CN110025650A - The content assaying method of gypenosides in the preparation method and Herb Gynostemmae Pentaphylli extract of a kind of Herb Gynostemmae Pentaphylli extract - Google Patents
The content assaying method of gypenosides in the preparation method and Herb Gynostemmae Pentaphylli extract of a kind of Herb Gynostemmae Pentaphylli extract Download PDFInfo
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Abstract
The invention belongs to the present invention relates to technical field of extraction of Chinese traditional medicine, specifically disclose the content assaying method of gypenosides in a kind of preparation method of Herb Gynostemmae Pentaphylli extract and Herb Gynostemmae Pentaphylli extract.The preparation method of the Herb Gynostemmae Pentaphylli extract, it includes following steps: taking the dry herb of gynostemma pentaphylla, ethyl alcohol is added after crushing and carries out heating and refluxing extraction, up to the Herb Gynostemmae Pentaphylli extract after being then concentrated and dried extracting solution；The amount ratio of the dry herb of the gynostemma pentaphylla and ethyl alcohol is 1g:7~9mL；The ethyl alcohol is that volume fraction is the ethanol water that volume fraction is 65%~75%；The number that is heated to reflux is 3~4 times；Being heated to reflux the time every time is 40~50min.Using nontoxic ethyl alcohol as Extraction solvent in this method, dissolvent residual caused by extracting using other toxic solvents is effectively prevented, while this method can be extracted to obtain higher gypenosides.
Description
Technical field
The present invention relates to technical field of extraction of Chinese traditional medicine, and in particular to a kind of preparation method of Herb Gynostemmae Pentaphylli extract and gynostemma pentaphylla
The content assaying method of gypenosides in extract.
Background technique
Gynostemma pentaphylla is Curcurbitaceae gynostemma pentaphyllum genus liana, is known as " south ginseng ", be the Ministry of Public Health in 2002 announce can
Chinese medicine for health food.Its principle active component be gypenoside, gynostemma pentaphylla glucosides, water-soluble amino acids, flavonoids,
The effect of multivitamin, microelement, minerals etc., replenish qi to invigorate the spleen, preventing phlegm from forming and stopping coughing, clearing heat and detoxicating.It clinically finds, twists
Stock is blue to be had reducing blood lipid, adjusts blood pressure, prevention and treatment thrombus, adjust blood glucose, promote sleep, slow aging, anti-anticancer, improve immunity, adjust
A variety of effects such as human physiological functions.
Gynostemma pentaphyllum Makino saponin extraction method mainly has methanol, n-butanol extraction method, biological extraction method, ultrasonic extraction at present
Method, silica gel adsorption, macroreticular resin absorbing method etc..These extracting methods easily cause organic reagent to remain, when people being caused to take
There are larger security risks.The gypenoside quality that different manufacturers extract is very different, troubling.Therefore, one kind is developed
Safe no solvent residue, and the preparation method of the high Herb Gynostemmae Pentaphylli extract of gypenosides content has and important applies valence
Value.
Summary of the invention
Primary technical problem to be solved by this invention is to provide a kind of preparation method of Herb Gynostemmae Pentaphylli extract.By the party
The Herb Gynostemmae Pentaphylli extract no solvent residue that method is prepared, securely and reliably, and gypenosides content is high.
Above-mentioned technical problem to be solved by this invention, is achieved by the following technical programs:
A kind of preparation method of Herb Gynostemmae Pentaphylli extract, which is characterized in that comprise the following steps: taking the dry herb of gynostemma pentaphylla,
Ethyl alcohol is added after crushing and carries out heating and refluxing extraction, up to the Herb Gynostemmae Pentaphylli extract after being then concentrated and dried extracting solution；
The amount ratio of the dry herb of the gynostemma pentaphylla and ethyl alcohol is 1g:7~9mL；
The ethyl alcohol is that volume fraction is the ethanol water that volume fraction is 65%~75%；
The number that is heated to reflux is 3~4 times；Being heated to reflux the time every time is 40~50min.
