CN105651903A - Determination method of siraitia grosvenorii saponin V in siraitia grosvenorii - Google Patents
Determination method of siraitia grosvenorii saponin V in siraitia grosvenorii Download PDFInfo
- Publication number
- CN105651903A CN105651903A CN201610234705.9A CN201610234705A CN105651903A CN 105651903 A CN105651903 A CN 105651903A CN 201610234705 A CN201610234705 A CN 201610234705A CN 105651903 A CN105651903 A CN 105651903A
- Authority
- CN
- China
- Prior art keywords
- grosvenor momordica
- extraction
- measuring method
- triterpene glucoside
- liquid
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
- G01N2030/027—Liquid chromatography
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N2030/062—Preparation extracting sample from raw material
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Steroid Compounds (AREA)
Abstract
The invention discloses a determination method of siraitia grosvenorii saponin V in siraitia grosvenorii. The determination method comprises the following steps: step 1: crushing the siraitia grosvenorii and extracting the siraitia grosvenorii with an ASE (Accelerated Solvent Extraction) method to obtain an extracting solution; step 2: after carrying out centrifugal separation on the extracting solution to obtain liquid supernatant; and step 3: analyzing the liquid supernatant by adopting liquid chromatography. The invention provides the determination method of the siraitia grosvenorii saponin V in the siraitia grosvenorii. The method disclosed by the invention is simple to operate and high in detection precision.
Description
Technical field
The present invention relates to test in laboratory field, particularly the measuring method of triterpene glucoside V in a kind of Grosvenor Momordica.
Background technology
Within 2010, pharmacopeia have recorded the method extracting triterpene glucoside V in Grosvenor Momordica: gets this product powder (crossing No. four sieves) about 0.5g, accurately weighed, to put in tool plug Erlenmeyer flask, precision adds methyl alcohol 50ml, close plug, weighed weight, reflux 2 hours, lets cool, weighed weight again, supply the weight of less loss with methyl alcohol, shake even, filter. Precision measures continuous filtrate 20ml, and recycling design is to dry, and the 10ml that adds water dissolves, by macroporous adsorptive resins AB-8 (internal diameter is 1cm, and post height is 10cm), with water 100ml wash-out, abandon the liquid that anhydrates, then with 20% ethanol 100ml wash-out, abandon elutriant, continuing with Diluted Alcohol 100ml wash-out, collect elutriant, recycling design is to dry, residue adds moving phase and dissolves, and is transferred in 10ml measuring bottle, adds moving phase to scale, shake even, to obtain final product.
The parameter of its liquid chromatography is: take octadecylsilane chemically bonded silica as weighting agent; Taking acetonitrile-water (23:77) as moving phase; Determined wavelength is 203nm. Theoretical stage number calculates by triterpene glucoside V peak should be not less than 3000.
The method operating process of pharmacopeia is complicated, requires high to the operating skill of operator.
Summary of the invention
It is an object of the invention to provide the measuring method of triterpene glucoside V in a kind of Grosvenor Momordica, the method is simple to operate, accuracy of detection height.
Technical scheme provided by the invention is: the measuring method of triterpene glucoside V in a kind of Grosvenor Momordica, comprises the following steps:
Step 1: adopt the extraction of ASE extraction process to be extracted liquid after being pulverized by Grosvenor Momordica;
Step 2: after extraction liquid centrifugation, obtain supernatant liquor;
Step 3: adopt liquid phase chromatography to analyze supernatant liquor;
Wherein, the analysis condition of liquid phase chromatography is:
A) instrument: two ternary liquid phase
B) chromatographic column specification: 3*100mm3um
C) post temperature: 40 DEG C
D) flow velocity: 0.3mL/min
E) moving phase: acetonitrile-water, volume ratio 23:77
F) determined wavelength: 203nm.
In above-mentioned Grosvenor Momordica in the measuring method of triterpene glucoside V, described step 1 is specially:
S11: after Grosvenor Momordica is pulverized, sieve;
S12: take 0.5 weight part mangosteen powder, mixes stand-by with 1 weight part diatomite;
S13: first add 2 weight part silica gel in the abstraction pool putting filtering membrane in advance well, adds appropriate diatomite to the Chi Kou reaching abstraction pool after mixing; The lid covering abstraction pool carries out static extracting; Extraction is extracted liquid after terminating;
Extraction conditions is: extraction solvent is methyl alcohol; Extraction temperature 100 DEG C; Static extracting time 5min; Flush volume 100%; Quiet cycle number of times 1 time.
