CN109160933A - A method of utilizing molecular clock Fructus Momordicae fructoside V - Google Patents
A method of utilizing molecular clock Fructus Momordicae fructoside V Download PDFInfo
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- CN109160933A CN109160933A CN201811086658.3A CN201811086658A CN109160933A CN 109160933 A CN109160933 A CN 109160933A CN 201811086658 A CN201811086658 A CN 201811086658A CN 109160933 A CN109160933 A CN 109160933A
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- fructus momordicae
- momordicae fructoside
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- fructoside
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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
- C07J17/005—Glycosides
Abstract
The present invention relates to a kind of methods using molecular clock Fructus Momordicae fructoside V comprising following steps: 1) Grosvenor Momordica Fruit being carried out ultrasonic immersion with ethyl alcohol；2) ultrasound carries out refluxing extraction after impregnating, and is separated by solid-liquid separation after refluxing extraction, filtrate is through being concentrated under reduced pressure to give Luo Han Guo Paste In Foods；3) Luo Han Guo Paste In Foods carry out molecular distillation and obtain the light of the V containing Fructus Momordicae fructoside, heavy constituent.The method of the present invention operating procedure is simple and convenient, and temperature is lower in entire technical process to destroy fragrance matter, and raw material has no introducing harmful substance from nature during the preparation process, and toxic solvent residue problem is not present；It is higher using Fructus Momordicae fructoside V purity prepared by the method for the present invention, reach 98.50% or more.
Description
Technical field
The invention belongs to active ingredients in natural plants to extract field, and in particular to a kind of to be prepared using molecular distillation technique
The method of Fructus Momordicae fructoside V provides a kind of new approaches to prepare glucoside compound using molecular distillation technique.
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.
Chinese patent CN200810073876.3 discloses the preparation method of Fructus Momordicae fructoside V, is to pass through silica gel column layer
Analysis and C18 reversed phase chromatography carry out separating-purifying to the thick glycosides containing Fructus Momordicae fructoside V, and obtained final products purity is only 70%
More than, this method prepare Fructus Momordicae fructoside V there are complex steps, product purity is lower the defects of.In addition, Chinese patent
CN200910044558.9 discloses a kind of production method of fructus of the Mogroside V content greater than 60%, mainly adopts
It mentioned, be concentrated with saccharification enzymatic hydrolysis, water, the separation of ion-exchange resin decolorization, macroporous absorbent resin and alumina column chromatography purification, and
Finished product is obtained through last concentrate drying.Chromatography of this method Jing Guo multistep, equally exists that operating process is cumbersome, takes a long time
Defect.
Summary of the invention
Present invention aims to overcome that prior art defect, provides and a kind of utilize molecular clock Fructus Momordicae fructoside V's
Method, 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 utilizing molecular clock Fructus Momordicae fructoside V comprising following steps:
1) Grosvenor Momordica Fruit is subjected to ultrasonic immersion with ethyl alcohol；
2) ultrasound carries out refluxing extraction after impregnating, and is separated by solid-liquid separation after refluxing extraction, filtrate is through being concentrated under reduced pressure to give sieve
Chinese fruit medicinal extract；
3) Luo Han Guo Paste In Foods carry out molecular distillation and obtain the light of the V containing Fructus Momordicae fructoside, heavy constituent.
In order to obtain higher Luo Han Guo Paste In Foods extraction efficiency, in step 1), Grosvenor Momordica Fruit and ethyl alcohol press solid-liquid ratio 4-
6 g:50mL are added, and ethyl alcohol volumetric concentration is 50-90%.Specifically, Siraitia grosvenorii is pulverized with stone roller alms bowl, be sieved (sieve
The aperture of net is 40-60 mesh), obtain Grosvenor Momordica Fruit.
Further, in step 1), ultrasonic time is 10-30 min, and ultrasonic power is 100-200 KHz.
In order to obtain preferable refluxing extraction effect, in step 2, reflux extracting time is 3-5 h.
