CN105954439A - ASE method for extracting isoferulic acid in Rhizoma Cimicifugae - Google Patents
ASE method for extracting isoferulic acid in Rhizoma Cimicifugae Download PDFInfo
- Publication number
- CN105954439A CN105954439A CN201610254586.3A CN201610254586A CN105954439A CN 105954439 A CN105954439 A CN 105954439A CN 201610254586 A CN201610254586 A CN 201610254586A CN 105954439 A CN105954439 A CN 105954439A
- Authority
- CN
- China
- Prior art keywords
- extraction
- rhizoma cimicifugae
- ase
- extracts
- extracting
- 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
- 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
-
- 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
Abstract
The invention discloses an ASE method for extracting isoferulic acid in Rhizoma Cimicifugae. The method comprises the following steps: step 1, crushing Rhizoma Cimicifugae and then sieving the crushed Rhizoma Cimicifugae; step 2, weighing 0.5 part by weight of Rhizoma Cimicifugae powder, uniformly mixing the Rhizoma Cimicifugae powder with 1 part by weight of quartz sand and standing the obtained mixture for subsequent usage; and step 3, adding a proper amount of quartz sand into an extraction pool equipped with a filtering membrane in advance until the quartz sand reaches the mouth of the extraction pool, covering a cover of the extraction pool and carrying out static extraction, wherein extract is obtained after completion of extraction, and extraction conditions are that 40% methanol is used as an extraction solvent, extraction temperature is 120 DEG C, static extraction time is 5 min, a flushing volume is 60%, four static cycles are carried out, and the volume percentage of 40% methanol is 40%. The ASE method for extracting isoferulic acid in Rhizoma Cimicifugae is simple to operate and high in detection precision.
Description
Technical field
The present invention relates to test in laboratory field, a kind of ASE method extracts the method for Hesperetic acid in Rhizoma Cimicifugae.
Background technology
Pharmacopeia in 2010 have recorded the method for Hesperetic acid in Rhizoma Cimicifugae of extracting: takes this product powder (crossing No. two sieves) about 0.5g,
Accurately weighed, put in tool plug conical flask, accurate addition 10% ethanol 25ml, close plug, weighed weight, it is heated to reflux 2.5 hours, puts
Cold, more weighed weight, supply the weight of less loss with 10% ethanol, shake up, filter, take subsequent filtrate, to obtain final product.Chromatographic condition is: with
Octadecylsilane chemically bonded silica is filler；With acetonitrile-0.1% phosphoric acid solution (13:87) for flowing phase；Detection wavelength is
316nm.Number of theoretical plate is calculated by Hesperetic acid peak should be not less than 5000.
The method operating process of pharmacopeia is complicated, 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 method and extract the method for Hesperetic acid in Rhizoma Cimicifugae, the method is simple to operate,
The method that extraction results is recorded with pharmacopeia is consistent.
The technical scheme that the present invention provides is: a kind of ASE method extracts the method for Hesperetic acid in Rhizoma Cimicifugae, including following step
Rapid:
Step 1: after Rhizoma Cimicifugae is pulverized, sieve；
Step 2: weigh 0.5 weight portion Rhizoma Cimicifugae powder, mix homogeneously stand-by with 1 weight portion quartz sand；
Step 3: add appropriate quartz sand in the abstraction pool putting filter membrane in advance well to the Chi Kou reaching abstraction pool；Lid
The lid of upper abstraction pool carries out static extracting；Extraction is extracted liquid after terminating；
Extraction conditions is: extractant is 40% methanol aqueous solution；Extraction temperature 120 DEG C；Static extracting time 5min；Punching
Wash volume 60%；Quiet cycle number of times 4 times；The described percentage by volume that 40% methanol aqueous solution is methanol is 40%.
In above-mentioned ASE method extracts Rhizoma Cimicifugae in the method for Hesperetic acid, the volume of described abstraction pool is 10ml.
In above-mentioned ASE method extracts Rhizoma Cimicifugae in the method for Hesperetic acid, the pressure of described static extracting is
1500psi。
In above-mentioned ASE method extracts Rhizoma Cimicifugae in the method for Hesperetic acid, the purge time of described static extracting is
90s。
In above-mentioned ASE method extracts Rhizoma Cimicifugae in the method for Hesperetic acid, also include after step 3: extract is existed
Under conditions of 15000r/min, centrifugal 3min, takes supernatant.
