CN105353053B - The content assaying method of scutellarin and scutellarin in a kind of Sculellaria barbata medicinal material or its granule - Google Patents
The content assaying method of scutellarin and scutellarin in a kind of Sculellaria barbata medicinal material or its granule Download PDFInfo
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- CN105353053B CN105353053B CN201510917013.XA CN201510917013A CN105353053B CN 105353053 B CN105353053 B CN 105353053B CN 201510917013 A CN201510917013 A CN 201510917013A CN 105353053 B CN105353053 B CN 105353053B
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- 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
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Abstract
The present invention relates to the content assaying method of scutellarin and scutellarin in a kind of Sculellaria barbata medicinal material or its granule.Its feature:Using common isocratic elution, the phosphoric acid of acetonitrile methanol 0.1% with volume ratio as 12.5: 15 16.2: 71.3 72.5 as mobile phase, at 340 ± 2nm of wavelength, while determining the scutellarin and scutellarin content in Sculellaria barbata medicinal material or its granule.Method is easy, quick, it is easy to which popularization is grasped;In three kinds of different chromatographic columns, each crest separates good.Compare with the method recorded under pharmacopeia one Sculellaria barbata medicinal material, prominent progress is a simplified sample treatment program, time, cost are saved, determined by the single composition of scutellarin, 2 kinds of compositions are promoted to determine simultaneously, quality controllability is improved, and overcomes scutellarin cladding impurity peaks, the drawbacks of content results owe accurate.
Description
Technical field
The content assaying method of scutellarin and scutellarin in a kind of Sculellaria barbata medicinal material or its granule.
Background technology
Sculellaria barbata dries herb for labiate Scutellaria barbata D.Don's.It is a kind of conventional Chinese medicine,
Has clearing heat and detoxicating, effect of stagnation resolvation diuresis.For furuncle swelling toxin, abscess of throat, the pain of injury caused by falling and tumbling, oedema, jaundice, snake bite and insect sting.
It is main to contain flavones ingredient, such as baicalein, wogonin, apiolin, cyanidenon, naringenin, scutellarin, 7- hydroxyl -5,8 two
Methoxy flavone, 7- hydroxyl -5,8 dimethoxy flavone -7-0- β-D-Glucose glycosides, 5,7,8,2- kaempferol -7-0- β -
D-Glucose glycosides etc., also contains some diterpene and triterpene lactone class etc..Its quality standard is in Chinese Pharmacopoeia version one and half in 2015
Uncharged thin layer differentiates project under branch lotus medicinal material, has recorded 2 assays, and one is, with scutellarin as index, to use
AAS, determines the general flavone content in medicinal material;Another is using HPLC methods, with methanol-water-acetic acid (35: 61: 4)
The content of scutellarin is determined for mobile phase.Consulting literatures are learnt, are all with the wild root of large-flowered skullcap in current Sculellaria barbata medicinal material and its preparation
Glycosides is index, using the mobile phase of pharmacopeia, determines Content Measurement of Scutellarin.Also find and determine simultaneously scutellarin, wooden slippers grass
The report of element and apiolin, but gradient elution is used, its relative amount is all than relatively low.Do not find also at present using isocratic
Wash-out, while determining the report of scutellarin and scutellarin.It is easy, quick, multi-objective control under above-mentioned background
The quality of Sculellaria barbata medicinal material and its granule, invented using common chromatograph, isocratic elution, while determine Sculellaria barbata and its
The content of scutellarin and scutellarin in granule.
The preparation method of Sculellaria barbata medicinal material granule takes Sculellaria barbata medicine materical crude slice 13000-14000g, adds water respectively 8 times and measures, and decocts
Boil extraction secondary, each 1-2 hours, filtration, 70 DEG C of filtrate is concentrated under reduced pressure, and concentrate is spray-dried or 70 DEG C of drying under reduced pressure, plus
Appropriate dextrin, mixes, and is granulation into 1000g, dispenses, and obtains Sculellaria barbata granule.