In order to obtain the Fructus Momordicae fructoside V of higher degree, in step 3), molecular distillation carries out in two times；First time molecule
Vapo(u)rizing temperature is 40 ± 5 DEG C, pressure 0.01-0.1Pa；Second of molecular distillation temperature is 60 ± 5 DEG C, pressure 0.01-
0.1 Pa。
Further, in step 3), the revolving speed of first time molecular distillation scraper plate is 120-140 rad/min, charging rate
0.5-1.5 mL/min；The revolving speed of second of molecular distillation scraper plate is 50-70 rad/min, charging rate 0.1-0.5 mL/
min。
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 for preparing Chinese fructoside V using molecular distillation technique, mainly include raw material ultrasonic extraction,
The operation such as Luo Han Guo Paste In Foods preparation, molecular distillation twice, by smashing Siraitia grosvenorii in the pretreatment of raw material stage, ultrasound, which is impregnated, to be come
Luo Han Guo Paste In Foods extraction efficiency is improved, further isolates and purifies Luo Han Guo Paste In Foods by molecular distillation technique to obtain purity higher
Fructus Momordicae fructoside V is light, heavy constituent.Compared to the prior art, beneficial effects of the present invention are as follows:
1) the method for the present invention operating procedure is simple and convenient, and temperature is lower in entire technical process to carry out brokenly fragrance matter
It is bad, and raw material has no introducing harmful substance from nature during the preparation process, and toxic solvent residue problem is not present；
2) higher using Fructus Momordicae fructoside V purity prepared by the method for the present invention, reach 98.50% or more.
Detailed description of the invention
Fig. 1 is the HPLC spectrogram that embodiment 1 prepares gained Luo Han Guo Paste In Foods heavy constituent 2#；
Fig. 2 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 utilizing molecular clock Fructus Momordicae fructoside V comprising following steps:
1) it after crushing Siraitia grosvenorii, crosses 40-60 mesh screen and obtains Grosvenor Momordica Fruit.60 g Grosvenor Momordica Fruits are weighed in 1000 mL
Round-bottomed flask in, the ethyl alcohol of 500 mL volumetric concentrations 80% is added into round-bottomed flask, round bottom flask is entered into ultrasonic cleaning
In device, ultrasound impregnates 30 min under conditions of 200 KHz；
2) after ultrasound is impregnated, round-bottomed flask is heated, 5 h of refluxing extraction with electric jacket, after refluxing extraction, is filtered,
Collect filtrate.Filtrate, which is concentrated under reduced pressure, to be removed most of solvent and obtains Luo Han Guo Paste In Foods (medicinal extract is a kind of thick mobility
Lotion), the yields of Luo Han Guo Paste In Foods is 30.12%；
3) Luo Han Guo Paste In Foods are 140 rad/min in scraper plate revolving speed, and vapo(u)rizing temperature is 40 DEG C, and distillation pressure is 0.1 Pa, charging
Speed carries out first time molecular distillation under conditions of being 0.3 mL/min, obtains Luo Han Guo Paste In Foods light component 1#, heavy constituent 2#, sieve
Chinese fruit heavy constituent 2# yield is 36.51%；
4) heavy constituent 2# is scraper plate revolving speed is 70 rad/min, vapo(u)rizing temperature is 60 DEG C, distillation pressure is 0.1 Pa, charging rate
To carry out second of molecular distillation under conditions of 0.5 mL/min, the light component 3#(of the V containing Fructus Momordicae fructoside wherein Siraitia grosvenorii is obtained
The yield of medicinal extract light component 3# be 3.63%),
The freeze-dried machine of the light component 3# of the V containing Fructus Momordicae fructoside is freeze-dried 24 h, obtains white powder crystal, as
Fructus Momordicae fructoside V finished product.
Luo Han Guo Paste In Foods in embodiment 1 are obtained into Siraitia grosvenorii heavy constituent 2# through first time molecular distillation and carry out efficient liquid phase inspection
It surveys, as a result, it has been found that: Fructus Momordicae fructoside V content is 53%(the result is shown in Figure 1 in heavy constituent 2#)；It will be obtained through second of molecular distillation
Fructus Momordicae fructoside V finished product carry out efficient liquid phase detection, find its purity be 98.52%(result see Fig. 2).
