CN105891380A - Method using ASE method to extract linarin in buddleja officinalis - Google Patents
Method using ASE method to extract linarin in buddleja officinalis Download PDFInfo
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- CN105891380A CN105891380A CN201610254587.8A CN201610254587A CN105891380A CN 105891380 A CN105891380 A CN 105891380A CN 201610254587 A CN201610254587 A CN 201610254587A CN 105891380 A CN105891380 A CN 105891380A
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- linarin
- ase
- flos buddlejae
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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
- 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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- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
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- Medicines Containing Plant Substances (AREA)
Abstract
The invention discloses a method using an ASE method to extract linarin in buddleja officinalis. The method includes the steps of firstly, crushing the buddleja officinalis, and sieving; secondly, weighing 0.5 part of buddleja officinalis powder, and evenly mixing with 0.5 part of diatomite for standby; thirdly, adding an appropriate amount of diatomite into an extraction tank with a preset filter membrane until the diatomite reaches the opening of the extraction tank, and covering the extraction tank; fourthly, performing ester removing on the mixture in the extraction tank; fifthly, extracting the mixture in the extraction tank after the fourth step to obtain extract. The method 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 linarin in Flos Buddlejae.
Background technology
Within 2015, pharmacopeia have recorded the method for linarin in Flos Buddlejae of extracting: takes this product coarse powder about 0.5g, accurately weighed, puts Soxhlet
In extractor, adding petroleum ether (60～90 DEG C) 100ml, be heated to reflux 2 hours, discard petroleum ether, medicinal residues volatilize, then add methanol
100ml continues to be heated to reflux 4 hours, and extracting solution is put in evaporating dish, is concentrated into appropriate, is transferred in 50ml measuring bottle, residue and
Container washs with a small amount of methanol, and washing liquid is incorporated in same measuring bottle. and add methanol to scale, shake up, filter, take subsequent filtrate, to obtain final product.
The parameter of its liquid chromatograph is: with octadecylsilane chemically bonded silica as filler；With methanol-0.1% glacial acetic acid (48:52)
For flowing phase；Detection wavelength is 326nm.
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 linarin in Flos Buddlejae, the method is simple to operate, extracts
Time is short, and extraction accuracy is high.
The technical scheme that the present invention provides is: a kind of ASE method extracts the method for linarin in Flos Buddlejae, comprises the following steps:
Step 1: after Flos Buddlejae is pulverized, sieve；
Step 2: weigh 0.5 weight portion Flos Buddlejae powder, mix homogeneously stand-by with 0.5 weight portion kieselguhr；
Step 3: in the abstraction pool putting filter membrane in advance well, adds appropriate kieselguhr to the Chi Kou reaching abstraction pool；Cover
The lid of abstraction pool；
Step 4: the mixture in abstraction pool is removed ester；
The ester condition is gone to be: extractant is normal hexane；Extraction temperature 80 DEG C；Static extracting time 7min；Flush volume 100%；
Quiet cycle number of times 1 time.
Step 5: after step 4 terminates, the mixture in abstraction pool is extracted；Extraction is extracted liquid after terminating；
Extraction conditions is: extractant is methanol；Extraction temperature 100 DEG C；Static extracting time 5min；Flush volume 60%；
Quiet cycle number of times 2 times.
In above-mentioned ASE method extracts Flos Buddlejae in the method for linarin, the volume of described abstraction pool is 10ml.
In above-mentioned ASE method extracts Flos Buddlejae in the method for linarin, the static extracting of described step 4 and step 5
Pressure is 1500psi.
In above-mentioned ASE method extracts Flos Buddlejae in the method for linarin, the purge time of described step 4 is 200s,
The purge time of step 5 is 60s.
In above-mentioned ASE method extracts Flos Buddlejae in the method for linarin, also including step 6, step 6 will be particularly as follows: will extract
Take liquid centrifugal 3min under conditions of 15000r/min, take supernatant.
In above-mentioned ASE method extracts Flos Buddlejae in the method for linarin, 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 method of the present invention is simple to operate, and extraction time is short, and extraction accuracy is high.
Accompanying drawing explanation
Fig. 1 is the rectangular plots of the chromatography 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 the present invention
Any restriction.
Embodiment 1:
Size-reduced for Flos Buddlejae machine is pulverized, excessively No. three sieves, about 0.5g, accurately weighed, mix homogeneously with 0.5g kieselguhr, stand-by,
It is moved into and puts filter membrane in advance wellAdding proper amount of silicon diatomaceous earth in 10ml abstraction pool, shaking is allowed to Chi Kou same gently
On one horizontal line, tighten abstraction pool upper cover.After extraction terminates, extract is shifted in 50ml volumetric flask, with methanol dilution extremely
Scale, under 15000r/min, centrifugal 5min, takes supernatant, enters LC and measures.
