CN105954377A - Extraction method for amentoflavone in Selaginella tamariscina - Google Patents
Extraction method for amentoflavone in Selaginella tamariscina Download PDFInfo
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- CN105954377A CN105954377A CN201610254519.1A CN201610254519A CN105954377A CN 105954377 A CN105954377 A CN 105954377A CN 201610254519 A CN201610254519 A CN 201610254519A CN 105954377 A CN105954377 A CN 105954377A
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- amentoflavone
- herba selaginellae
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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
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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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- Chemical & Material Sciences (AREA)
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- General Physics & Mathematics (AREA)
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Abstract
The invention discloses an extraction method for amentoflavone in Selaginella tamariscina. The method comprises the following steps: step 1, crushing Selaginella tamariscina and then sieving the crushed Selaginella tamariscina; step 2, weighing 0.2 part by weight of Selaginella tamariscina powder, uniformly mixing the Selaginella tamariscina powder with 1 part by weight of diatomite and standing the obtained mixture for subsequent usage; and step 3, adding a proper amount of the mixture obtained in the step 2 into an extraction pool equipped with a filtering membrane in advance until the diatomite 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 methanol is used as an extraction solvent, extraction temperature is 110 DEG C, static extraction time is 5 min, a flushing volume is 80%, and three static cycles are carried out. The extraction method for amentoflavone in Selaginella tamariscina is simple to operate and short in consumed time and lowers requirements on operation skills of the skilled.
Description
Technical field
The present invention relates to test in laboratory field, the extracting method of amentoflavone in a kind of Herba Selaginellae.
Background technology
Pharmacopeia in 2010 have recorded the method for amentoflavone in Herba Selaginellae of extracting: takes this product powder (crossing No. three sieves) about 0.2g, essence
Close weighed, put in tool plug conical flask, accurate addition methanol 50ml, weighed weight, it is heated to reflux 5 hours, lets cool, more weighed
Weight, supplies the weight of less loss, shakes up with methanol, filters, takes subsequent filtrate, to obtain final product.Chromatographic condition is: with octadecyl silicon
Alkane bonded silica gel is filler；With methanol as mobile phase A, with 0.1% phosphoric acid solution as Mobile phase B, by different proportion of mobile phase
Regulation carries out gradient elution；Detection wavelength is 330nm.Number of theoretical plate is calculated by amentoflavone peak should be not less than 3000.
The method operating process of pharmacopeia is complicated, and the operant skill of operator is required height, and detection speed is slow simultaneously, it is impossible to meet
The purpose of quickly detection in commercial Application.
Summary of the invention
It is an object of the invention to provide the extracting method of amentoflavone in a kind of Herba Selaginellae, the method is simple to operate, and extraction efficiency is high,
Detection speed is fast.
The technical scheme that the present invention provides is: the extracting method of amentoflavone in a kind of Herba Selaginellae, comprises the following steps:
Step 1: after Herba Selaginellae is pulverized, sieve；
Step 2: weigh 0.2 weight portion Herba Selaginellae powder, mix homogeneously stand-by with the kieselguhr of 1 weight portion；
Step 3: mixture step 2 obtained is put in the abstraction pool putting filter membrane in advance well, adds appropriate kieselguhr extremely
Reach the Chi Kou of abstraction pool；The lid covering abstraction pool carries out static extracting；Extraction is extracted liquid after terminating；
Extraction conditions is: extractant is methanol；Extraction temperature 110 DEG C；Static extracting time 5min；Flush volume 80%；
Quiet cycle number of times 3 times.
In above-mentioned Herba Selaginellae in the extracting method of amentoflavone, the volume of described abstraction pool is 5ml.
In above-mentioned Herba Selaginellae in the extracting method of amentoflavone, the pressure of described static extracting is 1500psi.
In above-mentioned Herba Selaginellae in the extracting method of amentoflavone, the purge time of described static extracting is 60s.