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 utilizing molecular clock Fructus Momordicae fructoside V comprising following steps:
1) it after crushing Siraitia grosvenorii, crosses 40-60 mesh screen and obtains Grosvenor Momordica Fruit.50 g Grosvenor Momordica Fruits are weighed in 1000 mL
Round-bottomed flask in, the ethyl alcohol of 500 mL volumetric concentrations 60% is added into round-bottomed flask, round bottom flask is entered into ultrasonic cleaning
In device, ultrasound impregnates 20 min under conditions of 150 KHz；
2) after ultrasound is impregnated, round-bottomed flask is heated, 4 h of refluxing extraction with electric jacket, after refluxing extraction, is filtered,
Collect filtrate.Filtrate, which is concentrated under reduced pressure, to be removed most of solvent and obtains Luo Han Guo Paste In Foods (medicinal extract is a kind of thick mobility
Lotion)；
3) Luo Han Guo Paste In Foods scraper plate revolving speed is 140 rad/min, vapo(u)rizing temperature is 40 DEG C, distillation pressure be 0.05 Pa, into
Expect to carry out first time molecular distillation under conditions of speed is 1.0 mL/min, obtains Luo Han Guo Paste In Foods light component 1#, heavy constituent 2#；
4) heavy constituent 2# scraper plate revolving speed is 60 rad/min, vapo(u)rizing temperature is 60 DEG C, distillation pressure be 0.05 Pa, charging speed
Degree carries out second of molecular distillation under conditions of being 0.3 mL/min, obtains the light component 3# containing Luo Han Guo Paste In Foods, will contain arhat
The freeze-dried machine of the light component 3# of fructoside V is freeze-dried 24 h, obtains white powder crystal, as Fructus Momordicae fructoside V
Finished product.
Detect and find through efficient liquid phase: the purity of Fructus Momordicae fructoside V finished product is 98.15%.
Embodiment 3
A method of utilizing molecular clock Fructus Momordicae fructoside V comprising following steps:
1) it after crushing Siraitia grosvenorii, crosses 40-60 mesh screen and obtains Grosvenor Momordica Fruit.40g Grosvenor Momordica Fruit is weighed in 1000 mL's
In round-bottomed flask, the ethyl alcohol of 500 mL volumetric concentrations 70% is added into round-bottomed flask, round bottom flask is entered into ultrasonic cleaner
In, ultrasound impregnates 10 min under conditions of 100 KHz；
2) after ultrasound is impregnated, round-bottomed flask is heated, 3 h of refluxing extraction with electric jacket, after refluxing extraction, is filtered,
Collect filtrate.Filtrate, which is concentrated under reduced pressure, to be removed most of solvent and obtains Luo Han Guo Paste In Foods (medicinal extract is a kind of thick mobility
Lotion)；
3) Luo Han Guo Paste In Foods 120 rad/min of scraper plate revolving speed, vapo(u)rizing temperature be 40 DEG C, distillation pressure be 0.01 Pa, charging speed
Degree carries out first time molecular distillation under conditions of being 0.5mL/min, obtains Luo Han Guo Paste In Foods light component 1#, heavy constituent 2#；
4) heavy constituent 2# is 50 rad/min of scraper plate revolving speed, vapo(u)rizing temperature are 60 DEG C, distillation pressure 0.01Pa, charging rate are
Second of molecular distillation is carried out under conditions of 0.1mL/min, is obtained the light component 3# containing Luo Han Guo Paste In Foods, will be contained Fructus Momordicae fructoside
The freeze-dried machine of the light component 3# of V is freeze-dried 24 h, obtains white powder crystal, as Fructus Momordicae fructoside V finished product.
Detect and find through efficient liquid phase: the purity of Fructus Momordicae fructoside V finished product is 98.27%.