Extraction conditions (being shown in Table 1) is:
Table 1
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: methanol-0.1% acetic acid, specifically, methanol and mass percent are 0.1% acetum volume ratio 48:
52, this volume ratio is the volume ratio under the conditions of 20 DEG C；
F) detection wavelength: 326nm；
Chromatography validation verification:
Take linarin reference substance appropriate, accurately weighed, add methanol and make every 1ml solution containing 0.1mg, to obtain final product.
Take linarin reference substance solution (concentration: 0.1321mg/ml), respectively precision draw this solution 0.5 μ l, 1 μ l, 2 μ l,
4 μ l, 5 μ l enter LC and measure, and measure according to said method, the results detailed in Table 2；Accompanying drawing 1 is corresponding with table 2, accompanying drawing 1
Abscissa represents absolute sample size, and vertical coordinate represents peak area.
Table 2
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 Flos Buddlejae, Flos Buddlejae is 4 batches, batch
Number be respectively 1508090,151118,20150701,141201；
The ASE extracting process of embodiment 1 is to a batch of Flos Buddlejae parallel testing twice, respectively ASE1 and ASE2 table
Show.
Concrete test result see table 3；
Table 3
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 any 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 linarin in Flos Buddlejae, it is characterised in that comprise the following steps:
Step 1: after Flos Buddlejae is pulverized, sieve；
Step 2: weigh 0.5 weight portion Flos Buddlejae powder, mix homogeneously stand-by with 0.5 weight portion kieselguhr；
Step 3: in the abstraction pool putting filter membrane in advance well, adds appropriate kieselguhr to the Chi Kou reaching abstraction pool；Cover
The lid of abstraction pool；
Step 4: the mixture in abstraction pool is removed ester；
The ester condition is gone to be: extractant is normal hexane；Extraction temperature 80 DEG C；Static extracting time 7min；Flush volume 100%；
Quiet cycle number of times 1 time.
Step 5: after step 4 terminates, the mixture in abstraction pool is extracted；Extraction is extracted liquid after terminating；
Extraction conditions is: extractant is methanol；Extraction temperature 100 DEG C；Static extracting time 5min；Flush volume 60%；
Quiet cycle number of times 2 times.
ASE method the most according to claim 1 extracts the method for linarin in Flos Buddlejae, it is characterised in that described
The volume of abstraction pool is 10ml.
ASE method the most according to claim 1 extracts the method for linarin in Flos Buddlejae, it is characterised in that described
The pressure of the static extracting of step 4 and step 5 is 1500psi.
ASE method the most according to claim 1 extracts the method for linarin in Flos Buddlejae, it is characterised in that described
The purge time of step 4 is 200s, and the purge time of step 5 is 60s.
ASE method the most according to claim 1 extracts the method for linarin in Flos Buddlejae, it is characterised in that also include
Step 6, step 6 is particularly as follows: by extract centrifugal 3min under conditions of 15000r/min, take supernatant.
ASE method the most according to claim 1 extracts the method for linarin in Flos Buddlejae, it is characterised in that described
The instrument that ASE extraction is used is ASE350 Accelerate solvent extraction instrument.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610254587.8A CN105891380A (en) | 2016-04-22 | 2016-04-22 | Method using ASE method to extract linarin in buddleja officinalis |
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| CN201610254587.8A CN105891380A (en) | 2016-04-22 | 2016-04-22 | Method using ASE method to extract linarin in buddleja officinalis |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106924991A (en) * | 2017-04-17 | 2017-07-07 | 广西壮族自治区梧州食品药品检验所 | A kind of method of recinine in ASE methods extraction castor bean |
| CN107014922A (en) * | 2017-04-17 | 2017-08-04 | 广西壮族自治区梧州食品药品检验所 | A kind of ASE HPLC methods determine the method that mist spends middle Determination of Linarin |
| CN107064384A (en) * | 2017-04-11 | 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 methods extract spinosin in spina date seed |
| CN111393490A (en) * | 2020-03-31 | 2020-07-10 | 右江民族医学院 | Method for extracting linarin from buddleja officinalis |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107064384A (en) * | 2017-04-11 | 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 methods extract spinosin in spina date seed |
| CN106924991A (en) * | 2017-04-17 | 2017-07-07 | 广西壮族自治区梧州食品药品检验所 | A kind of method of recinine in ASE methods extraction castor bean |
| CN107014922A (en) * | 2017-04-17 | 2017-08-04 | 广西壮族自治区梧州食品药品检验所 | A kind of ASE HPLC methods determine the method that mist spends middle Determination of Linarin |
| CN111393490A (en) * | 2020-03-31 | 2020-07-10 | 右江民族医学院 | Method for extracting linarin from buddleja officinalis |
| CN111393490B (en) * | 2020-03-31 | 2023-05-30 | 右江民族医学院 | Method for extracting linarin from buddleja officinalis |
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Application publication date: 20160824 |