CN105929089A - Method for extracting cimicifugoside, cimicifugin, sec-o-glucosylhamaudol and 5-O-methylvisammioside in divaricate saposhnikovia root - Google Patents
Method for extracting cimicifugoside, cimicifugin, sec-o-glucosylhamaudol and 5-O-methylvisammioside in divaricate saposhnikovia root Download PDFInfo
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- CN105929089A CN105929089A CN201610254653.1A CN201610254653A CN105929089A CN 105929089 A CN105929089 A CN 105929089A CN 201610254653 A CN201610254653 A CN 201610254653A CN 105929089 A CN105929089 A CN 105929089A
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- cimicifugoside
- glucosylhamaudol
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- 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
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- 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
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- 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
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Abstract
The invention discloses a method for extracting cimicifugoside, cimicifugin, sec-o-glucosylhamaudol and 5-O-methylvisammioside in divaricate saposhnikovia root. The method comprises the following steps: step 1, crushing the divaricate saposhnikovia root and sieving the crushed divaricate saposhnikovia root; step 2, weighing 0.25 part by weight of divaricate saposhnikovia root powder, uniformly mixing the divaricate saposhnikovia root powder with 0.3 part by weight of diatomite and standing the obtained mixture for subsequent usage; step 3, transferring the mixture obtained in the step 2 into an extraction tank equipped with a filtering membrane in advance, adding a proper amount of diatomite until the diatomite reaches the mouth of the extraction tank, covering a cover of the extraction tank and carrying out static extraction, wherein extract is obtained after completion of extraction, and extraction conditions are that a mixed solution of methanol and ethanol in a volume ratio of 9: 1 is used as an extraction solvent, extraction temperature is 110 DEG C, static extraction time is 7 min, a flushing volume is 100% and three static cycles are carried out. The method for extracting cimicifugoside, cimicifugin, sec-o-glucosylhamaudol and 5-O-methylvisammioside in the divaricate saposhnikovia root is simple to operate, thorough in extraction and short in operation time.
Description
Technical field
The present invention relates to test in laboratory field, cimicifugoside in particularly a kind of extraction Radix Saposhnikoviae, cimifugin, sec-o-glucosylhamaudol and
The method of 5-O-methyl-visamminol.
Background technology
Within 2015, pharmacopeia have recorded cimicifugoside and the extracting method of 5-O-methyl-visamminol in Radix Saposhnikoviae: takes this product thin
Powder about 0.25g, accurately weighed, put in tool plug conical flask, the accurate methanol 10ml that adds, weighed weight, water-bath refluxes 2 little
Time, let cool, more weighed weight, supply the weight of less loss with methanol, shake up, filter, take subsequent filtrate, to obtain final product.
Liquid chromatographic detection condition is: with octadecylsilane chemically bonded silica as filler；With methanol-water (40:60) it is
Flowing phase；Detection wavelength is 254nm.Number of theoretical plate is calculated by cimicifugoside peak should be not less than 2000.
" in HPLC method mensuration Radix Saposhnikoviae, cimicifugoside, cimifugin, 5-O-methyl-visamminol and sec-o-glucosylhamaudol contains document
Amount " the 6th phase of volume 28 pharmacy time magazine on November 25th, 2010 describe by reflux, extract, cimicifugoside, cimifugin,
5-O-methyl-visamminol and the content of sec-o-glucosylhamaudol method for measuring.
Pharmacopeia and method operating process of the prior art are complicated, and the operant skill of operator is required height.
Summary of the invention
It is an object of the invention to provide cimicifugoside, cimifugin, sec-o-glucosylhamaudol and 5-O-methyl in a kind of extraction Radix Saposhnikoviae and tie up this
The method of ammiol glycosides, the method is simple to operate, and thoroughly, the operating time is short in extraction.
The technical scheme that the present invention provides is: cimicifugoside, cimifugin, sec-o-glucosylhamaudol and 5-O-first in a kind of extraction Radix Saposhnikoviae
The method of base visamminol glycosides, comprises the following steps:
Step 1: after Radix Saposhnikoviae is pulverized, sieve；
Step 2: weigh 0.25 weight portion Radix Saposhnikoviae powder, mixs homogeneously stand-by with 0.3 weight portion kieselguhr；
Step 3: the mixture in S12 is moved in the abstraction pool putting filter membrane in advance well, add appropriate kieselguhr to reaching
Chi Kou to abstraction pool；The lid covering abstraction pool carries out static extracting；Extraction is extracted liquid after terminating；
Extraction conditions is: extractant be volume ratio be methanol and the mixed solution of ethanol of 9:1；Extraction temperature 110 DEG C；
Static extracting time 7min；Flush volume 100%；Quiet cycle number of times 3 times.
Cimicifugoside, cimifugin, sec-o-glucosylhamaudol and the method for 5-O-methyl-visamminol in above-mentioned extraction Radix Saposhnikoviae
In, the volume of described abstraction pool is 5ml, and the pressure of described static extracting is 1500psi, described static extracting
Purge time is 100s.
Cimicifugoside, cimifugin, sec-o-glucosylhamaudol and the method for 5-O-methyl-visamminol in above-mentioned extraction Radix Saposhnikoviae
In, the instrument that described ASE extraction is used is 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 thoroughly, the operating time is short in extraction.
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 this
Bright any restriction.