The content of the invention
Using common isocratic elution, it is 12.5 with volume ratio: 15-16.2: 71.3-72.5 acetonitrile-methanol -0.1%
Phosphoric acid is mobile phase;Column temperature:30℃;At 340 ± 2nm;The wild root of large-flowered skullcap in Sculellaria barbata medicinal material and its granule is determined simultaneously
The content of glycosides and scutellarin.Method is easy, quick, it is easy to which popularization is grasped;In three kinds of different chromatographic columns, each crest is separated
Well, baseline is steady, and appearance is finished in 44 minutes.
By methodological study, the sample size of scutellarin in 0.0744~0.744 μ g, with peak area in good linear
Relation (is shown in Table 1, Fig. 1), and regression equation is:Y=44.173X-0.9457, r=0.9999;Scutellarin sample size is 0.0516
~0.3612 μ g, are in good linear relationship (being shown in Table 2, Fig. 2) with peak area, and regression equation is:Y=51.554X-0.184, r
=0.9999.Using sample-adding recovery experiment, as a result show:The average recovery rate of scutellarin is 101.18% (n=9), and RSD is
2.67% (being shown in Table 3);The average recovery rate of scutellarin is 101.08% (n=9), and RSD is 1.94% (being shown in Table 4).Precision
(being shown in Table 5), stability (being shown in Table 6), repeated (being shown in Table 7), specificity (see Fig. 3 .4.5) and post durability (are shown in Table 8, figure
6.7.8) experiment meets methodology requirement.Scutellarin and scutellarin suitable for Sculellaria barbata medicinal material and its granule
Quantitative determination.
The technical solution adopted for the present invention to solve the technical problems is:
(1) chromatographic condition is 12.5 with system suitability with volume ratio: 15-16.2: 71.3-72.5 acetonitrile-first
The phosphoric acid of alcohol -0.1% is mobile phase;Column temperature:30℃;Detection wavelength is 340 ± 2nm;Number of theoretical plate presses the calculating of scutellarin peak should
It is not less than 3000;
(2) preparation of reference substance solution takes scutellarin respectively and scutellarin reference substance is appropriate, accurately weighed, puts palm fibre
In colo(u)r specification bottle, plus 70% methyl alcohol is made every 1ml μ g containing scutellarin 40, and scutellarin is the solution of 12 μ g, molten as reference substance
Liquid;
(3) preparation of need testing solution takes Sculellaria barbata fine medicinal material powder 0.5g, accurately weighed;Or Sculellaria barbata granule
0.1g, it is accurately weighed;Put respectively in conical flask with cover, precision adds 70% methyl alcohol 25ml, close plug, weighed weight, fine medicinal material powder
With power 250W, ultrasonically treated 30 minutes of frequency 33kHz, granule with power 250W, ultrasonically treated 10 points of frequency 33kHz
Clock, is let cool, then weighed weight, and the weight of less loss is supplied with 70% methyl alcohol, is shaken up, filtration, is taken filtrate and is filtered with 0.45 μm of micropore
Membrane filtration mistake, subsequent filtrate is used as need testing solution;
(4) determination method is accurate respectively draws above-mentioned reference substance solution and each 10 μ l of need testing solution, injects liquid chromatogram
Instrument, determines the content of scutellarin and scutellarin.
With Shimadzu Wondasil C18With Di Madima Diamonsil C18Chromatographic column, preferred Sculellaria barbata medicinal material and its matches somebody with somebody
The determination techniques scheme of square particle is:
(1) phosphorus of acetonitrile-methanol -0.1% of chromatographic condition and system suitability with volume ratio as 12.5: 15: 72.5
Acid is mobile phase;Column temperature:30℃;Detection wavelength is 340 ± 2nm;Number of theoretical plate is calculated by scutellarin peak and should be not less than 3000;
(2) preparation of reference substance solution takes scutellarin respectively and scutellarin reference substance is appropriate, accurately weighed, puts palm fibre
In colo(u)r specification bottle, plus 70% methyl alcohol is made every 1ml μ g containing scutellarin 40, and scutellarin is the solution of 12 μ g, molten as reference substance
Liquid;
(3) preparation of need testing solution takes Sculellaria barbata fine medicinal material powder 0.5g, accurately weighed;Or Sculellaria barbata granule
0.1g, it is accurately weighed;Put respectively in conical flask with cover, precision adds 70% methyl alcohol 25ml, close plug, weighed weight, fine medicinal material powder
With power 250W, ultrasonically treated 10 minutes of frequency 33kHz, granule with power 250W, ultrasonically treated 30 points of frequency 33kHz
Clock, is let cool, then weighed weight, and the weight of less loss is supplied with 70% methyl alcohol, is shaken up, filtration, is taken filtrate and is filtered with 0.45 μm of micropore
Membrane filtration mistake, subsequent filtrate is used as need testing solution;
(4) determination method is accurate respectively draws above-mentioned reference substance solution and each 10 μ l of need testing solution, injects liquid chromatogram
Instrument, determines the content of scutellarin and scutellarin.
