CN106918662A - A kind of method that ASE-HPLC methods determine Content Measurement of Scutellarin in Sculellaria barbata - Google Patents
A kind of method that ASE-HPLC methods determine Content Measurement of Scutellarin in Sculellaria barbata Download PDFInfo
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- CN106918662A CN106918662A CN201710165725.XA CN201710165725A CN106918662A CN 106918662 A CN106918662 A CN 106918662A CN 201710165725 A CN201710165725 A CN 201710165725A CN 106918662 A CN106918662 A CN 106918662A
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- 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
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- G—PHYSICS
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- 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
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- G01N2030/062—Preparation extracting sample from raw material
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Abstract
The invention discloses a kind of method that ASE-HPLC methods determine Content Measurement of Scutellarin in Sculellaria barbata, belong to field of chemical detection.The method for aiming to provide the quality of a kind of easier, quick control Sculellaria barbata medicinal material and its granule, the method is using the Sculellaria barbata sample after ASE extraction crushing, wherein ASE extracting process includes first using petroleum ether extraction, then again with methanol extraction, collects methanol extraction liquid；The content of also scutelloside in methanol extraction liquid is determined using HPLC methods.The present invention can be used to control the quality of Sculellaria barbata medicinal material and its granule.
Description
Technical field
The invention belongs to Content Measurement of Scutellarin in field of chemical detection, especially a kind of ASE-HPLC methods measure Sculellaria barbata
Method.
Background technology
Sculellaria barbata dries herb for labiate Sculellaria barbata Scutellaria barbata D.Don's, taste is pungent, hardship,
It is cold.Return lung, liver and kidney channel.It is clearing heat and detoxicating, stagnation resolvation diuresis.Can be used for furuncle swelling toxin, abscess of throat, the pain of injury caused by falling and tumbling, oedema, jaundice,
Snake bite and insect sting.Clinic is used for the diseases such as treatment liver cancer, stomach cancer, lung cancer, and its principle active component is flavone compound.It is wild yellow
A kind of reed mentioned in ancient books glycosides is a kind of content active material higher in Sculellaria barbata,《Chinese Pharmacopoeia》(version one in 2015) is made with Content Measurement of Scutellarin
It is the important indicator of its quality evaluation, with cerebral vascular resistance is reduced, improves brain blood circulation, increases cerebral blood flow (CBF) and antiplatelet
The effect of aggegation, modern pharmacological research shows that scutellarin has significantly to tumour cell, hepatoma cell proliferation and invasive ability
Inhibitory action.At present, in Sculellaria barbata the extracting method of scutellarin have alcohol extracting circumfluence method, supercritical extraction, soxhlet extraction,
Ultrasonic extraction, macroporous resin purification method etc., assay method has ultraviolet spectrophotometry, high performance liquid chromatography, Capillary Electrophoresis
Method but above method pre-treatment extraction time is long, determination step is cumbersome.Compared with conventional method, the advantage that ASE is protruded is to shorten
Extraction time, solvent consumption is reduced, improve extraction efficiency.
The present invention determines the content of scutellarin in Sculellaria barbata using ASE-HPLC methods, and easy to operate, quick, result is accurate
Really.
The content of the invention
For above-mentioned deficiency, the present invention is intended to provide a kind of easier, quick control Sculellaria barbata medicinal material and its granule
Quality method, the method using ASE-HPLC methods determine Sculellaria barbata in scutellarin content.
In order to solve the above-mentioned technical problem, the technical scheme that the present invention is provided is such：A kind of ASE-HPLC methods are determined
The method of Content Measurement of Scutellarin, comprises the steps successively in Sculellaria barbata：
Step 1：Sculellaria barbata sample after being crushed using ASE extractions, wherein ASE extracting process include first being extracted with petroleum ether
Take, then again with methanol extraction, collect methanol extraction liquid；
Step 2：The content of also scutelloside in methanol extraction liquid is determined using HPLC methods.
Further, described step 1 includes following sub-steps：
Step S1：By Sculellaria barbata sample comminution, No. three sieves are crossed, take the powder 1g after sieving；
Step S2：Mix with the diatomite of 1g, loaded on being placed with the 10mlASE abstraction pools of fibrous filter membrane, plus diatomite is extremely
It is parallel with pond mouthful, use petroleum ether extraction；
Step S3：Petroleum ether extraction liquid is given up, adds methanol solution to carry out reextraction to the dregs of a decoction；
Step S4：Extract is collected, and adds methanol solution to be settled to 100ml, filtered, obtain methanol extraction liquid.