The present invention effectively prevents solvent caused by extracting using other toxic solvents using nontoxic ethyl alcohol as Extraction solvent
Residual.During the extraction process, inventor has found dosage, the volume fraction of ethyl alcohol of gynostemma pentaphylla dry herb and ethyl alcohol, extracts secondary
Several and extraction time Gynostemma pentaphyllum Makino total saposins contents influences are very big, and the selection of any one parameter or multi-parameter is improper all
Causing the content of gypenosides reduces；Inventor gropes through a large amount of experiment, has developed and mentions under above-mentioned integrated condition
The Herb Gynostemmae Pentaphylli extract obtained, gypenosides content with higher.
Most preferably, the amount ratio of the dry herb of the gynostemma pentaphylla and ethyl alcohol is 1g:8mL.
Inventor is through a large amount of experiment discovery, when the amount ratio of the dry herb of gynostemma pentaphylla and ethyl alcohol is 1g:8mL, strand
The content highest of blue total saposins.When the amount ratio of the dry herb of gynostemma pentaphylla and ethyl alcohol is more than or less than 1g:8mL, gynostemma pentaphyllum total soap
The content of glycosides can decline.
Most preferably, it is the ethanol water that volume fraction is 70% that the ethyl alcohol, which is volume fraction,.
Inventor is through a large amount of experiment discovery, when ethyl alcohol is the ethanol water that volume fraction selects that volume fraction is 70%
When, the content highest of gypenosides.When volume fraction of ethanol is more than or less than 70%, the content of gypenosides can
Decline.
Most preferably, the number that is heated to reflux is 3 times.
Inventor is through a large amount of experiment discovery, when being heated to reflux number is 3 times, the content highest of gypenosides.
When being heated to reflux number more than or less than 3 times, the content of gypenosides can decline.
Most preferably, being heated to reflux the time every time is 45min.
Inventor is through a large amount of experiment discovery, when being heated to reflux the time every time is 45min, the content of gypenosides
Highest.When being heated to reflux the time every time more than or less than 45min, the content of gypenosides can decline.
The present invention also provides a kind of content assaying methods of gypenosides in Herb Gynostemmae Pentaphylli extract, and it includes following steps
It is rapid:
Reference substance preparation step: precision weighs ginsenoside Rb1, add ethyl alcohol that the ginsenoside of 1.5~2.5mg/mL is made
Rb1Ethanol solution；
Test sample preparation step: the Herb Gynostemmae Pentaphylli extract 0.05 for taking any one of Claims 1 to 55 preparation method to be prepared
Then~0.15g is settled to 500ml volumetric flask with ethyl alcohol dissolution, then takes 0.5~1.5ml solution to 10ml volumetric flask, volatilize molten
Agent is spare；
Reference substance measurement and Specification Curve of Increasing step: accurate respectively to draw different amounts of reference substance solution in 10ml appearance
Measuring bottle volatilizes solvent, the vanillic aldehyde ethanol solution of 0.3~0.6mL and the sulfuric acid solution of 3~6mL is then added, in 55~65
DEG C heating water bath develops the color 10~20min, and absorbance, using absorbance value A as ordinate, concentration are measured at 530~540nm wavelength
Standard curve is drawn for abscissa；
Sample measurement and content calculate step: precision measures test sample, and the vanillic aldehyde second of 0.3~0.6mL is then added
The sulfuric acid solution of alcoholic solution and 3~6mL, in 55~65 DEG C of heating water baths 10~20min of colour developing, at 530~540nm wavelength
Measure absorbance；The content of gypenosides is finally calculated according to the corresponding densimeter of absorbance in standard curve.
In assay step, the preparation condition of reference substance and test sample, reference substance with and sample measurement strip
Part can all influence precision, repeatability, stability and the accuracy of assay；Inventor gropes through a large amount of test, obtains
Out the preparation condition of above-mentioned reference substance and test sample, reference substance with and the determination condition of sample under obtained assay
Method, with good precision, repeatability, stability and accuracy.
