CN105801660A - Method for extracting ginsenoside Rg1 and Re in ginseng leaves through ASE - Google Patents
Method for extracting ginsenoside Rg1 and Re in ginseng leaves through ASE Download PDFInfo
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- CN105801660A CN105801660A CN201610234882.7A CN201610234882A CN105801660A CN 105801660 A CN105801660 A CN 105801660A CN 201610234882 A CN201610234882 A CN 201610234882A CN 105801660 A CN105801660 A CN 105801660A
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- 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
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Abstract
The invention discloses a method for extracting ginsenoside Rg1 and Re in ginseng leaves through ASE.The method comprises the following steps that 1, the ginseng leaves are screened after being smashed; 2, 0.2 part by weight of momordica grosvenori fruit powder is weighed and evenly mixed with 1 part by weight of kieselguhr for use; 3, the mixture obtained in the step 2 is added to an extracting pool where a filter membrane is placed in advance, a proper amount of kieselguhr is added till the mixture reaches a pool mouth of the extracting pool, the extracting pool is covered with a cover for static extracting, extract liquor is obtained after extracting is finished, and according to extracting conditions, methyl alcohol serves as an extracting solvent, the extracting temperature is 110 DEG C, the static extracting time is 7 min, the flushing volume is 80%, and the number of times of static circulation is 3.The method for extracting ginsenoside Rg1 and Re in the ginseng leaves through ASE is easy to operate and high in extracting precision.
Description
Technical field
The present invention relates to test in laboratory field, particularly a kind of ASE extracts the method for ginsenoside Rg_1 and Re in Folium Ginseng.
Background technology
Within 2015, pharmacopeia is recorded: takes this product powder and is about 0.2g, accurately weighed, put in apparatus,Soxhlet's, add chloroform 30ml, be heated to reflux 1 hour, discard chloroform liquid, chloroform flung to by medicinal residues, adding methanol 30ml, be heated to reflux 3 hours, extracting solution low temperature is evaporated, the 10ml that adds water makes dissolving, add petroleum ether (30～60 DEG C) to extract 2 times, each 10ml, discard ether liquid, by D101 type macroporous adsorptive resins, (internal diameter is 1.5cm to water liquid, column length is 15cm), with water 50ml eluting, discard water liquid.Again with 20% ethanol 50ml eluting, discarding 20% ethanol elution, continue with 80% ethanol 80ml eluting, collect eluent 70ml, be evaporated, residue adds methanol and dissolves, and is transferred in 10ml measuring bottle, adds methanol to scale, shake up, and filters, takes subsequent filtrate, to obtain final product.
The method operating process of pharmacopeia is complicated, and washing steps is many, and the operant skill of operator is required height.
Summary of the invention
It is an object of the invention to provide a kind of ASE and extract the method for ginsenoside Rg_1 and Re in Folium Ginseng, the method is simple to operate, and extraction accuracy is high.
Technical scheme provided by the invention is: a kind of ASE extracts the method for ginsenoside Rg_1 and Re in Folium Ginseng, comprises the following steps:
Step 1: after Folium Ginseng is pulverized, sieve；
Step 2: weigh 0.2 weight portion mangosteen powder, mixs homogeneously stand-by with 1 weight portion kieselguhr；
Step 3: add the obtained mixture of step 2 in the abstraction pool putting filter membrane in advance well, adds appropriate kieselguhr to the Chi Kou reaching abstraction pool；The lid covering abstraction pool carries out static extracting；Extraction is extracted liquid after terminating；
Extraction conditions is: extractant is methanol；Extraction temperature 110 DEG C；Static extracting time 7min；Flush volume 80%；Quiet cycle number of times 3 times.
Extracting in Folium Ginseng in the method for ginsenoside Rg_1 and Re at above-mentioned ASE, the volume of described abstraction pool is 10ml.
Extracting in Folium Ginseng in the method for ginsenoside Rg_1 and Re at above-mentioned ASE, the pressure of described static extracting is 1500psi.