Further, the extraction described in step S2, parameter is as follows：Extraction temperature is 80 DEG C；Extraction time is 5min；Extraction
Number of times is 1 time；Flush volume is 100%；Purge time is 120s.
Further, the extraction described in step S3, parameter is as follows：Extraction temperature is 120 DEG C；Extraction time is 8min；Extraction
Number of times is taken for 3 times；Flush volume is 60%；Purge time is 60s.
Further, the detection parameter of the HPLC methods described in step 2 is：Chromatographic column is Thermo Syncronis C18；
Mobile phase is methanol-acetic acid-water；Flow velocity is 0.3mL/min；Detection wavelength is 335nm；Column temperature is 40 DEG C；Sample size is 5 μ l.
Further, the specification of described chromatographic column is 3mm × 100mm, 3 μm.
Further, the volume ratio of described mobile phase methanol-Acetic Acid-Water is 30:66:4.
The present invention compared with conventional method, with following advantages：
Sample pre-treatments program under the present invention and Chinese Pharmacopoeia version one Sculellaria barbata medicinal material in 2015 compares, pharmacopeia side
Method is cumbersome, time-consuming, and only sample extraction is accomplished by 6-7 hours, spends petroleum ether and methyl alcohol 225ml；And medicinal material extract of the present invention
Cost 13 minutes, petroleum ether and methyl alcohol 110ml.
The present invention can accurately, it is easy, assay quickly is carried out to scutellarin in Sculellaria barbata.
Brief description of the drawings
Fig. 1 is the result of the test figure of Extracting temperature；
Fig. 2 is the result of the test figure of extraction time；
Fig. 3 is the result of the test figure of cycle-index；
Fig. 4 is scutellarin linear graph.
Specific implementation method
With reference to specific embodiment, claim of the invention is described in further detail, but do not constitute it is right
Any limitation of the invention, the modification of any limited number of time made in the claims in the present invention protection domain, still in the present invention
Claims within.
Embodiment 1
1 instrument and reagent
ASE350 type Accelerate solvent extractions instrument (DIONEX companies of the U.S.)；U3000 high performance liquid chromatographs (U.S. Thermo
Fisher companies), with UV-detector, quaternary gradient pump, automatic sampler；The a ten thousandth electronic balance of XA205DU types ten is (auspicious
Scholar Mettler-Toledo companies)；ELGA PURELAB ClassicUVF cleaning systems.
Scutellarin (lot number：110824-201207, source：National Institute for Food and Drugs Control)；
Methyl alcohol is chromatographically pure；
Petroleum ether (60~90 DEG C)；
Glacial acetic acid is pure for analysis；
Ultra-pure water (laboratory self-control)；
0.45 μm of miillpore filter (U.S., Aglient companies).
Sample：Sculellaria barbata medicinal material (place of production Hunan, lot number 1511024；Place of production Hubei, lot number 150523；Place of production Hunan, batch
Numbers 151001；Place of production Sichuan, lot number：16012017) Wuzhou or Yulin medicinal material market, are purchased from, through Guangxi Wuzhou food and medicine
It is the drying of labiate Sculellaria barbata Scutellaria barbata D.Don that inspection institute deputy director pharmacist of traditional Chinese medicine's Huang Heng is accredited as
Herb.
2 experimental techniques
2.1 chromatographic conditions
Chromatographic column：Thermo-Syncronis C18(3mm × 100mm, 3 μm)；
Mobile phase：Methanol-acetic acid-water (30:66:4)；
Flow velocity：0.3mL/min；
Detection wavelength：335nm；
Column temperature：40℃；
Sample size：5μl.
The preparation of 2.2 reference substance solutions
Take scutellarin reference substance appropriate, it is accurately weighed, plus mobile phase is made solution of every 1ml containing 80 μ g, obtains final product.
The preparation of 2.3 need testing solutions
Accurate Sculellaria barbata powder (crossing No. three sieves) about 1g for weighing different lot numbers, is well mixed with about 1g diatomite respectively,
To be moved into put well in advance in the ASE 10ml abstraction pools of fibrous filter membrane and add appropriate diatomite and fill up extraction pond, gently shaking is allowed to
With Chi Kou in the same horizontal line, tighten and covered on abstraction pool, be put into rapid extracting device and extracted.First with petroleum ether to sample
Carry out except ester (80 DEG C, 5min is circulated 1 time, and flush volume 100%, purge time is 120s), (120 with methyl alcohol as Extraction solvent
DEG C, 8min is circulated 3 times, and flush volume is 60%；Purge time is 60s) extraction terminate after, extract is transferred to
In 100ml measuring bottles, plus methanol dilution is to scale, shakes up, filtration, obtains final product.