In above-mentioned ASE method extracts Rhizoma Cimicifugae in the method for Hesperetic acid, the instrument that described ASE extraction is used
For ASE350 Accelerate solvent extraction instrument.
The present invention is after using technique scheme, and it has the beneficial effect that
The extracting process of the present invention is simple to operate, and extraction time is short, and the method that effect of extracting is recorded with pharmacopeia is consistent, repeats
Property is good.
Accompanying drawing explanation
Fig. 1 is the rectangular plots of the chromatography validation verification of the present invention；
Fig. 2 is the chromatogram of the Hesperetic acid reference substance of the present invention；
Fig. 3 is that the present invention uses official method to test the chromatogram obtained；
Fig. 4 is the extraction of the present invention and method of testing obtains chromatogram.
Detailed description of the invention
Below in conjunction with detailed description of the invention, technical scheme is described in further detail, but do not constitute right
Any restriction of the present invention.
Embodiment 1:
Size-reduced for Rhizoma Cimicifugae machine was pulverized No. three sieves, about 0.5g, accurately weighed, mix homogeneously with 1g quartz sand, stand-by, move
Enter to putting glass fiber filter in advance well10ml abstraction pool adds appropriate amount of quartz sand, gently shaking be allowed to
Chi Kou in the same horizontal line, tightens abstraction pool upper cover.After extraction terminates, extract is shifted in 50ml volumetric flask, use
20% methanol dilution is to scale, and under 15000r/min, centrifugal 3min, takes supernatant, enters LC and measures.
Extraction conditions (being shown in Table 1) is:
Table 1
| Best practice | |
| Abstraction pool volume (ml) | 10 |
| Extractant | 40% methanol |
| Pressure (psi) | 1500 |
| Temperature (DEG C) | 120 |
| The static extracting time (min) | 5 |
| Quiet cycle number of times | 4 |
| Flush volume (%) | 60 |
| Purge time (s) | 90 |
Analysis method is LC liquid chromatography, liquid-phase chromatographic analysis condition:
A) the double ternary liquid phase (U-3000) of instrument: Thermo；
B) chromatographic column: Thermo Syncronis C18 3*100mm 3um, i.e. carbon 18 chromatographic column, diameter 3mm, length
100mm, particle diameter 3 microns；
C) column temperature: 40 DEG C；
D) flow velocity: 0.5mL/min；
E) flowing phase: acetonitrile-0.1% phosphoric acid；Wherein, acetonitrile and volume ratio 13 that mass percent is 0.1% phosphoric acid:
87；It should be noted that in the present invention, volume ratio refers both to the volume ratio under the conditions of 20 DEG C.
F) detection wavelength: 316nm；
Chromatography validation verification:
Take Hesperetic acid reference substance appropriate, accurately weighed, add methanol and make every 1ml solution containing 40ug, obtain different Resina Ferulae
Acid reference substance.
Take Hesperetic acid reference substance appropriate, accurately weighed, put in brown measuring bottle, add 10% ethanol make every 1ml containing different Ah
The solution of acid Wei 40 μ g, then precision absorption this solution 0.1 μ l, 0.2 μ l, 0.5 μ l, 1 μ l, 2 μ l enter LC and measure, and depend on respectively
Measure according to said method, the results detailed in Table 2；Accompanying drawing 1 is corresponding with table 2, accompanying drawing 1 abscissa indicated concentration, and vertical coordinate represents face, peak
Long-pending.Accompanying drawing 2 is the chromatogram using above-mentioned LC liquid chromatography for measuring of Hesperetic acid reference substance.
Table 2
The repeatability checking of the extracting process of embodiment 1:
Take sample (lot number: the 1504183) 0.5g of identical lot number, totally 3 parts, accurately weighed, extract by ASE extracting method and supply
Test sample solution, sample size is 1 μ L, with above-mentioned chromatographic condition parallel test, records the content of Hesperetic acid in sample and is shown in Table two,
RSD is 2.70%, and test shows that ASE extracting method repeatability is good, the results detailed in Table 3
Table 3
The degree of accuracy test of the extracting process of embodiment 1
Using the ASE extracting process of embodiment 1 and the extracting process of pharmacopeia to extract Rhizoma Cimicifugae, Rhizoma Cimicifugae is 2 batches, lot number
It is respectively 1504183,20150801；
The ASE extracting process of embodiment 1 is to a batch of Rhizoma Cimicifugae parallel testing twice, respectively ASE1 and ASE2 table
Show.
