CN104876988A - Method for extracting linarin from wild chrysanthemum flower - Google Patents
Method for extracting linarin from wild chrysanthemum flower Download PDFInfo
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- CN104876988A CN104876988A CN201510243008.5A CN201510243008A CN104876988A CN 104876988 A CN104876988 A CN 104876988A CN 201510243008 A CN201510243008 A CN 201510243008A CN 104876988 A CN104876988 A CN 104876988A
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- wild chrysanthemum
- linarin
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Abstract
The invention discloses a method for extracting linarin from wild chrysanthemum flower, which comprises the following steps: 1. pulverizing wild chrysanthemum flower, passing through a 50-mesh screen, and mixing with diatomite; 2. extracting linarin by ASE (accelerated solvent extraction), and collecting the extracting solution, wherein the extraction solvent adopted by the ASE is methanol; and 3. carrying out centrifugal separation on the extracting solution to obtain the linarin-containing supernate. The method has the advantages of high extraction speed and high precision.
Description
Technical field
The present invention relates to technical field of chemical detection, particularly a kind of method extracting linarin from Wild Chrysanthemum.
Background technology
This product is the dry capitulum of feverfew mother chrysanthemum ChrysanthemumindicumL..Autumn, to pluck when spending in season in winter two just open, dry, or dry after steaming.This product is that class is spherical, diameter 0.3 ~ 1cm, brown color.Involucre is made up of 4 ~ 5 layers of bract, the avette or bar shaped of outer bract, greyish-green or light brown in the middle part of outside surface, usually by white hair, and edge film quality; Internal layer bract oblong, film quality, outside surface is without hair.Residual total bennet that involucre base portion has.Ligulate flower 1 is taken turns, and yellow to brown color, shrinkage is curling; Tubiform floret is most, deep yellow.Body is light.Gas fragrance, bitter.The extracting method recorded in pharmacopeia is: this product powder (crossing No. three sieves) about 0.25g is got in the preparation of need testing solution.Accurately weighed, put in tool plug Erlenmeyer flask, precision adds methyl alcohol 100ml, weighed weight, and reflux 3 hours, lets cool, more weighed weight, supplies the weight of less loss, shake up with methyl alcohol, filters, gets subsequent filtrate, to obtain final product.The above-mentioned method duration extracting linarin from Wild Chrysanthemum, requires high to operator.
Summary of the invention
The object of this invention is to provide a kind ofly to extract rapidly, the method extracting linarin from Wild Chrysanthemum that precision is high.
Technical scheme provided by the invention is: a kind of method extracting linarin from Wild Chrysanthemum, comprises the following steps:
Step 1: Wild Chrysanthemum is pulverized and cross No. three sieve after mix with diatomite;
Step 2: adopt ASE extraction process extraction linarin, collect extraction liquid, wherein, the extraction solvent that ASE extraction process adopts is methyl alcohol;
Step 3: extraction liquid is carried out the supernatant liquor that centrifugation obtains containing linarin.
Extract in the method for linarin from Wild Chrysanthemum above-mentioned, in described step 1, Wild Chrysanthemum and diatomaceous weight ratio are 1:1.
Extract in the method for linarin from Wild Chrysanthemum above-mentioned, described step 2 comprises following sub-step:
S1: open filter paper at the bottom pad 3-6 of abstraction pool, then add diatomite as bottom;
S2: add Wild Chrysanthemum and diatomaceous mixture that step 1 obtains in abstraction pool;
S3: add appropriate diatomite as top layer in abstraction pool;
S4: adopt methyl alcohol to extract; Wherein, extraction parameters is: extraction temperature 100 DEG C; Cycle index 2 times; Static extracting time 10min; Flush volume 100%; Purge time 60s.
Extract in the method for linarin from Wild Chrysanthemum above-mentioned, the weight of described Wild Chrysanthemum and diatomaceous mixture is 0.5g, and the volume of described abstraction pool is 10ml.
Extract in the method for linarin from Wild Chrysanthemum above-mentioned, described step 3 is specially: extraction liquid is placed in 100ml volumetric flask, with methanol dilution to scale, shakes up and get final product, and gets 2mL centrifugal 5min under 15000r/min, gets supernatant liquor.
The present invention is after employing technique scheme, and its beneficial effect had is:
Adopt ASE extraction process when methyl alcohol is as extraction agent, effectively can improve effect of extracting, improve extraction precision, reduce extraction time and solvent load, avoid the defect that the long solvent load of official method extraction time is large.