2.4 system suitabilities
It is each appropriate that precision measures reference substance solution under " 2.2 ", " 2.3 " item, need testing solution, by chromatostrip under " 2.1 " item
Part is measured, and records chromatogram.
Under the chromatographic condition, each composition can be efficiently separated, separating degree ＞ 1.5.
Result shows that other compositions determine noiseless.
2.5 orthogonal tests
Optimal result is have selected in above-mentioned single factor experiment, to eliminate influencing each other between each factor, using L9
(33) orthogonal test optimized to the scutellarin extraction conditions in Sculellaria barbata, determined and pharmacopeia side with orthogonal experiments
Method extracts the optimal extracting factor of result matching.Orthogonal experiment range analysis the results are shown in Table 1.As shown in Table 1, half is influenceed
Each factor primary-slave relation of the scutellarin extraction effect in lotus is：Extracting temperature>Extraction time>Cycle-index.With reference to each list
Factorial experiments result, show that the optimal extraction process matched with official method extraction result is combined as：Methyl alcohol is molten as extracting
Agent, Extracting temperature is 120 DEG C, extracts 8min, is circulated 3 times.
Table 1
2.5.1 the selection of Extracting temperature
Precision weighs Sculellaria barbata sample 1g, adds the mixing of equivalent diatomite, loaded on 10ml abstraction pools, extraction is filled up with diatomite
Take pond.With methyl alcohol as Extraction solvent, respectively at 80 DEG C, 100 DEG C, 120 DEG C, 5min is extracted 1 time, then enter by " 2.1 " chromatographic condition
Row determines analysis.
As a result：When temperature is 120 DEG C, the recovery rate highest of scutellarin, the optimal Extracting temperature of experiment selection is 120 DEG C
(referring to Fig. 1).
2.5.2 the selection of extraction time
Precision weighs Sculellaria barbata sample 1g, adds the mixing of equivalent diatomite, loaded on 10ml abstraction pools, extraction is filled up with diatomite
Take pond.Extract 5 at 120 DEG C respectively, 8,10min, extract 1 time, then analysis is measured by " 2.1 " chromatographic condition.
As a result：Increasing over time extracted amount is also increasing, and after extraction time is 8min, increases over time
The extracted amount of scutellarin increases little, so for time-consuming raising operating efficiency, this tests the optimal extraction of selection
Time is set to 8min (referring to Fig. 2).
2.5.3 the selection of cycle-index
Precision weighs Sculellaria barbata sample 1g, adds the mixing of equivalent diatomite, loaded on 10ml abstraction pools, extraction is filled up with diatomite
Take pond.8min is extracted at 120 DEG C, circulation is extracted 3 times, it is independent every time to collect extract solution, then surveyed by " 2.1 " chromatographic condition
Setting analysis.The amount of the 3rd extraction scutellarin is 3 times the 10.3% of extraction total amount, so 2 extractions of circulation are not complete enough
's.
As a result：The optimal cycle-index of this experimental selection is 3 times (referring to Fig. 3).
The drafting of 2.6 standard curves
Scutellarin reference substance solution (0.06687mg/ml) is taken, it is accurate respectively to draw the solution 0.1 μ l, 0.2 μ l, 0.5 μ
L, 0.8 μ l, 1 μ l are determined into HPLC, and are determined according to the above method.The results detailed in Table 2.
Linear regression is carried out with concentration (ng)-peak area, regression equation is tried to achieve：Y=11.6990x-29.9160, R2=
0.9996, in good linear relationship in 6.687~66.87ng encloses.Refer to Fig. 4.
Table 2
2.7 replica tests
The sample 1g of identical lot number (16012107) is taken, it is totally 9 parts, accurately weighed, need testing solution is extracted by ASE methods, enter
Sample amount is 1 μ l, and with above-mentioned chromatographic condition parallel test, the content for measuring scutellarin in sample is shown in Table, and RSD is 0.9%.Knot
Fruit refers to table 3.
Table 3
2.8 precision and stability test
Scutellarin reference substance solution (0.06687mg/ml) is taken, continuous sample introduction 6 times records peak area, and peak area RSD is
1.8%, show that instrument precision is good.
Same need testing solution is taken, is placed at room temperature, determined in accordance with the law respectively at 0,1,3,6,12h.
