CN105891381A - Method using ASE to extract amygdalin in semen persicae - Google Patents
Method using ASE to extract amygdalin in semen persicae Download PDFInfo
- Publication number
- CN105891381A CN105891381A CN201610255699.5A CN201610255699A CN105891381A CN 105891381 A CN105891381 A CN 105891381A CN 201610255699 A CN201610255699 A CN 201610255699A CN 105891381 A CN105891381 A CN 105891381A
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- CN
- China
- Prior art keywords
- ase
- amygdalin
- semen persicae
- extraction
- extracts
- 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.)
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Classifications
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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
-
- 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 a method using ASE to extract amygdalin in semen persicae. The method includes the steps of firstly, crushing the semen persicae, and sieving; secondly, weighing 0.3 part of semen persicae powder, and evenly mixing with 1 part of quartz sand for standby; thirdly, adding an appropriate amount of quartz sand into an extraction tank with a preset filter membrane until the quartz sand 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 extracts the method for Amygdalin in Semen Persicae.
Background technology
Pharmacopeia in 2015 have recorded the method extracting Amygdalin in Semen Persicae: takes this product meal about 0.3g, accurately weighed, puts tool plug
In conical flask, add petroleum ether (60～90 DEG C) 50ml, be heated to reflux 1 hour, let cool, filter, discard petroleum ether liquid, the dregs of a decoction
And filter paper volatilizes solvent, put in former conical flask, accurate addition 70% methyl alcohol 50ml, weighed weight, it is heated to reflux 1 hour,
Let cool, more weighed weight, supply the weight of less loss with 70% methyl alcohol, shake up, filter.Precision measures subsequent filtrate 5ml, puts 10ml
In measuring bottle, add 50% methyl alcohol to scale, shake up, to obtain final product.Under 15000r/min, centrifugal 3min, takes supernatant, enters LC
Measure.
The parameter of its liquid chromatogram is: with octadecylsilane chemically bonded silica as filler；With methanol-water (20:80) for flowing
Phase；Detection wavelength is 210nm.
The method operating process of pharmacopeia is complicated, and the operative skill of operating personnel is required height.
Summary of the invention
It is an object of the invention to provide a kind of method that ASE extracts Amygdalin in Semen Persicae, the method is simple to operate, extracts degree
Height, the operating time is short.
The technical scheme that the present invention provides is: a kind of ASE extracts the method for Amygdalin in Semen Persicae, comprises the following steps:
Step 1: after peach kernel is pulverized, sieve；
Step 2: weigh 0.3 weight portion peach kernel powder, mixes stand-by with 1 weight portion quartz sand；
Step 3: in the abstraction pool putting filter membrane in advance well, adds appropriate quartz sand 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 n-hexane；Extraction temperature 80 DEG C；Static extracting time 5min；Flush volume 60%；
Quiet cycle number of times 2 times.
Step 5: after step 4 terminates, the mixture in abstraction pool is extracted；Extraction is extracted liquid after terminating；
Extraction conditions is: extractant is 70% methyl alcohol；Extraction temperature 100 DEG C；Static extracting time 5min；Flush volume 100%；
Quiet cycle number of times 1 time；The described percentage by volume that 70% methyl alcohol is methyl alcohol is 70%.
In above-mentioned ASE extracts the method for Amygdalin in Semen Persicae, the volume of described abstraction pool is 5ml.
In above-mentioned ASE extracts the method for Amygdalin in Semen Persicae, the pressure of the static extracting of described step 4 and step 5
It is 1500psi.
In above-mentioned ASE extracts the method for Amygdalin in Semen Persicae, the purge time of described step 4 and step 5 is 90s.
In above-mentioned ASE extracts the method for Amygdalin in Semen Persicae, also including step 6, step 6 is particularly as follows: by extract
Under conditions of 15000r/min, centrifugal 3min, takes supernatant.
In above-mentioned ASE extracts the method for Amygdalin in Semen Persicae, 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 extraction degree is high, and the operating time is short.
Accompanying drawing explanation
Fig. 1 is that the present invention uses official method to test the chromatogram obtained；
Fig. 2 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 does not constitute the present invention
Any restriction.
Embodiment 1:
Size-reduced for peach kernel machine is pulverized, excessively No. three sieves, about 0.3g, accurately weighed, mix with 1g quartz sand, stand-by,
It is moved into and put glass fiber filter in advance well5ml 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
70% 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
70% methyl alcohol refers to the percentage by volume of methyl alcohol in the methanol aqueous solution under the conditions of 20 DEG C.
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-water (volume ratio 20:80)；
F) detection wavelength: 210nm；
The reappearance checking of the extracting process of embodiment 1:
Take sample (lot number: the 20150801) 0.3g of identical lot number, totally 4 parts, accurately weighed, extract by ASE extracting method
Need testing solution, sample size is 1 μ L, with above-mentioned chromatographic condition parallel test, records the content of amarogentin in sample and is shown in Table
Two, RSD are 1.9%, and test shows that ASE extracting method repeatability is good, the results detailed in Table 2
Table 2
The accuracy test of the extracting process of 1.2 embodiments 1
Using the ASE extracting process of embodiment 1 and the extracting process of pharmacopeia to extract peach kernel, peach kernel is 3 batches, and lot number divides
It is not 20150801,150701,1511028；
The ASE extracting process of embodiment 1 is to a batch of peach kernel parallel testing twice, and respectively ASE1 and ASE2 represents.