Most preferably, the reference substance preparation step specifically: precision weighs ginsenoside Rb1, ethyl alcohol is added to be made
The ginsenoside Rb of 2mg/mL1Ethanol solution.
Most preferably, the test sample preparation step specifically: take the preparation method preparation of any one of Claims 1 to 55
Then obtained Herb Gynostemmae Pentaphylli extract 0.1g is settled to 500ml volumetric flask with ethyl alcohol dissolution, then takes 1ml solution to 10ml capacity
Bottle, it is spare to volatilize solvent；
Most preferably, reference substance measurement and Specification Curve of Increasing step specifically: accurate absorption is different amounts of right respectively
According to product solution in 10ml volumetric flask, solvent is volatilized, the vanillic aldehyde ethanol solution of 0.5mL and the sulfuric acid solution of 5mL is then added,
In 50 DEG C of heating water baths colour developing 15min, absorbance is measured at 538nm wavelength, using absorbance value A as ordinate, concentration is cross
Coordinate draws standard curve；
The vanillic aldehyde ethanol solution is that mass fraction is 8% vanillic aldehyde ethanol solution；The sulfuric acid solution is matter
Amount score is 77% sulfuric acid solution；
The different amounts of reference substance solution refers to the reference substance solution changed from the 20 μ l equivalent of μ l~200；
The regression equation of the standard curve is y=2.9571x+0.0394, related coefficient 0.9952.
Most preferably, sample measurement and content calculate step specifically: precision measures test sample, and 0.5mL is then added
Vanillic aldehyde ethanol solution and 5mL sulfuric acid solution, develop the color 15min in 50 DEG C of heating water baths, measure and inhale at 538nm wavelength
Luminosity；The content of gypenosides is finally calculated according to the corresponding densimeter of absorbance in standard curve.
The utility model has the advantages that (1) the present invention provides a kind of preparation method of completely new Herb Gynostemmae Pentaphylli extract, with nothing in this method
The ethyl alcohol of poison is Extraction solvent, effectively prevents dissolvent residual caused by extracting using other toxic solvents, and this method can mention
Obtain higher gypenosides content；It is especially 1g:8mL, second in the amount ratio of the dry herb of gynostemma pentaphylla and ethyl alcohol
It is 70% ethanol water that alcohol, which selects volume fraction, and being heated to reflux number is 3 times, and being heated to reflux the time every time is 45min's
Under the conditions of can extract to obtain highest gypenosides content；Obtaining gypenosides content under this condition is
0.1025mg/ml；(2) in addition, the present invention also provides a kind of assay sides of gypenosides in Herb Gynostemmae Pentaphylli extract
Method, this method have good precision, repeatability, stability and accuracy.
Specific embodiment
The present invention is explained further below in conjunction with specific embodiment, but embodiment does not do any type of limit to the present invention
It is fixed.
One, the content assaying method of gypenosides is as follows in Herb Gynostemmae Pentaphylli extract of the present invention:
(1) prepared by test sample
The dry herb of gynostemma pentaphylla is crushed, 50 meshes is crossed, weighs 50g, add 70% ethyl alcohol 400ml, refluxing extraction 45min,
Pour out extracting solution；The dregs of a decoction add 70% ethyl alcohol 400ml, refluxing extraction 45min to pour out extracting solution, extract 3 times repeatedly, merge and extract
Liquid, twice, filtrate decompression concentration obtains Herb Gynostemmae Pentaphylli extract for filtration.0.1g Herb Gynostemmae Pentaphylli extract is taken, is settled to ethyl alcohol dissolution
500ml volumetric flask takes 1ml solution to 10ml volumetric flask, sets that volatilize solvent in 80 DEG C of water-baths spare.
(2) prepared by reference substance
Precision weighs ginsenoside Rb1The solution that every 1ml contains 2mg is made with ethyl alcohol in 4mg, spare.