As a result the RSD of scutellarin peak area is 0.8%, shows need testing solution stabilization in 12h.
2.9 sample sizes are determined
The results detailed in Table 4：
Table 4
3. conclusion
In Sculellaria barbata the extraction of scutellarin press official method operation time-consuming and complex steps, by objective factor influenceed compared with
It is cause repeatability poor more；Short using the Accelerate solvent extraction method extraction scutellarin time, extraction efficiency is high, and easy to operate
Can Automated condtrol.
Result shows that the extraction result of Accelerate solvent extraction method is higher with pharmacopeia extracting method matching degree, and the data obtained weight
Existing property is good.
According to the final extraction conditions of assay optimization：With petroleum ether to sample carry out except ester (80 DEG C, 5min, circulate 1 time,
Flush volume 100%) after, with methyl alcohol as Extraction solvent, at 120 DEG C, 8min is circulated 3 times.
The present invention provides a kind of selectable high efficiency extracting method for the assay of scutellarin in Sculellaria barbata.
It is above-described be only presently preferred embodiments of the present invention, it is all made in the range of the spirit and principles in the present invention appoint
What modification, equivalent and improvement etc., should be included within the scope of the present invention.
Claims (7)
1. a kind of method that ASE-HPLC methods determine Content Measurement of Scutellarin in Sculellaria barbata, it is characterised in that successively including following steps
Suddenly：
Step 1：Sculellaria barbata sample after being crushed using ASE extractions, wherein ASE extracting process include first using petroleum ether extraction, so
Again with methanol extraction afterwards, collects methanol extraction liquid；
Step 2：The content of also scutelloside in methanol extraction liquid is determined using HPLC methods.
2. the method that a kind of ASE-HPLC methods according to claim 1 determine Content Measurement of Scutellarin in Sculellaria barbata, its feature
It is that described step 1 includes following sub-steps：
Step S1：By Sculellaria barbata sample comminution, No. three sieves are crossed, take the powder 1g after sieving；
Step S2：Mix with the diatomite of 1g, loaded on being placed with the 10mlASE abstraction pools of fibrous filter membrane, plus diatomite to and pond
Mouth is parallel, uses petroleum ether extraction；
Step S3：Petroleum ether extraction liquid is given up, adds methanol solution to carry out reextraction to the dregs of a decoction；
Step S4：Extract is collected, and adds methanol solution to be settled to 100ml, filtered, obtain methanol extraction liquid.
3. the method that a kind of ASE-HPLC methods according to claim 2 determine Content Measurement of Scutellarin in Sculellaria barbata, its feature
It is that the extraction described in step S2, parameter is as follows：Extraction temperature is 80 DEG C；Extraction time is 5min；Extraction times are 1 time；Punching
It is 100% to wash volume；Purge time is 120s.
4. the method that a kind of ASE-HPLC methods according to claim 2 determine Content Measurement of Scutellarin in Sculellaria barbata, its feature
It is that the extraction described in step S3, parameter is as follows：Extraction temperature is 120 DEG C；Extraction time is 8min；Extraction times are 3 times；
Flush volume is 60%；Purge time is 60s.
5. the method that a kind of ASE-HPLC methods according to claim 1 determine Content Measurement of Scutellarin in Sculellaria barbata, its feature
It is that the detection parameter of the HPLC methods described in step 2 is：Chromatographic column is Thermo Syncronis C18；Mobile phase be methyl alcohol-
Acetic Acid-Water；Flow velocity is 0.3mL/min；Detection wavelength is 335nm；Column temperature is 40 DEG C；Sample size is 5 μ l.
6. the method that a kind of ASE-HPLC methods according to claim 5 determine Content Measurement of Scutellarin in Sculellaria barbata, its feature
It is that the specification of described chromatographic column is 3mm × 100mm, 3 μm.
7. the method that a kind of ASE-HPLC methods according to claim 5 determine Content Measurement of Scutellarin in Sculellaria barbata, its feature
It is that the volume ratio of described mobile phase methanol-Acetic Acid-Water is 30:66:4.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108387669A (en) * | 2018-02-12 | 2018-08-10 | 重庆医药高等专科学校 | A kind of method for building up of rheum officinale quality evaluation system |
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2017
- 2017-03-20 CN CN201710165725.XA patent/CN106918662A/en active Pending
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| CN104910225A (en) * | 2015-05-12 | 2015-09-16 | 广西壮族自治区梧州食品药品检验所 | Method for extracting baicalin from radix scutellariae |
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Application publication date: 20170704 |