Accompanying drawing explanation
Fig. 1 is the test spectrogram of embodiments of the invention 1;
Fig. 2 is the test spectrogram of standard of the present invention;
Fig. 3 is the present invention is separated the sample obtained test spectrogram according to official method.
Embodiment
Below in conjunction with embodiment, technical scheme of the present invention is described in further detail, but does not form any limitation of the invention.
Embodiment 1:
Instrument used by the present embodiment and consumptive material are: pulverizer, electronic analytical balance (XA205DU): sensibility reciprocal 0.001g, accelerated solvent extraction model: ASE-350 (10ml abstraction pool, 50ml receiving flask), volumetric flask: 100ml, centrifuge tube: 2ml.
Step 1: get Wild Chrysanthemum powder (crossing No. three sieves) about 0.25g, accurately weighed, mix with 0.25g diatomite, stand-by;
Step 2: pad 3 ~ 6 (commercialization filter paper 1) self-control circular filter paper (diameter 27mm) bottom abstraction pool, add the sample mixed that step 1 obtains after adding about 1g diatomite, add appropriate diatomite again, gently jolting make it with Chi Kou in the same horizontal line, tighten abstraction pool upper cover.
Step 3:ASE extracts, and extraction parameters is as following table 1
Table 1 ASE extraction parameters
Step 4: after extraction terminates, extraction liquid is placed in 100ml volumetric flask, with methanol dilution to scale, shakes up and get final product.Get 2mL centrifugal 5min under 15000r/min, get supernatant liquor.
The preparation of standard
Get linarin reference substance appropriate, accurately weighed, add dissolve with methanol and make the solution of every 1ml containing 25 μ g, to obtain final product.
Detect
Adopt Shimadzu 2010 liquid chromatograph to detect, detect parameters is:
Chromatographic column: BDS HYPERSIL C18 2.4um 4.6 × 100mm, column temperature: 40 DEG C, flow velocity: 0.6mL/min, moving phase: methyl alcohol-0.5% Glacial acetic acid (39:61), determined wavelength: 334nm, sample size 10 μ l.
Following Fig. 1 and Fig. 2 of detected result of embodiment 1 and standard.Fig. 3 records by pharmacopeia separation method and detects the spectrogram obtained, and is specially: the preparation of need testing solution: get Wild Chrysanthemum powder (crossing No. three sieves) about 0.25g.Accurately weighed, put in tool plug Erlenmeyer flask, precision adds methyl alcohol 100ml, weighed weight, and reflux 3 hours, lets cool, more weighed weight, supplies the weight of less loss, shake up with methyl alcohol, filters, gets subsequent filtrate, to obtain final product.Can be found by three spectrogram contrasts, the sample of present method resulting separation can obtain collection of illustrative plates complete clearly, and the sample test spectrogram obtained with the separation method of pharmacopeia record has height repeatability.
Present method separation accuracy is high, and the used time is short, is conducive to the operation of Simplified analysis personnel.
Above-describedly be only preferred embodiment of the present invention, all do within the scope of the spirit and principles in the present invention any amendment, equivalently to replace and improvement etc., all should be included within protection scope of the present invention.
Claims (3)
1. from Wild Chrysanthemum, extract a method for linarin, it is characterized in that, comprise the following steps:
Step 1: Wild Chrysanthemum is pulverized and cross No. three sieve after mix with diatomite;
Step 2: adopt ASE extraction process extraction linarin, collect extraction liquid, wherein, the extraction solvent that ASE extraction process adopts is methyl alcohol;
Step 3: extraction liquid is carried out the supernatant liquor that centrifugation obtains containing linarin;
In described step 1, Wild Chrysanthemum and diatomaceous weight ratio are 1:1.
Described step 2 comprises following sub-step:
S1: open filter paper at the bottom pad 3-6 of abstraction pool, then add diatomite as bottom;
S2: add Wild Chrysanthemum and diatomaceous mixture that step 1 obtains in abstraction pool;
S3: add appropriate diatomite as top layer in abstraction pool;
S4: adopt methyl alcohol to extract; Wherein, extraction parameters is: extraction temperature 100 DEG C; Cycle index 2 times; Static extracting time 10min; Flush volume 100%; Purge time 60s.
2. the method extracting linarin from Wild Chrysanthemum according to claim 1, is characterized in that, the weight of described Wild Chrysanthemum and diatomaceous mixture is 0.5g, and the volume of described abstraction pool is 10ml.
3., according to the arbitrary described method extracting linarin from Wild Chrysanthemum of claim 1 to 2, it is characterized in that, described step 3 is specially: extraction liquid is placed in 100ml volumetric flask, with methanol dilution to scale, shake up and get final product, get 2mL centrifugal 5min under 15000r/min, get supernatant liquor.