(3) reference substance measurement and Specification Curve of Increasing
Accurate 60 μ l of reference substance solution, 80 μ l, 100 μ l, 120 μ l, 140 μ l, the 160 μ l of drawing are in 10ml volumetric flask respectively,
It sets in 80 DEG C of water-baths and volatilizes solvent.Being separately added into 8% vanillic aldehyde ethanol solution, (it is molten that 800mg vanillic aldehyde is dissolved in 10ml dehydrated alcohol
Xie Zhong, ready-to-use) 0.5ml, 77% sulfuric acid solution 5ml shakes up, close plug, sets 60 DEG C of heating water bath colour developing 15min, take out, vertical
I.e. with the cooling 10min of ice water, using reagent of accompanying as blank, according to the Pharmacopoeia of the People's Republic of China 2015 version one it is ultraviolet-
Visible spectrophotometry (annex VA) measures absorbance, using absorbance value A as ordinate, concentration (mg at 538nm wavelength
Ml-1 standard curve) is drawn for abscissa, calculating regression equation is y=2.9571x+0.0394, related coefficient 0.9952, people
Join saponin(e Rb1Content has good linear relationship within the scope of 0.12~0.32mg/ml.
(4) sample measurement and content calculate
Precision measures above-mentioned test sample and 8% vanillic aldehyde ethanol solution 0.5ml is added, and 77% sulfuric acid solution 5ml shakes up, close
Plug sets 60 DEG C of heating water baths colour developing 15min, takes out, 10min is cooled down with ice water immediately, according to determined by ultraviolet spectrophotometry.Finally
The content of gypenosides is calculated according to the corresponding densimeter of absorbance in standard curve.
Two, methodological study is as follows:
(1) precision test
Precision draws 60 μ l of reference substance solution, sets 10ml volumetric flask, by 2.1.3.1 lower method measurements, is repeated 6 times, RSD
Value is 1.14%, shows that instrument precision is good.
(2) repetitive test
5 parts of test solution are taken, according to determined by ultraviolet spectrophotometry, is repeated 5 times, RSD value is 1.36%, shows this method
Reproducibility is good.
(3) stability test
Take with a test solution, respectively 0h, 2h, 4h, 6h, 8h, for 24 hours when measure, RSD value is 1.87%, is shown
The sample liquid is stablized interior for 24 hours.
(4) accuracy test
The sample solution that precision draws 1ml known concentration sets 10ml volumetric flask, precision be added sample size 80%, 100%,
120% reference substance is separately added into 8% vanillic aldehyde ethanol solution 0.5ml, 77% sulfuric acid solution 5ml, shakes up, close plug sets 60 DEG C
Heating water bath colour developing 15min, takes out, and immediately with the cooling 10min of ice water, by 2.1.3.1 lower measurements, testing the rate of recovery is
99.3%, RSD 1.01% shows that the method sample recovery rate is good.
The preparation of 1 Herb Gynostemmae Pentaphylli extract of embodiment
The dry herb of gynostemma pentaphylla is taken, 50 meshes are smashed it through, ethyl alcohol is added and carries out heating and refluxing extraction, then by extracting solution
Up to the Herb Gynostemmae Pentaphylli extract after concentrate drying；The amount ratio of the dry herb of the gynostemma pentaphylla and ethyl alcohol is 1g:8mL；
The ethyl alcohol is the ethanol water that volume fraction is 70%；The number that is heated to reflux is 3 times；When being heated to reflux every time
Between be 45min.
It is 0.1025mg/ referring to gypenosides content in above method measurement under this condition Herb Gynostemmae Pentaphylli extract
ml。
The preparation of 1 Herb Gynostemmae Pentaphylli extract of comparative example
The dry herb of gynostemma pentaphylla is taken, 50 meshes are smashed it through, ethyl alcohol is added and carries out heating and refluxing extraction, then by extracting solution
Up to the Herb Gynostemmae Pentaphylli extract after concentrate drying；The amount ratio of the dry herb of the gynostemma pentaphylla and ethyl alcohol is 1g:8mL；
The ethyl alcohol is the ethanol water that volume fraction is 70%；The number that is heated to reflux is 1 time；When being heated to reflux every time
Between be 45min.