Fig. 3 is the chromatogram that sample 1504183 obtains according to the method described in pharmacopeia；
Fig. 4 is that sample 1504183 obtains according to ASE extracting process and LC liquid chromatography test (ASE2) of the present invention
Chromatogram.
Concrete test result see table 4；
Table 4
Above-described be only presently preferred embodiments of the present invention, all made in the range of the spirit and principles in the present invention appoint
What amendment, equivalent and improvement etc., should be included within the scope of the present invention.
Claims (6)
1. an ASE method extracts the method for Hesperetic acid in Rhizoma Cimicifugae, it is characterised in that comprise the following steps:
Step 1: after Rhizoma Cimicifugae is pulverized, sieve；
Step 2: weigh 0.5 weight portion Rhizoma Cimicifugae powder, mix homogeneously stand-by with 1 weight portion quartz sand；
Step 3: add appropriate quartz sand in the abstraction pool putting filter membrane in advance well to the Chi Kou reaching abstraction pool；Cover extraction
The lid taking pond carries out static extracting；Extraction is extracted liquid after terminating；
Extraction conditions is: extractant is 40% methanol aqueous solution；Extraction temperature 120 DEG C；Static extracting time 5min；Rinse body
Long-pending 60%；Quiet cycle number of times 4 times；The described percentage by volume that 40% methanol aqueous solution is methanol is 40%.
ASE method the most according to claim 1 extracts the method for Hesperetic acid in Rhizoma Cimicifugae, it is characterised in that described extraction
The volume taking pond is 10ml.
ASE method the most according to claim 1 extracts the method for Hesperetic acid in Rhizoma Cimicifugae, it is characterised in that described is quiet
The pressure of state extraction is 1500psi.
ASE method the most according to claim 1 extracts the method for Hesperetic acid in Rhizoma Cimicifugae, it is characterised in that described is quiet
The purge time of state extraction is 90s.
ASE method the most according to claim 1 extracts the method for Hesperetic acid in Rhizoma Cimicifugae, it is characterised in that after step 3
Also include: by extract centrifugal 3min under conditions of 15000r/min, take supernatant.
ASE method the most according to claim 1 extracts the method for Hesperetic acid in Rhizoma Cimicifugae, it is characterised in that described ASE
The instrument that extraction is used is ASE350 Accelerate solvent extraction instrument.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610254586.3A CN105954439A (en) | 2016-04-22 | 2016-04-22 | ASE method for extracting isoferulic acid in Rhizoma Cimicifugae |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610254586.3A CN105954439A (en) | 2016-04-22 | 2016-04-22 | ASE method for extracting isoferulic acid in Rhizoma Cimicifugae |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105954439A true CN105954439A (en) | 2016-09-21 |
Family
ID=56914715
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610254586.3A Pending CN105954439A (en) | 2016-04-22 | 2016-04-22 | ASE method for extracting isoferulic acid in Rhizoma Cimicifugae |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105954439A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106885861A (en) * | 2017-04-11 | 2017-06-23 | 广西壮族自治区梧州食品药品检验所 | A kind of method that ASE HPLC methods determine isoferulic acid content in rattletop |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2004088271A2 (en) * | 2002-10-29 | 2004-10-14 | Target Discovery, Inc. | Method for increasing ionization efficiency in mass spectroscopy |
| CN1675554A (en) * | 2002-08-19 | 2005-09-28 | N·V·努特里西阿 | Matrixes for matrix-assisted laser desorption/ionization and application thereof |
| US20060183863A1 (en) * | 2005-02-14 | 2006-08-17 | Ciphergen Biosystems, Inc. | Zwitterionic polymers |
| WO2013007807A1 (en) * | 2011-07-12 | 2013-01-17 | Bionorica Se | Selected cimicifuga fractions for the treatment of osteoporosis |