Embodiment 1:
Size-reduced for Radix Saposhnikoviae machine is pulverized, crosses No. five sieves, take about 0.25g, accurately weighed, mix homogeneously with 0.3g kieselguhr,
Stand-by, it is moved into and puts filter membrane in advance wellAbstraction pool adds proper amount of silicon diatomaceous earth, 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,
With methanol dilution to scale, shake up, filter, take subsequent filtrate, to obtain final product.
Extraction conditions (being shown in Table 1) is:
Table 1
Analysis method is LC liquid chromatography, liquid-phase chromatographic analysis condition:
A) instrument: Agilent 1200
B) chromatographic column: Ultimate XB-C18 liquid-phase chromatographic column i.e. column diameter 3mm of 3mm*100mm3.0 μm,
Length 100mm, particle diameter 3.0 μm.
C) column temperature: 30 DEG C
D) flow velocity: 0.3mL/min
E) flowing phase: methanol-water gradient elution, the volume ratio of 0-5min first alcohol and water is 4:6；5-8min first alcohol and water
Volume ratio is 3:7；The volume ratio of 8-15min first alcohol and water is 25:75；The volume ratio of 15-25min first alcohol and water is 2:8；
Above-mentioned volume ratio is the volume ratio under the conditions of 20 DEG C；
F) detection wavelength: 254nm
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 Radix Saposhnikoviae, Radix Saposhnikoviae is 4 batches, batch
Number be respectively 20141201,151001,150929,1511016；
Concrete test result see table 2；
Table 2
The above-described presently preferred embodiments of the present invention that is only, all made in the range of the spirit and principles in the present invention any repair
Change, equivalent and improvement etc., should be included within the scope of the present invention.
Claims (3)
1. the method extracting cimicifugoside in Radix Saposhnikoviae, cimifugin, sec-o-glucosylhamaudol and 5-O-methyl-visamminol,
It is characterized in that, comprise the following steps:
Step 1: after Radix Saposhnikoviae is pulverized, sieve；
Step 2: weigh 0.25 weight portion Radix Saposhnikoviae powder, mixs homogeneously stand-by with 0.3 weight portion kieselguhr；
Step 3: the mixture in S12 is moved in the abstraction pool putting filter membrane in advance well, add appropriate kieselguhr to reaching
Chi Kou to abstraction pool；The lid covering abstraction pool carries out static extracting；Extraction is extracted liquid after terminating；
Extraction conditions is: extractant be volume ratio be methanol and the mixed solution of ethanol of 9:1；Extraction temperature 110 DEG C；
Static extracting time 7min；Flush volume 100%；Quiet cycle number of times 3 times.
In extraction Radix Saposhnikoviae the most according to claim 1, cimicifugoside, cimifugin, sec-o-glucosylhamaudol and 5-O-methyl tie up this
The method of ammiol glycosides, it is characterised in that the volume of described abstraction pool is 5ml, the pressure of described static extracting is
1500psi, the purge time of described static extracting is 100s.
In extraction Radix Saposhnikoviae the most according to claim 1, cimicifugoside, cimifugin, sec-o-glucosylhamaudol and 5-O-methyl tie up this
The method of ammiol glycosides, it is characterised in that the instrument that described ASE extraction is used is ASE350 Accelerate solvent extraction
Instrument.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610254653.1A CN105929089A (en) | 2016-04-22 | 2016-04-22 | Method for extracting cimicifugoside, cimicifugin, sec-o-glucosylhamaudol and 5-O-methylvisammioside in divaricate saposhnikovia root |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610254653.1A CN105929089A (en) | 2016-04-22 | 2016-04-22 | Method for extracting cimicifugoside, cimicifugin, sec-o-glucosylhamaudol and 5-O-methylvisammioside in divaricate saposhnikovia root |
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| CN105929089A true CN105929089A (en) | 2016-09-07 |
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| CN201610254653.1A Pending CN105929089A (en) | 2016-04-22 | 2016-04-22 | Method for extracting cimicifugoside, cimicifugin, sec-o-glucosylhamaudol and 5-O-methylvisammioside in divaricate saposhnikovia root |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109932453A (en) * | 2019-04-10 | 2019-06-25 | 康美（北京）药物研究院有限公司 | A kind of detection method of radix saposhnikoviae |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1895408A (en) * | 2006-06-27 | 2007-01-17 | 天津中新药业集团股份有限公司达仁堂制药厂 | Radix saposhnikoviae Tong Sheng capsules, preparation and quality control thereof |
-
2016
- 2016-04-22 CN CN201610254653.1A patent/CN105929089A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1895408A (en) * | 2006-06-27 | 2007-01-17 | 天津中新药业集团股份有限公司达仁堂制药厂 | Radix saposhnikoviae Tong Sheng capsules, preparation and quality control thereof |
Non-Patent Citations (2)
| Title |
|---|
| WEI LI等: "Pressurized liquid extraction followed by LC-ESI/MS for analysis of four chromones in Radix Saposhnikoviae", 《J. SEP. SCI.》 * |
| 宗晓菲等: "药用植物防风中色原酮类成分的提取", 《贵州农业科学》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109932453A (en) * | 2019-04-10 | 2019-06-25 | 康美（北京）药物研究院有限公司 | A kind of detection method of radix saposhnikoviae |
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