With Agilent Agilent Eclipse Plus C18Chromatographic column, preferred Sculellaria barbata medicinal material and its granule
Determination techniques scheme is:
(1) acetonitrile-methanol -0.1% of chromatographic condition and system suitability with volume ratio as 12.5: 16.2: 71.3
Phosphoric acid is mobile phase;Column temperature:30℃;Detection wavelength is 340 ± 2nm;Number of theoretical plate is calculated by scutellarin peak and should be not less than
3000;
(2) preparation of reference substance solution takes scutellarin respectively and scutellarin reference substance is appropriate, accurately weighed, puts palm fibre
In colo(u)r specification bottle, plus 70% methyl alcohol is made every 1ml μ g containing scutellarin 40, and scutellarin is the solution of 12 μ g, molten as reference substance
Liquid;
(3) preparation of need testing solution takes Sculellaria barbata fine medicinal material powder 0.5g, accurately weighed;Or Sculellaria barbata granule
0.1g, it is accurately weighed;Put respectively in conical flask with cover, precision adds 70% methyl alcohol 25ml, close plug, weighed weight, fine medicinal material powder
With power 250W, ultrasonically treated 30 minutes of frequency 33kHz, granule with power 250W, ultrasonically treated 10 points of frequency 33kHz
Clock, is let cool, then weighed weight, and the weight of less loss is supplied with 70% methyl alcohol, is shaken up, filtration, is taken filtrate and is filtered with 0.45 μm of micropore
Membrane filtration mistake, subsequent filtrate is used as need testing solution;
(4) determination method is accurate respectively draws above-mentioned reference substance solution and each 10 μ l of need testing solution, injects liquid chromatogram
Instrument, determines the content of scutellarin and scutellarin.
Principle of the invention is as follows:
Scutellarin and scutellarin are the relations of glycosides and aglycon, are all flavone compounds, containing multiple polyphenol hydroxyls, easily
Aqueous alcohol is dissolved in, the two spectral absorption figure is consistent, all has absorption maximum (see Fig. 9,10) in 288 ± 2nm and 340 ± 2nm, but
Sensitivity is high at 340nm, so with 340nm as Detection wavelength, carrying out assay.Directly with aqueous methanol ultrasonic extraction medicinal material
Or scutellarin and scutellarin in granule, after filtration, sample introduction.Without extraction, without being evaporated, it is easy, quick, real
With.By adjusting the volume ratio of acetonitrile, methyl alcohol and 0.1% phosphoric acid, make 2 kinds of compositions in 3 kinds of different chromatographic columns, in 44 minutes
Appearance is finished.Again according to 2 kinds of sample sizes of composition within the specific limits, good linear relationship is presented with its peak area, and
For quantitative determining.
Innovative point of the invention and have the beneficial effect that:
(1) using common isocratic elution, reverse-phase chromatographic column, with volume ratio as 12-12.5: 15-16.2: 71.3-72.5
The phosphoric acid of acetonitrile-methanol -0.1% is mobile phase;Scutellarin and the open country in Sculellaria barbata medicinal material and its granule are determined simultaneously
The content of baicalein.By adjusting the ratio of mobile phase, make 2 kinds of compositions in three kinds of different chromatographic columns, appearance is complete within 44 minutes
Finish, each crest separates good.The report that still belongs to the first time is quantitative determined while scutellarin and scutellarin.Realize easy, fast
The hope of victory, science, specification, Two indices control medicinal material and its granule quality.
