is taken to be placed in subcritical abstraction kettle, be added into subcritical abstraction kettle butane and propane (volume ratio 1:
1) 2200mL is as extractant, and under conditions of extraction temperature is 25 DEG C, extracting pressure is 2.0 MPa, 3 h of extraction obtain arhat
Fruit extract；
3) Siraitia grosvenorii extract is concentrated under reduced pressure to remove 60% extractant, then vapo(u)rizing temperature is 50 DEG C, distillation pressure is
0.03 Pa, scraper plate revolving speed are 65 rad/min, charging rate carries out molecular distillation under conditions of being 0.08 mL/min, are obtained
The light component of V containing Fructus Momordicae fructoside, then freeze-dried machine are freeze-dried 24 h, obtain white powder crystal, as Siraitia grosvenorii
Glucosides V finished product, yield 12.69%.
Fructus Momordicae fructoside V finished product obtained by above-mentioned preparation is carried out efficient liquid phase detection, testing result discovery: purity is
97.83%。
Claims (6)
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Cited By (1)
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| CN113603742A (en) * | 2021-08-06 | 2021-11-05 | 湖南华诚生物资源股份有限公司 | Preparation method of mogroside V |
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Application publication date: 20190201 |