In above-mentioned Grosvenor Momordica in the measuring method of triterpene glucoside V, the volume of described abstraction pool is 10ml.
In above-mentioned Grosvenor Momordica in the measuring method of triterpene glucoside V, the pressure of described static extracting is 1500psi.
In above-mentioned Grosvenor Momordica in the measuring method of triterpene glucoside V, the purge time of described static extracting is 60s.
In above-mentioned Grosvenor Momordica in the measuring method of triterpene glucoside V, step 2 is specially: by extraction liquid centrifugal 3min when 15000r/min, get supernatant liquor.
In above-mentioned Grosvenor Momordica in the measuring method of triterpene glucoside V, described instrument is ThermoU3000UHPLC liquid chromatograph.
In above-mentioned Grosvenor Momordica in the measuring method of triterpene glucoside V, described chromatographic column is ThermoSyncronisC18.
In above-mentioned Grosvenor Momordica in the measuring method of triterpene glucoside V, the instrument that described ASE extraction process adopts is ASE350 Accelerate solvent extraction instrument.
The present invention is after adopting technique scheme, and its useful effect having is:
The detection method of the present invention is simple to operate, and precision is consistent with the precision of official method, and repeatability is good.
Accompanying drawing explanation
Fig. 1 is the rectangular coordinates figure of the stratographic analysis validation verification of the present invention;
Fig. 2 is the color atlas of the triterpene glucoside V reference substance of the present invention;
Fig. 3 is that the present invention adopts official method to test the color atlas obtained;
Fig. 4 is that the extraction of the present invention and testing method obtain color atlas.
Embodiment
Below in conjunction with embodiment, the technical scheme of the present invention is described in further detail, but does not form any limitation of the invention.
Embodiment 1:
Grosvenor Momordica is pulverized through pulverizer, cross No. three sieves, about 0.5g, accurately weighed, mix with 1g diatomite, stand-by, putting filtering membrane in advance well10ml abstraction pool first adds 2g silica gel, after add the sample mixed, then add appropriate diatomite, gently jolting make it with Chi Kou in the same horizontal line, tighten abstraction pool upper cover. Extraction is shifted extraction liquid in 25ml volumetric flask, is diluted to scale with methyl alcohol after terminating, and under 15000r/min, centrifugal 3min, gets supernatant liquor, enters LC and measures.
Extraction conditions (see table 1) is:
Table 1
| Close with pharmacopeia | |
| Abstraction pool volume (ml) | 10 |
| Extraction solvent | Methyl alcohol |
| Pressure (psi) | 1500 |
| Temperature (DEG C) | 100 |
| The static extracting time (min) | 5 |
| Quiet cycle number of times | 1 |
| Flush volume (%) | 100 |
| Purge time (s) | 60 |
Analytical procedure is LC liquid phase chromatography, liquid-phase chromatographic analysis condition:
A) the two ternary liquid phase (U-3000) of instrument: Thermo;
B) chromatographic column: ThermoSyncronisC183*100mm3um, i.e. carbon 18 chromatographic column, diameter 3mm, length 100mm, particle diameter 3 microns;
C) post temperature: 40 DEG C;
D) flow velocity: 0.3mL/min;
E) moving phase: acetonitrile-water (volume ratio 23:77);
F) determined wavelength: 203nm;
Stratographic analysis validation verification:
Get triterpene glucoside V reference substance appropriate, accurately weighed, add moving phase and make the solution of every 1ml containing 0.2mg, obtain triterpene glucoside V reference substance.
Get triterpene glucoside V reference substance appropriate, accurately weighed, put in brown measuring bottle, acetonitrile makes the solution of every 1ml containing isoferulic acid 880.4 �� g to add 50%, then accurate this solution 0.1 �� l of absorption, 0.2 �� l, 0.5 �� l, 0.8 �� l, 1.0 �� l enter LC and measure respectively, and according to above-mentioned LC liquid chromatography for measuring, the results detailed in Table 2; Accompanying drawing 1 is corresponding with table 2, and accompanying drawing 1 X-coordinate indicated concentration, ordinate zou represents peak area. Accompanying drawing 2 is the color atlas adopting above-mentioned LC liquid chromatography for measuring of triterpene glucoside V reference substance.