(2) Sculellaria barbata medicinal material is because that containing the approximate flavonoids of various properties, will obtain the good various flavone components of separating degree
Chromatographic peak, it is necessary to studied by the multifactor serviceability test of chromatographic column.The present invention is obtained in three kinds of different chromatographic columns,
All separate good chromatographic condition (see Fig. 6,7,8).Overcome the assay bar recorded under pharmacopeia one Sculellaria barbata medicinal material
Part, it is impossible to which scutellarin and scutellarin crest are efficiently separated into (see Figure 11), and the drawbacks of lead to not accurate quantitative analysis and determine,
Ensure that the accuracy and reappearance of content results.
(3) the sample pre-treatments program under the present invention and Chinese Pharmacopoeia version one Sculellaria barbata medicinal material in 2015 compares, medicine
Allusion quotation 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 of the present invention
Extract and spend 0.5 hour, 70% methyl alcohol 25ml;Granule spends 10 minutes, 70% methyl alcohol 25ml.Stone is replaced with aqueous methanol
Oily ether and methyl alcohol, not only reduce liposoluble constituent proposition, and after terminating beneficial to measure, the flushing protection of chromatographic column.Fully
Progress of the invention is embodied with significant practical function.
(4) in the content of scutellarin and scutellarin, this method only needs the common liquid with UV-detector
Chromatography, it becomes possible to easy, fast and accurately quantitative determined.
Brief description of the drawings
The linear relationship chart of Fig. 1 scutellarins
The linear relationship chart of Fig. 2 scutellarins
Fig. 3 is scutellarin and scutellarin reference substance HPLC chromatogram
Fig. 4 is Sculellaria barbata medicinal material HPLC chromatogram
Fig. 5 is Sculellaria barbata granule HPLC chromatogram
Fig. 6 serviceability tests-Shimadzu Wondasil C18The sample HPLC chromatogram of (4.6 × 250mm)
The sample HPLC chromatogram of Fig. 7 serviceability tests-Di Ma dimonsil posts (4.6 × 250mm)
Fig. 8 Agilent Agilent Eclipse Plus C18The sample HPLC chromatogram of post (4.6 × 250mm)
The spectral scan figure of Fig. 9 scutellarins
The spectral scan figure of Figure 10 scutellarins
Figure 11 pharmacopeia records the granule HPLC chromatogram that flowing is separated
Fig. 1, Fig. 2 ordinate are peak area;Abscissa is sample size (μ g)
Fig. 9,10 ordinates are absorption intensity (mAU);Abscissa is absorbing wavelength (nm)
Fig. 3, Fig. 4, Fig. 5, Fig. 6, Fig. 7, Fig. 8, Tu11Zhong, the 1. scutellarin of scutellarin 2.
The specific embodiment of the invention
Embodiment 1:
(1) phosphorus of acetonitrile-methanol -0.1% of chromatographic condition and system suitability with volume ratio as 12.5: 15: 72.5
Acid is mobile phase;Column temperature:30℃;Detection wavelength is 340 ± 2nm;Number of theoretical plate is calculated by scutellarin peak and should be not less than 3000;
(2) preparation of reference substance solution takes scutellarin respectively and scutellarin reference substance is appropriate, accurately weighed, puts palm fibre
In colo(u)r specification bottle, plus 70% methyl alcohol is made every 1ml μ g containing scutellarin 40, and scutellarin is the solution of 12 μ g, molten as reference substance
Liquid;
(3) preparation of need testing solution takes Sculellaria barbata fine medicinal material powder 0.5g, accurately weighed;Or Sculellaria barbata granule
0.1g, it is accurately weighed;Put respectively in conical flask with cover, precision adds 70% methyl alcohol 25ml, close plug, weighed weight, fine medicinal material powder
With power 250W, ultrasonically treated 30 minutes of frequency 33kHz, granule with power 250W, ultrasonically treated 10 points of frequency 33kHz
Clock, is let cool, then weighed weight, and the weight of less loss is supplied with 70% methyl alcohol, is shaken up, filtration, is taken filtrate and is filtered with 0.45 μm of micropore
Membrane filtration mistake, subsequent filtrate is used as need testing solution;
(4) determination method is accurate respectively draws above-mentioned reference substance solution and each 10 μ l of need testing solution, injects liquid chromatogram
Instrument, determines the content of scutellarin and scutellarin.3 batches of commercially available Sculellaria barbata medicinal materials and three batches of granule contents are determined, is tied
Fruit is shown in Table 9.