Claims (6)
1. a kind of method using molecular clock Fructus Momordicae fructoside V, which comprises the steps of:
1) Grosvenor Momordica Fruit is subjected to ultrasonic immersion with ethyl alcohol；
2) ultrasound carries out refluxing extraction after impregnating, and is separated by solid-liquid separation after refluxing extraction, filtrate is through being concentrated under reduced pressure to give sieve
Chinese fruit medicinal extract；
3) Luo Han Guo Paste In Foods carry out molecular distillation and obtain the light of the V containing Fructus Momordicae fructoside, heavy constituent.
2. utilizing the method for molecular clock Fructus Momordicae fructoside V as described in claim 1, which is characterized in that in step 1), sieve
Chinese fruit powder end and ethyl alcohol are added by solid-liquid ratio 4-6 g:50mL, and ethyl alcohol volumetric concentration is 50-90%.
3. utilizing the method for molecular clock Fructus Momordicae fructoside V as described in claim 1, which is characterized in that in step 1), surpass
The sound time is 10-30 min, and ultrasonic power is 100-200 KHz.
4. utilizing the method for molecular clock Fructus Momordicae fructoside V as described in claim 1, which is characterized in that in step 2, return
Stream extraction time is 3-5 h.
5. utilizing the method for molecular clock Fructus Momordicae fructoside V as described in Claims 1-4 is any, which is characterized in that step
3) in, molecular distillation carries out in two times；First time molecular distillation temperature is 40 ± 5 DEG C, pressure 0.01-0.1Pa；Second
Molecular distillation temperature is 60 ± 5 DEG C, and pressure is 0.01-0.1 Pa.
6. utilizing the method for molecular clock Fructus Momordicae fructoside V as claimed in claim 5, which is characterized in that in step 3), the
The revolving speed of molecular distillation scraper plate is 120-140 rad/min, charging rate 0.5-1.5 mL/min；Second of molecule steams
The revolving speed for evaporating scraper plate is 50-70 rad/min, charging rate 0.1-0.5 mL/min.
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Citations (4)
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|---|---|---|---|---|
| CN101029071A (en) * | 2007-04-05 | 2007-09-05 | 上海交通大学 | Method for preparing high-purity Momordia grosvenori aglycone from Momordia grosvenori |
| CN101397239A (en) * | 2008-09-11 | 2009-04-01 | 中健行集团有限公司 | Method for preparing needle polyprenols by using solvent extraction method |
| CN101444333A (en) * | 2008-11-28 | 2009-06-03 | 华芳烟用香料有限公司 | Method of preparing Grosvenor momordica extract and application thereof |
| CN102675398A (en) * | 2012-05-27 | 2012-09-19 | 唐忠海 | Method for extracting momordica grosvenori glycoside V and farnesol from grosvenor momordica fruits |
-
2018
- 2018-09-18 CN CN201811086658.3A patent/CN109160933A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101029071A (en) * | 2007-04-05 | 2007-09-05 | 上海交通大学 | Method for preparing high-purity Momordia grosvenori aglycone from Momordia grosvenori |
| CN101397239A (en) * | 2008-09-11 | 2009-04-01 | 中健行集团有限公司 | Method for preparing needle polyprenols by using solvent extraction method |
| CN101444333A (en) * | 2008-11-28 | 2009-06-03 | 华芳烟用香料有限公司 | Method of preparing Grosvenor momordica extract and application thereof |
| CN102675398A (en) * | 2012-05-27 | 2012-09-19 | 唐忠海 | Method for extracting momordica grosvenori glycoside V and farnesol from grosvenor momordica fruits |
Non-Patent Citations (3)
| Title |
|---|
| 李燕 等: "分子蒸馏技术在天然产物分离纯化中应用进展", 《粮食与油脂》 * |
| 林硕 等: "罗汉果有效成分提取的研究进展", 《中国食品添加剂》 * |
| 罗永明: "《中药化学成分提取分离技术与方法》", 31 January 2016, 上海科学技术出版社 * |
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Application publication date: 20190108 |