Extracting in Folium Ginseng in the method for ginsenoside Rg_1 and Re at above-mentioned ASE, the purge time of described static extracting is 60s.
Extract in Folium Ginseng in the method for ginsenoside Rg_1 and Re at above-mentioned ASE, also include after step 3: join after extract is diluted in centrifuge tube and purify, obtain filtrate after then filtering, added with graphitic carbon SPE post in described centrifuge tube.
The present invention is after adopting technique scheme, and it has the beneficial effect that
The extracting process of the present invention is simple to operate, and precision is consistent with the precision of official method, reproducible.
Accompanying drawing explanation
Fig. 1 is the rectangular plots of chromatography ginsenoside Rg1's validation verification of the present invention；
Fig. 2 is the rectangular plots of chromatography ginsenoside Re's validation verification of the present invention.
Detailed description of the invention
Below in conjunction with detailed description of the invention, technical scheme is described in further detail, but does not constitute any limitation of the invention.
Embodiment 1:
Size-reduced for Folium Ginseng sample machine is pulverized, crosses No. three sieves, about 0.2g, accurately weighed, mix homogeneously with 1g kieselguhr, stand-by, being moved in the ASE10ml abstraction pool putting filter membrane in advance well and add proper amount of silicon diatomaceous earth, jolting so as to Chi Kou in the same horizontal line, tightens abstraction pool upper cover gently.After extraction terminates, extract being transferred to after being evaporated in evaporating dish and dissolve and be settled to 10mL volumetric flask with methanol, absorption 1ml sample liquid is equipped with the 2ml centrifuge tube of 100mgGCB and purifies, and solution enters HPLC after crossing 0.22 micron membrane filter and measures.
Extraction conditions (see table 1) is:
Table 1
| Close with pharmacopeia | |
| Abstraction pool volume (ml) | 10 |
| Extractant | Methanol |
| Pressure (psi) | 1500 |
| Temperature (DEG C) | 110 |
| The static extracting time (min) | 7 |
| Quiet cycle number of times | 3 |
| Flush volume (%) | 80 |
| Purge time (s) | 60 |
Analysis method is LC liquid chromatography, liquid-phase chromatographic analysis condition:
A) the double; two ternary liquid phase (U-3000) of instrument: Thermo
B) chromatographic column: ThermoSyncronisDim. (mm) AQ1.7 μm of 50 × 2.1mm
C) column temperature: 40 DEG C
D) flow velocity: 0.3mL/min
E) mobile phase: acetonitrile-water gradient (1min acetonitrile: the volume ratio of water is 60:40；1-3min acetonitrile: the volume ratio of water is 70:30；3-8min acetonitrile: the volume ratio of water is 80:20)
F) detection wavelength: 203nm
Chromatography validation verification:
Take ginsenoside Rg1's reference substance, ginsenoside Re's reference substance in right amount, accurately weighed, add methanol and be respectively prepared every 1ml solution containing ginsenoside Rg1 0.2mg, ginsenoside Re 0.2mg.
Take ginsenoside Rg1's reference substance, ginsenoside Re's reference substance, accurately weighed, add methanol and make every 1ml mixed solution containing about 0.2mg, to obtain final product, then precision draws this solution 0.5 μ l, 1 μ l, 1.5 μ l, 2 μ l, 3 μ l entrance LC mensuration respectively, and measures according to said method.Carry out linear regression with concentration (mg/ml)-peak area, try to achieve regression equation: ginsenoside Rg1 y=1264.2x+7.6763, R2=0.99979, ginsenoside Rg1 y=1148.8x-0.96132, R2=0.99998, ginsenoside Rg1 is at 0.0911～0.5466mg/ml, and ginsenoside Rg1 is good linear relationship within the scope of 0.1013～0.6078mg/ml.Table 2 and Fig. 1 are ginsenoside Rg1's linear test result；Table 3 and Fig. 2 are ginsenoside Re's linear test result；Wherein, the abscissa indicated concentration of Fig. 1 and 2, vertical coordinate represents peak area.