It is 0.0682mg/ referring to gypenosides content in above method measurement under this condition Herb Gynostemmae Pentaphylli extract
ml.This method is different from the extraction time of embodiment 1, but gypenosides content is much in its obtained Herb Gynostemmae Pentaphylli extract
Less than embodiment 1.
The preparation of 2 Herb Gynostemmae Pentaphylli extract of comparative example
The dry herb of gynostemma pentaphylla is taken, 50 meshes are smashed it through, ethyl alcohol is added and carries out heating and refluxing extraction, then by extracting solution
Up to the Herb Gynostemmae Pentaphylli extract after concentrate drying；The amount ratio of the dry herb of the gynostemma pentaphylla and ethyl alcohol is 1g:8mL；
The ethyl alcohol is the ethanol water that volume fraction is 70%；The number that is heated to reflux is 2 times；When being heated to reflux every time
Between be 45min.
It is 0.0607mg/ referring to gypenosides content in above method measurement under this condition Herb Gynostemmae Pentaphylli extract
ml.This method is different from the extraction time of embodiment 1, but gypenosides content is much in its obtained Herb Gynostemmae Pentaphylli extract
Less than embodiment 1.
The preparation of 3 Herb Gynostemmae Pentaphylli extract of comparative example
The dry herb of gynostemma pentaphylla is taken, 50 meshes are smashed it through, ethyl alcohol is added and carries out heating and refluxing extraction, then by extracting solution
Up to the Herb Gynostemmae Pentaphylli extract after concentrate drying；The amount ratio of the dry herb of the gynostemma pentaphylla and ethyl alcohol is 1g:8mL；
The ethyl alcohol is the ethanol water that volume fraction is 70%；The number that is heated to reflux is 3 times；When being heated to reflux every time
Between be 30min.
It is 0.0607mg/ referring to gypenosides content in above method measurement under this condition Herb Gynostemmae Pentaphylli extract
ml.This method is different from the extraction time of embodiment 1, but gypenosides content is much in its obtained Herb Gynostemmae Pentaphylli extract
Less than embodiment 1.
The preparation of 4 Herb Gynostemmae Pentaphylli extract of comparative example
The dry herb of gynostemma pentaphylla is taken, 50 meshes are smashed it through, ethyl alcohol is added and carries out heating and refluxing extraction, then by extracting solution
Up to the Herb Gynostemmae Pentaphylli extract after concentrate drying；The amount ratio of the dry herb of the gynostemma pentaphylla and ethyl alcohol is 1g:8mL；
The ethyl alcohol is the ethanol water that volume fraction is 70%；The number that is heated to reflux is 3 times；When being heated to reflux every time
Between be 60min.
It is 0.0770mg/ referring to gypenosides content in above method measurement under this condition Herb Gynostemmae Pentaphylli extract
ml.This method is different from the extraction time of embodiment 1, but gypenosides content is much in its obtained Herb Gynostemmae Pentaphylli extract
Less than embodiment 1.
The preparation of 5 Herb Gynostemmae Pentaphylli extract of comparative example
The dry herb of gynostemma pentaphylla is taken, 50 meshes are smashed it through, ethyl alcohol is added and carries out heating and refluxing extraction, then by extracting solution
Up to the Herb Gynostemmae Pentaphylli extract after concentrate drying；The amount ratio of the dry herb of the gynostemma pentaphylla and ethyl alcohol is 1g:8mL；
The ethyl alcohol is the ethanol water that volume fraction is 70%；The number that is heated to reflux is 3 times；When being heated to reflux every time
Between be 90min.
It is 0.0624mg/ referring to gypenosides content in above method measurement under this condition Herb Gynostemmae Pentaphylli extract
ml.This method is different from the extraction time of embodiment 1, but gypenosides content is much in its obtained Herb Gynostemmae Pentaphylli extract
Less than embodiment 1.