Table 2
The circulation ratio checking of the extracting process of 1.1 embodiments 1:
Get the sample (lot number: 1510180) 0.5g of identical lot number, totally 6 parts, accurately weighed, extracting need testing solution by ASE extracting method, sample size is 1 �� L, with above-mentioned chromatographic condition parallel test, the content recording triterpene glucoside V in sample is in table 2, RSD is 1.46%, and test shows that ASE extracting method repeatability is good, the results detailed in Table 3
Table 3
The tolerance range test of the extracting process of 1.2 embodiments 1
Adopting the ASE extracting process of embodiment 1 and the extracting process of pharmacopeia to be extracted by Grosvenor Momordica, Grosvenor Momordica is 3 batches, and lot number is respectively 1508166,1510180,150723;
The ASE extracting process of embodiment 1, to the Grosvenor Momordica parallel testing twice of same batch, is respectively ASE1 and ASE2 and represents.
Fig. 3 is the color atlas that sample 1510180 obtains according to the method described in pharmacopeia;
Fig. 4 is the color atlas that sample 1510180 obtains according to ASE extracting process and LC liquid phase chromatography test (ASE2) of the present invention.
Concrete test result sees the following form 4;
Table 4
The above-described better embodiment being only the present invention, all any amendment, equivalent replacement and improvement etc. done within the scope of the spirit and principles in the present invention, all should be included within protection scope of the present invention.
Claims (9)
1. the measuring method of triterpene glucoside V in a Grosvenor Momordica, it is characterised in that, comprise the following steps:
Step 1: adopt the extraction of ASE extraction process to be extracted liquid after being pulverized by Grosvenor Momordica;
Step 2: after extraction liquid centrifugation, obtain supernatant liquor;
Step 3: adopt liquid phase chromatography to analyze supernatant liquor;
Wherein, the analysis condition of liquid phase chromatography is:
A) instrument: two ternary liquid phase chromatographic instrument
B) chromatographic column specification: carbon 18 chromatographic column, 3*100mm3um
C) post temperature: 40 DEG C
D) flow velocity: 0.3mL/min
E) moving phase: acetonitrile-water, volume ratio 23:77
F) determined wavelength: 203nm.
2. the measuring method of triterpene glucoside V in Grosvenor Momordica according to claim 1, it is characterised in that, described step 1 is specially:
S11: after Grosvenor Momordica is pulverized, sieve;
S12: take 0.5 weight part mangosteen powder, mixes stand-by with 1 weight part diatomite;
S13: first add 2 weight part silica gel in the abstraction pool putting filtering membrane in advance well, adds appropriate diatomite to the Chi Kou reaching abstraction pool after mixing; The lid covering abstraction pool carries out static extracting; Extraction is extracted liquid after terminating;
Extraction conditions is: extraction solvent is methyl alcohol; Extraction temperature 100 DEG C; Static extracting time 5min; Flush volume 100%; Quiet cycle number of times 1 time.
3. the measuring method of triterpene glucoside V in Grosvenor Momordica according to claim 2, it is characterised in that, the volume of described abstraction pool is 10ml.
4. the measuring method of triterpene glucoside V in Grosvenor Momordica according to claim 2, it is characterised in that, the pressure of described static extracting is 1500psi.
5. the measuring method of triterpene glucoside V in Grosvenor Momordica according to claim 2, it is characterised in that, the purge time of described static extracting is 60s.
6. the measuring method of triterpene glucoside V in Grosvenor Momordica according to claim 1, it is characterised in that, step 2 is specially: by extraction liquid centrifugal 3min when 15000r/min, get supernatant liquor.
7. the measuring method of triterpene glucoside V in Grosvenor Momordica according to claim 1, it is characterised in that, described instrument is ThermoU3000UHPLC liquid chromatograph.
8. the measuring method of triterpene glucoside V in Grosvenor Momordica according to claim 7, it is characterised in that, described chromatographic column is ThermoSyncronisC18.