Embodiment 2:
(1) acetonitrile-methanol -0.1% of chromatographic condition and system suitability with volume ratio as 12.5: 16.2: 71.3
Phosphoric acid is mobile phase;Column temperature:30℃;Detection wavelength is 340 ± 2nm;Number of theoretical plate is calculated by scutellarin peak and should be not less than
3000;
(2) preparation of reference substance solution takes scutellarin respectively and scutellarin reference substance is appropriate, accurately weighed, puts palm fibre
In colo(u)r specification bottle, plus 70% methyl alcohol is made every 1ml μ g containing scutellarin 40, and scutellarin is the solution of 12 μ g, molten as reference substance
Liquid;
(3) preparation of need testing solution takes Sculellaria barbata fine medicinal material powder 0.5g, accurately weighed;Or Sculellaria barbata granule
0.1g, it is accurately weighed;Put respectively in conical flask with cover, precision adds 70% methyl alcohol 25ml, close plug, weighed weight, fine medicinal material powder
With power 250W, ultrasonically treated 30 minutes of frequency 33kHz, granule with power 250W, ultrasonically treated 10 points of frequency 33kHz
Clock, is let cool, then weighed weight, and the weight of less loss is supplied with 70% methyl alcohol, is shaken up, filtration, is taken filtrate and is filtered with 0.45 μm of micropore
Membrane filtration mistake, subsequent filtrate is used as need testing solution;
(4) determination method is accurate respectively draws above-mentioned reference substance solution and each 10 μ l of need testing solution, injects liquid chromatogram
Instrument, determines the content of scutellarin and scutellarin.
The scutellarin sample size of table 1 and peak area
The scutellarin sample size of table 2 and peak area
The recovery test result of scutellarin in the sample of table 3
The recovery test result of scutellarin in the sample of table 4
The Precision Experiment result (peak area) of table 5
The stability experiment result (peak area) of table 6
The replica test result (mg/g) of table 7
Assay result (mg/g) of the serviceability test of the table 8-difference chromatographic column to same sample
Note:Chromatographic column specification is all 4.6 × 250mm in upper table.
The assay result (mg/g) of the Sculellaria barbata medicinal material of table 9 and granule
Claims (4)
1. in a kind of Sculellaria barbata medicinal material or its granule scutellarin and scutellarin content assaying method, its feature exists
In:
(1) chromatographic condition is 12.5 with system suitability with volume ratio: 15-16.2: 71.3-72.5 acetonitrile-methanol-
0.1% phosphoric acid is mobile phase;Column temperature:30℃;Detection wavelength is 340 ± 2nm;Number of theoretical plate presses the calculating of scutellarin peak should not be low
In 3000;
(2) preparation of reference substance solution takes scutellarin respectively and scutellarin reference substance is appropriate, accurately weighed, puts brown amount
In bottle, plus 70% methyl alcohol is made every 1ml μ g containing scutellarin 40, and scutellarin is the solution of 12 μ g, used as reference substance solution;
(3) preparation of need testing solution takes Sculellaria barbata fine medicinal material powder 0.5g, accurately weighed;Or Sculellaria barbata granule 0.1g, essence
It is close weighed;In putting conical flask with cover respectively, precision adds 70% methyl alcohol 25ml, close plug, weighed weight, and fine medicinal material powder is with power
Ultrasonically treated 30 minutes of 250W, frequency 33kHz, with power 250W, ultrasonically treated 10 minutes of frequency 33kHz lets cool granule,
Weighed weight, the weight of less loss is supplied with 70% methyl alcohol again, is shaken up, filtration, is taken filtrate and is filtered with 0.45 μm of miillpore filter, is continued
Filtrate is used as need testing solution;
(4) determination method is accurate respectively draws above-mentioned reference substance solution and each 10 μ l of need testing solution, injects liquid chromatograph, surveys
Determine the content of scutellarin and scutellarin.