The preparation of 6 Herb Gynostemmae Pentaphylli extract of comparative example
The dry herb of gynostemma pentaphylla is taken, 50 meshes are smashed it through, ethyl alcohol is added and carries out heating and refluxing extraction, then by extracting solution
Up to the Herb Gynostemmae Pentaphylli extract after concentrate drying；The amount ratio of the dry herb of the gynostemma pentaphylla and ethyl alcohol is 1g:8mL；
The ethyl alcohol is the ethanol water that volume fraction is 70%；The number that is heated to reflux is 3 times；When being heated to reflux every time
Between be 120min.
It is 0.0617mg/ referring to gypenosides content in above method measurement under this condition Herb Gynostemmae Pentaphylli extract
ml.This method is different from the extraction time of embodiment 1, but gypenosides content is much in its obtained Herb Gynostemmae Pentaphylli extract
Less than embodiment 1.
The preparation of 7 Herb Gynostemmae Pentaphylli extract of comparative example
The dry herb of gynostemma pentaphylla is taken, 50 meshes are smashed it through, ethyl alcohol is added and carries out heating and refluxing extraction, then by extracting solution
Up to the Herb Gynostemmae Pentaphylli extract after concentrate drying；The amount ratio of the dry herb of the gynostemma pentaphylla and ethyl alcohol is 1g:4mL；
The ethyl alcohol is the ethanol water that volume fraction is 70%；The number that is heated to reflux is 3 times；When being heated to reflux every time
Between be 15min.
It is 0.0891mg/ referring to gypenosides content in above method measurement under this condition Herb Gynostemmae Pentaphylli extract
ml.This method is different from the extraction time of embodiment 1 and solid-liquid ratio, but gynostemma pentaphyllum total soap in its obtained Herb Gynostemmae Pentaphylli extract
Glycosides content is far smaller than embodiment 1.
The preparation of 8 Herb Gynostemmae Pentaphylli extract of comparative example
The dry herb of gynostemma pentaphylla is taken, 50 meshes are smashed it through, ethyl alcohol is added and carries out heating and refluxing extraction, then by extracting solution
Up to the Herb Gynostemmae Pentaphylli extract after concentrate drying；The amount ratio of the dry herb of the gynostemma pentaphylla and ethyl alcohol is 1g:14mL；
The ethyl alcohol is the ethanol water that volume fraction is 70%；The number that is heated to reflux is 3 times；When being heated to reflux every time
Between be 15min.
It is 0.0854mg/ referring to gypenosides content in above method measurement under this condition Herb Gynostemmae Pentaphylli extract
ml.This method is different from the extraction time of embodiment 1 and solid-liquid ratio, but gynostemma pentaphyllum total soap in its obtained Herb Gynostemmae Pentaphylli extract
Glycosides content is far smaller than embodiment 1.
The preparation of 9 Herb Gynostemmae Pentaphylli extract of comparative example
The dry herb of gynostemma pentaphylla is taken, 50 meshes are smashed it through, ethyl alcohol is added and carries out heating and refluxing extraction, then by extracting solution
Up to the Herb Gynostemmae Pentaphylli extract after concentrate drying；The amount ratio of the dry herb of the gynostemma pentaphylla and ethyl alcohol is 1g:10mL；
The ethyl alcohol is the ethanol water that volume fraction is 60%；The number that is heated to reflux is 3 times；When being heated to reflux every time
Between be 15min.
It is 0.0864mg/ referring to gypenosides content in above method measurement under this condition Herb Gynostemmae Pentaphylli extract
ml.This method is different from the concentration of the extraction time of embodiment 1, solid-liquid ratio and ethyl alcohol, but its obtained Herb Gynostemmae Pentaphylli extract
Middle gypenosides content is far smaller than embodiment 1.
The preparation of 10 Herb Gynostemmae Pentaphylli extract of comparative example
The dry herb of gynostemma pentaphylla is taken, 50 meshes are smashed it through, ethyl alcohol is added and carries out heating and refluxing extraction, then by extracting solution
Up to the Herb Gynostemmae Pentaphylli extract after concentrate drying；The amount ratio of the dry herb of the gynostemma pentaphylla and ethyl alcohol is 1g:10mL；
The ethyl alcohol is the ethanol water that volume fraction is 50%；The number that is heated to reflux is 3 times；When being heated to reflux every time
Between be 15min.