| CN103235054A (en) * | 2013-04-17 | 2013-08-07 | 宁波检验检疫科学技术研究院 | Method for determining banned and restricted compounds in toys with accelerated solvent extraction and gas chromatograph-mass spectrometer |
| CN104749280A (en) * | 2015-03-30 | 2015-07-01 | 神威药业集团有限公司 | Quality control method for salvia miltiorrhiza injection |
-
2016
- 2016-04-22 CN CN201610254586.3A patent/CN105954439A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1675554A (en) * | 2002-08-19 | 2005-09-28 | N·V·努特里西阿 | Matrixes for matrix-assisted laser desorption/ionization and application thereof |
| WO2004088271A2 (en) * | 2002-10-29 | 2004-10-14 | Target Discovery, Inc. | Method for increasing ionization efficiency in mass spectroscopy |
| US20060183863A1 (en) * | 2005-02-14 | 2006-08-17 | Ciphergen Biosystems, Inc. | Zwitterionic polymers |
| WO2013007807A1 (en) * | 2011-07-12 | 2013-01-17 | Bionorica Se | Selected cimicifuga fractions for the treatment of osteoporosis |
| CN103235054A (en) * | 2013-04-17 | 2013-08-07 | 宁波检验检疫科学技术研究院 | Method for determining banned and restricted compounds in toys with accelerated solvent extraction and gas chromatograph-mass spectrometer |
| CN104749280A (en) * | 2015-03-30 | 2015-07-01 | 神威药业集团有限公司 | Quality control method for salvia miltiorrhiza injection |
Non-Patent Citations (4)
| Title |
|---|
| SUDARSAN MUKHOPADHYAY 等: "Optimization of extraction process for phenolic acids from black cohosh (Cimicifuga racemosa) by pressurized liquid extraction", 《JOURNAL OF THE SCIENCE OF FOOD AND AGRICULTURE》 * |
| 刘平怀: "《生物工艺实验》", 31 March 2012 * |
| 司丹丹 等: "RP-HPLC法同时测定升麻中3种有机酸的含量", 《沈阳药科大学学报》 * |
| 李攻科 等: "《样品前处理仪器与装置》", 31 May 2007 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106885861A (en) * | 2017-04-11 | 2017-06-23 | 广西壮族自治区梧州食品药品检验所 | A kind of method that ASE HPLC methods determine isoferulic acid content in rattletop |
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 | |
| CN105954381A (en) | Determination method for isoferulic acid in Rhizoma Cimicifugae | |
| CN105891380A (en) | Method using ASE method to extract linarin in buddleja officinalis | |
| CN105687675A (en) | Method for extracting peimine and peiminine from Fritillaria thunbergii | |
| CN105954385A (en) | Method for extracting oleanolic acid and hederagenin in clematis root | |
| CN105954383A (en) | Determination method for oleanolic acid and hederagenin in clematis root | |
| CN105954439A (en) | ASE method for extracting isoferulic acid in Rhizoma Cimicifugae | |
| CN105699577A (en) | Method for analyzing amentoflavone in selaginella tamariscina | |
| CN105929058A (en) | Determination method for indirubin in Folium isatidis | |
| CN105738536A (en) | Extraction method for indirubin in folium isatidis | |
| CN105929090A (en) | Method for extracting curculigoside in Curculigo orchioides | |
| CN105675765A (en) | Determination method for prim-O-glucosylcimifugin and 5-O-methylvisammioside in radix saposhnikoviae | |
| CN105699542A (en) | Method for measuring cimicifugoside, cimifugin, sec-o-glucosylhamaudol and 5-O-methylvisammioside in divaricate saposhnikovia roots | |
| CN105784869A (en) | Determination method for psoralen and isopsoralen in fructus psoraleae | |
| CN105954407A (en) | Method for determination of curculigine in curculigo orchioides | |
| CN105699543A (en) | Determination method for rosmarinic acid in perilla fruit | |
| CN105954386A (en) | ASE extraction method for rosmarinic acid in perilla seed | |
| CN105954387A (en) | Determination method for curculigoside in Curculigo orchioides | |
| CN105929073A (en) | Method for simultaneously detecting baicalin and baicalein in Radix Scutellariae | |
| CN105954405A (en) | Method for determination of pectolinarin in buddleja officinalis | |
| CN105651903A (en) | Determination method of siraitia grosvenorii saponin V in siraitia grosvenorii | |
| CN105699541A (en) | Method for measuring astragaloside in spleen-stomach invigorating and qi replenishing pill through rapid solvent extraction-HPLC-ELSD |
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 |
Application publication date: 20160921 |
|
| RJ01 | Rejection of invention patent application after publication |