Table 2 ginsenoside Rg1's linear test result
Table 3 ginsenoside Re's linear test result
The repeatability checking of the extracting process of 1.1 embodiments 1:
Take sample (lot number: the 15071601) 0.2g of identical lot number, totally 3 parts, accurately weighed, extracting need testing solution by ASE extracting method, sample size is 1 μ L, with above-mentioned chromatographic condition parallel test, record the total amount of sample ginsenoside Rg1 and ginsenoside Re in Table 1, RSD is 0.5%, and test shows that ASE extracting method repeatability is good, the results detailed in Table 4.
Table 4
The degree of accuracy test of the extracting process of 1.2 embodiments 1
Folium Ginseng is extracted by the extracting process adopting the ASE extracting process of embodiment 1 and pharmacopeia, and Folium Ginseng is 3 batches, lot number respectively 15071601,120303,1407221；
The Folium Ginseng of same batch is adopted the equipment parallel testing twice of same size by the ASE extracting process of embodiment 1, and respectively ASE1 and ASE2 represents.
Concrete test result is shown in table 5 below；
Table 5
The above-described presently preferred embodiments of the present invention that is only, all any amendment, equivalent replacement and improvement etc. made within the scope of the spirit and principles in the present invention, should be included within protection scope of the present invention.
Claims (5)
1. an ASE extracts the method for ginsenoside Rg_1 and Re in Folium Ginseng, it is characterised in that comprise the following steps:
Step 1: after Folium Ginseng is pulverized, sieve；
Step 2: weigh 0.2 weight portion mangosteen powder, mixs homogeneously stand-by with 1 weight portion kieselguhr；
Step 3: add the obtained mixture of step 2 in the abstraction pool putting filter membrane in advance well, adds appropriate kieselguhr to the Chi Kou reaching abstraction pool；The lid covering abstraction pool carries out static extracting；Extraction is extracted liquid after terminating；
Extraction conditions is: extractant is methanol；Extraction temperature 110 DEG C；Static extracting time 7min；Flush volume 80%；Quiet cycle number of times 3 times.
2. ASE according to claim 1 extracts the method for ginsenoside Rg_1 and Re in Folium Ginseng, it is characterised in that the volume of described abstraction pool is 10ml.
3. ASE according to claim 2 extracts the method for ginsenoside Rg_1 and Re in Folium Ginseng, it is characterised in that the pressure of described static extracting is 1500psi.
4. ASE according to claim 3 extracts the method for ginsenoside Rg_1 and Re in Folium Ginseng, it is characterised in that the purge time of described static extracting is 60s.
5. ASE according to claim 1 extracts the method for ginsenoside Rg_1 and Re in Folium Ginseng, it is characterized in that, also include after step 3: join after extract is diluted in centrifuge tube and purify, obtain filtrate after then filtering, added with graphitic carbon SPE post in described centrifuge tube.
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| Application Number | Priority Date | Filing Date | Title |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101498701A (en) * | 2009-03-09 | 2009-08-05 | 南京大学 | Detection method for phthalate ester residue |
| CN102331468A (en) * | 2011-08-03 | 2012-01-25 | 北京师范大学 | Method for testing water deposits or estrogen coalitions in soil |
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2016
- 2016-04-15 CN CN201610234882.7A patent/CN105801660A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101498701A (en) * | 2009-03-09 | 2009-08-05 | 南京大学 | Detection method for phthalate ester residue |
| CN102331468A (en) * | 2011-08-03 | 2012-01-25 | 北京师范大学 | Method for testing water deposits or estrogen coalitions in soil |
Non-Patent Citations (3)
| Title |
|---|
| 宋文斌等: "加速溶剂萃取-液相色谱-紫外检测法测定人参中多种人参皂甙含量", 《现代科学仪器》 * |
| 李启艳等: "快速溶剂萃取_超高效液相色谱法测定稳心颗粒中皂苷类成分", 《药物分析杂志》 * |
| 石矛等: "快速溶剂萃取仪提取保健食品中人参皂苷条件优化", 《食品安全质量检测报告》 * |
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Application publication date: 20160727 |