It is 0.0736mg/ referring to gypenosides content in above method measurement under this condition Herb Gynostemmae Pentaphylli extract
ml.This method is different from the concentration of the extraction time of embodiment 1, solid-liquid ratio and ethyl alcohol, but its obtained Herb Gynostemmae Pentaphylli extract
Middle gypenosides content is far smaller than embodiment 1.
The preparation of 11 Herb Gynostemmae Pentaphylli extract of comparative example
The dry herb of gynostemma pentaphylla is taken, 50 meshes are smashed it through, ethyl alcohol is added and carries out heating and refluxing extraction, then by extracting solution
Up to the Herb Gynostemmae Pentaphylli extract after concentrate drying；The amount ratio of the dry herb of the gynostemma pentaphylla and ethyl alcohol is 1g:10mL；
The ethyl alcohol is the ethanol water that volume fraction is 85%；The number that is heated to reflux is 3 times；When being heated to reflux every time
Between be 15min.
It is 0.0841mg/ referring to gypenosides content in above method measurement under this condition Herb Gynostemmae Pentaphylli extract
ml.This method is different from the concentration of the extraction time of embodiment 1, solid-liquid ratio and ethyl alcohol, but its obtained Herb Gynostemmae Pentaphylli extract
Middle gypenosides content is far smaller than embodiment 1.
The preparation of 12 Herb Gynostemmae Pentaphylli extract of comparative example
The dry herb of gynostemma pentaphylla is taken, 50 meshes are smashed it through, ethyl alcohol is added and carries out heating and refluxing extraction, then by extracting solution
Up to the Herb Gynostemmae Pentaphylli extract after concentrate drying；The amount ratio of the dry herb of the gynostemma pentaphylla and ethyl alcohol is 1g:10mL；
The ethyl alcohol is the ethanol water that volume fraction is 95%；The number that is heated to reflux is 3 times；When being heated to reflux every time
Between be 15min.
It is 0.0818mg/ referring to gypenosides content in above method measurement under this condition Herb Gynostemmae Pentaphylli extract
ml.This method is different from the concentration of the extraction time of embodiment 1, solid-liquid ratio and ethyl alcohol, but its obtained Herb Gynostemmae Pentaphylli extract
Middle gypenosides content is far smaller than embodiment 1.
The dry herb of gynostemma pentaphylla and ethyl alcohol can be seen that by the gypenosides content of embodiment 1 and above-mentioned comparative example
The content influence of dosage, the volume fraction of ethyl alcohol, extraction time and extraction time Gynostemma pentaphyllum Makino total saposins is very big, any one
The improper reduction that can all cause gypenosides content of the selection of parameter or multi-parameter.
Claims (10)
1. a kind of preparation method of Herb Gynostemmae Pentaphylli extract, which is characterized in that comprise the following steps: taking the dry herb of gynostemma pentaphylla, powder
Ethyl alcohol is added after broken and carries out heating and refluxing extraction, up to the Herb Gynostemmae Pentaphylli extract after being then concentrated and dried extracting solution；
The amount ratio of the dry herb of the gynostemma pentaphylla and ethyl alcohol is 1g:7~9mL；
The ethyl alcohol is that volume fraction is the ethanol water that volume fraction is 65%~75%；
The number that is heated to reflux is 3~4 times；Being heated to reflux the time every time is 40~50min.
2. the preparation method of Herb Gynostemmae Pentaphylli extract according to claim 1, which is characterized in that the gynostemma pentaphylla is dry complete
The amount ratio of grass and ethyl alcohol is 1g:8mL.
3. the preparation method of Herb Gynostemmae Pentaphylli extract according to claim 1, which is characterized in that the ethyl alcohol is volume point
Number is the ethanol water that volume fraction is 70%.
4. the preparation method of Herb Gynostemmae Pentaphylli extract according to claim 1, which is characterized in that described is heated to reflux number
It is 3 times.