Fig. 1 is the chromatogram that sample 20150801 obtains according to the method described in pharmacopeia；
Fig. 2 is that sample 20150801 obtains according to ASE extracting process and LC liquid chromatography test (ASE2) of the present invention
Chromatogram.
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. the method that an ASE extracts Amygdalin in Semen Persicae, it is characterised in that comprise the following steps:
Step 1: after peach kernel is pulverized, sieve；
Step 2: weigh 0.3 weight portion peach kernel powder, mixes stand-by with 1 weight portion quartz sand；
Step 3: in the abstraction pool putting filter membrane in advance well, adds appropriate quartz sand 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 n-hexane；Extraction temperature 80 DEG C；Static extracting time 5min；Flush volume 60%；
Quiet cycle number of times 2 times.
Step 5: after step 4 terminates, the mixture in abstraction pool is extracted；Extraction is extracted liquid after terminating；
Extraction conditions is: extractant is 70% methyl alcohol；Extraction temperature 100 DEG C；Static extracting time 5min；Flush volume 100%；
Quiet cycle number of times 1 time；The described percentage by volume that 70% methyl alcohol is methyl alcohol is 70%.
ASE the most according to claim 1 extracts the method for Amygdalin in Semen Persicae, it is characterised in that described extraction
The volume in pond is 5ml.
ASE the most according to claim 1 extracts the method for Amygdalin in Semen Persicae, it is characterised in that described step 4
It is 1500psi with the pressure of the static extracting of step 5.
ASE the most according to claim 1 extracts the method for Amygdalin in Semen Persicae, it is characterised in that described step 4
It is 90s with the purge time of step 5.
ASE the most according to claim 1 extracts the method for Amygdalin in Semen Persicae, it is characterised in that also include step 6,
Described step 6 is particularly as follows: by extract centrifugal 3min under conditions of 15000r/min, take supernatant.
ASE the most according to claim 1 extracts the method for Amygdalin in Semen Persicae, 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 |
|---|---|---|---|
| CN201610255699.5A CN105891381A (en) | 2016-04-22 | 2016-04-22 | Method using ASE to extract amygdalin in semen persicae |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610255699.5A CN105891381A (en) | 2016-04-22 | 2016-04-22 | Method using ASE to extract amygdalin in semen persicae |
Publications (1)
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| CN105891381A true CN105891381A (en) | 2016-08-24 |
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ID=56704603
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| Application Number | Title | Priority Date | Filing Date |
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| CN201610255699.5A Pending CN105891381A (en) | 2016-04-22 | 2016-04-22 | Method using ASE to extract amygdalin in semen persicae |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2004014409A1 (en) * | 2002-08-12 | 2004-02-19 | Herb Valley | Developing method for separating d-amygdalin and neoamygdalin by reversed-phase hplc and optimum conditions for inhibition of racemization of amygdalin |
| CN104177455A (en) * | 2014-09-04 | 2014-12-03 | 南京标科生物科技有限公司 | Method for extracting amygdalin from bitter almond |
| CN104777249A (en) * | 2015-04-07 | 2015-07-15 | 湖北端正药业股份有限公司 | Method for determining content of effective ingredient amygdalin in loquat leaf cough syrup |
-
2016
- 2016-04-22 CN CN201610255699.5A patent/CN105891381A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2004014409A1 (en) * | 2002-08-12 | 2004-02-19 | Herb Valley | Developing method for separating d-amygdalin and neoamygdalin by reversed-phase hplc and optimum conditions for inhibition of racemization of amygdalin |
| CN104177455A (en) * | 2014-09-04 | 2014-12-03 | 南京标科生物科技有限公司 | Method for extracting amygdalin from bitter almond |
| CN104777249A (en) * | 2015-04-07 | 2015-07-15 | 湖北端正药业股份有限公司 | Method for determining content of effective ingredient amygdalin in loquat leaf cough syrup |
Non-Patent Citations (4)
| Title |
|---|
| A. RADOIČIĆ 等: "Development and Validation of a TLC-densitometric Method for the Ouantitatlve Determination of Amygdalin", 《8TH AEGEAN ANALYTICAL CHEMISTRY DAYS》 * |
| JIHYUN LEE 等: "Quantification of Amygdalin in Nonbitter,Semibitter,and Bitter Almonds (Prunusdulcis) by UHPLC-(ESI)QqQ MS/MS", 《JOURNAL OF AGRICULTURAL AND FOOD CHEMISTRY》 * |
| 国家药典委员会 编: "《中华人民共和国药典 2015年版 一部》", 30 June 2015 * |
| 钱平 等: "桃仁定性鉴别与含量测定研究", 《中国药事》 * |
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Application publication date: 20160824 |