In above-mentioned Herba Selaginellae in the extracting method of amentoflavone, step 2 is particularly as follows: by extract at the bar of 15000r/min
Under part, centrifugal 3min, takes supernatant.
In above-mentioned Herba Selaginellae in the extracting method of amentoflavone, 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 the used time is short, and precision is high, effectively reduces the operant skill to technical staff
Requirement.
Accompanying drawing explanation
Fig. 1 is the test collection of illustrative plates of embodiment 1 and pharmacopeia record in the present invention；
Fig. 2 is the test collection of illustrative plates that the method using pharmacopeia to record in the present invention obtains.
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 Herba Selaginellae machine is pulverized, excessively No. three sieves, about 0.2g, accurately weighed, mix homogeneously with 1g kieselguhr, stand-by,
Being moved into put well in advance and add proper amount of silicon diatomaceous earth in the ASE5ml abstraction pool of filter membrane, shaking is allowed to Chi Kou same gently
On horizontal line, tighten abstraction pool upper cover.After extraction terminates, extract is shifted in 25ml volumetric flask, with methanol dilution to carving
Degree, under 15000r/min, centrifugal 3min, takes supernatant, enters HPLC and measures.
Extraction conditions (being shown in Table 1) is:
Table 1
| Abstraction pool volume (ml) | 5 |
| Extractant | Methanol |
| Pressure (psi) | 1500 |
| Temperature (DEG C) | 110 |
| The static extracting time (min) | 5 |
| Quiet cycle number of times | 3 |
| Flush volume (%) | 80 |
| Purge time (s) | 60 |
Analysis method is LC liquid chromatography, liquid-phase chromatographic analysis condition:
A) the double ternary liquid phase chromatograph (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 3um.
C) column temperature: 40 DEG C
D) flow velocity: 0.5mL/min
E) flowing phase: methanol-0.1% phosphoric acid (volume ratio 55:45, wherein 0.1% phosphoric acid be mass percent be the phosphoric acid of 0.1%
Aqueous solution)
F) detection wavelength: 330nm
Chromatography validation verification:
Take amentoflavone reference substance appropriate, accurately weighed, add methanol and make every 1ml solution containing 25ug, to obtain final product.
Take amentoflavone reference substance appropriate, accurately weighed, add methanol and make every 1ml solution containing 25 μ g, to obtain final product, so
Rear precision respectively draws this solution 0.1 μ l, 0.2 μ l, 0.5 μ l, 1 μ l, 2 μ l entrance LC mensuration, and surveys according to said method
Fixed, the results detailed in Table 2.Carry out linear regression with concentration (μ g/ml)-peak area, try to achieve regression equation: y=17.132x+
9.1974, R2=0.99998.Amentoflavone in the range of 2.7～53.9 μ g/ml in good linear relationship.
Table 2 linear test result
The repeatability checking of the extracting process of embodiment 1:
Take sample (lot number: the 1409122 Guangxi) 0.2g of identical lot number, totally 3 parts, accurately weighed, by ASE extracting method
Extracting need testing solution, sample size is 1 μ L, with above-mentioned chromatographic condition parallel test, records amentoflavone in sample
Content is shown in Table two, and 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 Herba Selaginellae, Herba Selaginellae is 4 batches, and lot number divides
It is not 1409122 (Guangxi), 141129 (Shandong), 20150701 (Hunan), 150301 (safe Rong)；
The ASE extracting process of embodiment 1 to using the equipment parallel testing twice of two set same sizes with a batch of Herba Selaginellae, point
Do not represent for ASE1 and ASE2.
In Fig. 1, label s is the collection of illustrative plates of the amentoflavone of pharmacopeia；
In Fig. 1, label T Herba Selaginellae is the collection of illustrative plates obtained according to the method for embodiment 1；
Fig. 2 is the collection of illustrative plates that the method recorded according to pharmacopeia obtains.
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 any amendment,
Equivalent and improvement etc., should be included within the scope of the present invention.