5. the preparation method of Herb Gynostemmae Pentaphylli extract according to claim 1, which is characterized in that being heated to reflux the time every time is
45min。
6. the content assaying method of gypenosides in a kind of Herb Gynostemmae Pentaphylli extract, which is characterized in that comprise the following steps:
Reference substance preparation step: precision weighs ginsenoside Rb1, add ethyl alcohol that the ginsenoside Rb of 1.5~2.5mg/mL is made1Second
Alcoholic solution；
Test sample preparation step: the Herb Gynostemmae Pentaphylli extract 0.05 for taking any one of Claims 1 to 55 preparation method to be prepared~
Then 0.15g is settled to 500ml volumetric flask with ethyl alcohol dissolution, then takes 0.5~1.5ml solution to 10ml volumetric flask, volatilize solvent
It is spare；
Reference substance measurement and Specification Curve of Increasing step: accurate respectively to draw different amounts of reference substance solution in 10ml capacity
Bottle, volatilizes solvent, the vanillic aldehyde ethanol solution of 0.3~0.6mL and the sulfuric acid solution of 3~6mL is then added, in 55~65 DEG C
Heating water bath 10~20min of colour developing, measures absorbance, using absorbance value A as ordinate, concentration is at 530~540nm wavelength
Abscissa draws standard curve；
Sample measurement and content calculate step: precision measures test sample, and the vanillic aldehyde ethyl alcohol that 0.3~0.6mL is then added is molten
The sulfuric acid solution of liquid and 3~6mL measures at 530~540nm wavelength in 55~65 DEG C of heating water baths 10~20min of colour developing
Absorbance；The content of gypenosides is finally calculated according to the corresponding densimeter of absorbance in standard curve.
7. content assaying method according to claim 6, which is characterized in that the reference substance preparation step specifically:
Precision weighs ginsenoside Rb1, add ethyl alcohol that the ginsenoside Rb of 2mg/mL is made1Ethanol solution.
8. content assaying method according to claim 6, which is characterized in that the test sample preparation step specifically:
Then the Herb Gynostemmae Pentaphylli extract 0.1g for taking any one of Claims 1 to 55 preparation method to be prepared is settled to ethyl alcohol dissolution
500ml volumetric flask, then take 1ml solution to 10ml volumetric flask, it is spare to volatilize solvent.
9. content assaying method according to claim 6, which is characterized in that reference substance measurement and Specification Curve of Increasing step
Suddenly specifically: it is accurate respectively to draw different amounts of reference substance solution in 10ml volumetric flask, solvent is volatilized, is then added 0.5mL's
The sulfuric acid solution of vanillic aldehyde ethanol solution and 5mL measures extinction in 50 DEG C of heating water baths colour developing 15min at 538nm wavelength
Degree, using absorbance value A as ordinate, concentration is that abscissa draws standard curve；
The vanillic aldehyde ethanol solution is that mass fraction is 8% vanillic aldehyde ethanol solution；The sulfuric acid solution is quality point
Number is 77% sulfuric acid solution；
The different amounts of reference substance solution refers to the reference substance solution changed from the 20 μ l equivalent of μ l~200；
The regression equation of the standard curve is y=2.9571x+0.0394, related coefficient 0.9952.
10. content assaying method according to claim 6, which is characterized in that sample measurement and content calculate step tool
Body are as follows: precision measures test sample, the vanillic aldehyde ethanol solution of 0.5mL and the sulfuric acid solution of 5mL is then added, in 50 DEG C of water-baths
Heating colour developing 15min, measures absorbance at 538nm wavelength；Finally according to the corresponding concentration calculation of absorbance in standard curve
The content of gypenosides out.
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| CN111480755A (en) * | 2020-04-23 | 2020-08-04 | 四川卫生康复职业学院 | Gynostemma pentaphylla beverage and preparation method thereof |
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| CN116098929A (en) * | 2023-03-07 | 2023-05-12 | 陕西嘉禾生物科技股份有限公司 | Method for extracting gynostemma pentaphylla total saponin from gynostemma pentaphylla |
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