9. the measuring method of triterpene glucoside V in Grosvenor Momordica according to claim 1, it is characterised in that, the instrument that described ASE extraction process adopts is ASE350 Accelerate solvent extraction instrument.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610234705.9A CN105651903A (en) | 2016-04-15 | 2016-04-15 | Determination method of siraitia grosvenorii saponin V in siraitia grosvenorii |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610234705.9A CN105651903A (en) | 2016-04-15 | 2016-04-15 | Determination method of siraitia grosvenorii saponin V in siraitia grosvenorii |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105651903A true CN105651903A (en) | 2016-06-08 |
Family
ID=56496508
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610234705.9A Pending CN105651903A (en) | 2016-04-15 | 2016-04-15 | Determination method of siraitia grosvenorii saponin V in siraitia grosvenorii |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105651903A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107064346A (en) * | 2017-03-29 | 2017-08-18 | 广西壮族自治区梧州食品药品检验所 | A kind of method that ASE HPLC determine triterpene glucoside V content in Momordica grosvenori |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102030795A (en) * | 2010-11-30 | 2011-04-27 | 哈尔滨商业大学 | Cucurbitane momordicoside and preparation method thereof |
| CN102973861A (en) * | 2012-12-21 | 2013-03-20 | 广西健丰药业有限公司 | Preparation method and quality control method of sugar-free compound fructus momordicae antitussive particles |
-
2016
- 2016-04-15 CN CN201610234705.9A patent/CN105651903A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102030795A (en) * | 2010-11-30 | 2011-04-27 | 哈尔滨商业大学 | Cucurbitane momordicoside and preparation method thereof |
| CN102973861A (en) * | 2012-12-21 | 2013-03-20 | 广西健丰药业有限公司 | Preparation method and quality control method of sugar-free compound fructus momordicae antitussive particles |
Non-Patent Citations (4)
| Title |
|---|
| 国家药典委员会: "罗汉果", 《中国药典2015年版》 * |
| 胡军影等: "R P 一H P L C 法测定罗汉果中罗汉果皂普V 的含量", 《药物分析杂志》 * |
| 贾林等: "ASE -HPLC法测定黄姜中薯蓣皂甙元的含量", 《化学分析计量》 * |
| 陈静: "人参、西洋参和三七药材内皂苷类有效成分分析的完整解决方案", 《道客巴巴》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107064346A (en) * | 2017-03-29 | 2017-08-18 | 广西壮族自治区梧州食品药品检验所 | A kind of method that ASE HPLC determine triterpene glucoside V content in Momordica grosvenori |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105954377A (en) | Extraction method for amentoflavone in Selaginella tamariscina | |
| CN105929059A (en) | Determination method for amygdalin in peach seed | |
| CN105954380A (en) | Determination method for linarin in Buddleja officinalis | |
| CN105651925A (en) | Determination method of ginsenosides Rg1 and Re in ginseng leaves | |
| CN105891380A (en) | Method using ASE method to extract linarin in buddleja officinalis | |
| CN105954383A (en) | Determination method for oleanolic acid and hederagenin in clematis root | |
| CN105699562B (en) | The assay method of oleanolic acid in a kind of root of Chinese clematis | |
| CN105954385A (en) | Method for extracting oleanolic acid and hederagenin in clematis root | |
| CN105687675A (en) | Method for extracting peimine and peiminine from Fritillaria thunbergii | |
| CN105699577A (en) | Method for analyzing amentoflavone in selaginella tamariscina | |
| CN105651903A (en) | Determination method of siraitia grosvenorii saponin V in siraitia grosvenorii | |
| CN105929058A (en) | Determination method for indirubin in Folium isatidis | |
| CN105699542A (en) | Method for measuring cimicifugoside, cimifugin, sec-o-glucosylhamaudol and 5-O-methylvisammioside in divaricate saposhnikovia roots | |
| CN105699543A (en) | Determination method for rosmarinic acid in perilla fruit | |
| CN105929090A (en) | Method for extracting curculigoside in Curculigo orchioides | |
| CN105675765A (en) | Determination method for prim-O-glucosylcimifugin and 5-O-methylvisammioside in radix saposhnikoviae | |
| CN105699541A (en) | Method for measuring astragaloside in spleen-stomach invigorating and qi replenishing pill through rapid solvent extraction-HPLC-ELSD | |
| CN105911176A (en) | Detection method of peimine and peiminine in thunberg fritillary bulb | |
| CN105954407A (en) | Method for determination of curculigine in curculigo orchioides | |
| CN105929071A (en) | Method for detecting mogroside V in Fructus Momordicae | |
| CN105784869A (en) | Determination method for psoralen and isopsoralen in fructus psoraleae | |
| CN105954386A (en) | ASE extraction method for rosmarinic acid in perilla seed | |
| CN106872611A (en) | A kind of method that ASE HPLC methods determine amentoflavone content in Selaginella tamariscina | |
| CN105954439A (en) | ASE method for extracting isoferulic acid in Rhizoma Cimicifugae | |
| CN105954387A (en) | Determination method for curculigoside in Curculigo orchioides |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20160608 |