Claims (6)
1. the extracting method of amentoflavone in a Herba Selaginellae, it is characterised in that comprise the following steps:
Step 1: after Herba Selaginellae is pulverized, sieve；
Step 2: weigh 0.2 weight portion Herba Selaginellae powder, mix homogeneously stand-by with the kieselguhr of 1 weight portion；
Step 3: mixture step 2 obtained is put in the abstraction pool putting filter membrane in advance well, adds appropriate kieselguhr extremely
Reach the Chi Kou of abstraction pool；The lid covering abstraction pool carries out static extracting；Extraction is extracted liquid after terminating；
Extraction conditions is: extractant is methanol；Extraction temperature 110 DEG C；Static extracting time 5min；Flush volume 80%；
Quiet cycle number of times 3 times.
The extracting method of amentoflavone in Herba Selaginellae the most according to claim 2, it is characterised in that described abstraction pool
Volume is 5ml.
The extracting method of amentoflavone in Herba Selaginellae the most according to claim 2, it is characterised in that described static extracting
Pressure be 1500psi.
The extracting method of amentoflavone in Herba Selaginellae the most according to claim 2, it is characterised in that described static extracting
Purge time be 60s.
The extracting method of amentoflavone in Herba Selaginellae the most according to claim 1, it is characterised in that step 2 particularly as follows:
By extract centrifugal 3min under conditions of 15000r/min, take supernatant.
The extracting method of amentoflavone in Herba Selaginellae the most according to claim 1, it is characterised in that described ASE extraction
Following the example of used instrument is ASE350 Accelerate solvent extraction instrument.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106872611A (en) * | 2017-04-17 | 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 amentoflavone content in Selaginella tamariscina |
| 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 |
| CN106959346A (en) * | 2017-04-17 | 2017-07-18 | 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 Geniposidic acid and acteoside content in plantain seed |
| CN106955502A (en) * | 2017-04-17 | 2017-07-18 | 广西壮族自治区梧州食品药品检验所 | A kind of method of Geniposidic acid and acteoside in ASE methods extraction plantain seed |
| CN107014932A (en) * | 2017-03-20 | 2017-08-04 | 广西壮族自治区梧州食品药品检验所 | A kind of method that ASE HPLC determine the acteoside content in bigleafbeautyberry root or leaf |
| CN107045030A (en) * | 2017-04-17 | 2017-08-15 | 广西壮族自治区梧州食品药品检验所 | A kind of method of calycosin glucoside in ASE methods extraction Radix Astragali |
| CN107064386A (en) * | 2017-04-17 | 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 HPLC methods determine calycosin glucoside content in the Radix Astragali |
| CN107216301A (en) * | 2017-05-23 | 2017-09-29 | 芜湖欧标农业发展有限公司 | A kind of preparation method of efficient hinokiflavone |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107014932A (en) * | 2017-03-20 | 2017-08-04 | 广西壮族自治区梧州食品药品检验所 | A kind of method that ASE HPLC determine the acteoside content in bigleafbeautyberry root or leaf |
| CN106872611A (en) * | 2017-04-17 | 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 amentoflavone content in Selaginella tamariscina |
| 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 |
| CN106959346A (en) * | 2017-04-17 | 2017-07-18 | 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 Geniposidic acid and acteoside content in plantain seed |
| CN106955502A (en) * | 2017-04-17 | 2017-07-18 | 广西壮族自治区梧州食品药品检验所 | A kind of method of Geniposidic acid and acteoside in ASE methods extraction plantain seed |
| CN107045030A (en) * | 2017-04-17 | 2017-08-15 | 广西壮族自治区梧州食品药品检验所 | A kind of method of calycosin glucoside in ASE methods extraction Radix Astragali |
| CN107064386A (en) * | 2017-04-17 | 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 HPLC methods determine calycosin glucoside content in the Radix Astragali |
| CN107216301A (en) * | 2017-05-23 | 2017-09-29 | 芜湖欧标农业发展有限公司 | A kind of preparation method of efficient hinokiflavone |
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Application publication date: 20160921 |