2. in a kind of Sculellaria barbata medicinal material according to claim 1 or its granule scutellarin and scutellarin content
Assay method, it is characterised in that described Sculellaria barbata granule is per the suitable 13~14g of primary crude drug of 1g.
3. in a kind of Sculellaria barbata medicinal material according to claim 1 or its granule scutellarin and scutellarin content
Assay method, is further characterized in that:
(1) chromatographic condition is by 12.5: 15: 72.5 phosphoric acid of acetonitrile-methanol -0.1% of volume ratio with system suitability
Mobile phase;Column temperature:30℃;Detection wavelength is 340 ± 2nm;Number of theoretical plate is calculated by scutellarin peak and should be not less than 3000;
(2) preparation of reference substance solution takes scutellarin respectively and scutellarin reference substance is appropriate, accurately weighed, puts brown amount
In bottle, plus 70% methyl alcohol is made every 1ml μ g containing scutellarin 40, and scutellarin is the solution of 12 μ g, used as reference substance solution;
(3) preparation of need testing solution takes Sculellaria barbata fine medicinal material powder 0.5g, accurately weighed;Or Sculellaria barbata granule 0.1g, essence
It is close weighed;In putting conical flask with cover respectively, precision adds 70% methyl alcohol 25ml, close plug, weighed weight, and fine medicinal material powder is with power
Ultrasonically treated 30 minutes of 250W, frequency 33kHz, with power 250W, ultrasonically treated 10 minutes of frequency 33kHz lets cool granule,
Weighed weight, the weight of less loss is supplied with 70% methyl alcohol again, is shaken up, filtration, is taken filtrate and is filtered with 0.45 μm of miillpore filter, is continued
Filtrate is used as need testing solution;
(4) determination method is accurate respectively draws above-mentioned reference substance solution and each 10 μ l of need testing solution, injects liquid chromatograph, surveys
Determine the content of scutellarin and scutellarin.
4. in a kind of Sculellaria barbata medicinal material according to claim 1 or its granule scutellarin and scutellarin content
Assay method, is further characterized in that:
(1) phosphoric acid of acetonitrile-methanol -0.1% of chromatographic condition and system suitability with volume ratio as 12.5: 16.2: 71.3
It is mobile phase;Column temperature:30℃;Detection wavelength is 340 ± 2nm;Number of theoretical plate is calculated by scutellarin peak and should be not less than 3000;
(2) preparation of reference substance solution takes scutellarin respectively and scutellarin reference substance is appropriate, accurately weighed, puts brown amount
In bottle, plus 70% methyl alcohol is made every 1ml μ g containing scutellarin 40, and scutellarin is the solution of 12 μ g, used as reference substance solution;
(3) preparation of need testing solution takes Sculellaria barbata fine medicinal material powder 0.5g, accurately weighed;Or Sculellaria barbata granule 0.1g, essence
It is close weighed;In putting conical flask with cover respectively, precision adds 70% methyl alcohol 25ml, close plug, weighed weight, and fine medicinal material powder is with power
Ultrasonically treated 30 minutes of 250W, frequency 33kHz, with power 250W, ultrasonically treated 10 minutes of frequency 33kHz lets cool granule,
Weighed weight, the weight of less loss is supplied with 70% methyl alcohol again, is shaken up, filtration, is taken filtrate and is filtered with 0.45 μm of miillpore filter, is continued
Filtrate is used as need testing solution;
(4) determination method is accurate respectively draws above-mentioned reference substance solution and each 10 μ l of need testing solution, injects liquid chromatograph, surveys
Determine the content of scutellarin and scutellarin.
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