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| CN201510243008.5A CN104876988A (en) | 2015-05-12 | 2015-05-12 | Method for extracting linarin from wild chrysanthemum flower |
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| CN201510243008.5A CN104876988A (en) | 2015-05-12 | 2015-05-12 | Method for extracting linarin from wild chrysanthemum flower |
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105687675A (en) * | 2016-04-15 | 2016-06-22 | 广西壮族自治区梧州食品药品检验所 | Method for extracting peimine and peiminine from Fritillaria thunbergii |
| CN105820051A (en) * | 2016-04-27 | 2016-08-03 | 广西壮族自治区梧州食品药品检验所 | Static extraction method for chlorogenic acid in wild chrysanthemum |
| CN105878334A (en) * | 2016-04-25 | 2016-08-24 | 广西壮族自治区梧州食品药品检验所 | Method for rapidly extracting flavonoid glycoside from momordica grosvenori tea |
| CN105891380A (en) * | 2016-04-22 | 2016-08-24 | 广西壮族自治区梧州食品药品检验所 | Method using ASE method to extract linarin in buddleja officinalis |
| CN105924489A (en) * | 2016-04-26 | 2016-09-07 | 广西壮族自治区梧州食品药品检验所 | Method for extracting platycodin in Radix Platycodonis through ASE |
| CN105954380A (en) * | 2016-04-22 | 2016-09-21 | 广西壮族自治区梧州食品药品检验所 | Determination method for linarin in Buddleja officinalis |
| CN105954405A (en) * | 2016-04-27 | 2016-09-21 | 广西壮族自治区梧州食品药品检验所 | Method for determination of pectolinarin in buddleja officinalis |
| CN105954406A (en) * | 2016-04-27 | 2016-09-21 | 广西壮族自治区梧州食品药品检验所 | Method for extracting pectolinarin in buddleja officinalis |
| CN106872609A (en) * | 2017-04-13 | 2017-06-20 | 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 Determination of content of linarin in Flos Chrysanthemi Indici |
| CN106918665A (en) * | 2017-04-11 | 2017-07-04 | 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 magnelin content in the flower bud of lily magnolia |
| 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 |
| CN106924990A (en) * | 2017-04-11 | 2017-07-07 | 广西壮族自治区梧州食品药品检验所 | A kind of method of magnelin in ASE methods extraction flower bud of lily magnolia |
| 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 |
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105687675A (en) * | 2016-04-15 | 2016-06-22 | 广西壮族自治区梧州食品药品检验所 | Method for extracting peimine and peiminine from Fritillaria thunbergii |
| CN105954380A (en) * | 2016-04-22 | 2016-09-21 | 广西壮族自治区梧州食品药品检验所 | Determination method for linarin in Buddleja officinalis |
| CN105891380A (en) * | 2016-04-22 | 2016-08-24 | 广西壮族自治区梧州食品药品检验所 | Method using ASE method to extract linarin in buddleja officinalis |
| CN105878334A (en) * | 2016-04-25 | 2016-08-24 | 广西壮族自治区梧州食品药品检验所 | Method for rapidly extracting flavonoid glycoside from momordica grosvenori tea |
| CN105924489A (en) * | 2016-04-26 | 2016-09-07 | 广西壮族自治区梧州食品药品检验所 | Method for extracting platycodin in Radix Platycodonis through ASE |
| CN105954405A (en) * | 2016-04-27 | 2016-09-21 | 广西壮族自治区梧州食品药品检验所 | Method for determination of pectolinarin in buddleja officinalis |
| CN105820051A (en) * | 2016-04-27 | 2016-08-03 | 广西壮族自治区梧州食品药品检验所 | Static extraction method for chlorogenic acid in wild chrysanthemum |
| CN105954406A (en) * | 2016-04-27 | 2016-09-21 | 广西壮族自治区梧州食品药品检验所 | Method for extracting pectolinarin in buddleja officinalis |
| CN106918665A (en) * | 2017-04-11 | 2017-07-04 | 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 magnelin content in the flower bud of lily magnolia |
| CN106924990A (en) * | 2017-04-11 | 2017-07-07 | 广西壮族自治区梧州食品药品检验所 | A kind of method of magnelin in ASE methods extraction flower bud of lily magnolia |
| 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 |
| CN106872609A (en) * | 2017-04-13 | 2017-06-20 | 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 Determination of content of linarin in Flos Chrysanthemi Indici |
| 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 |
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Application publication date: 20150902 |