CN105353053A - Content determination method for scutellarin and scutellarein in sculellaria barbata medicinal material and formula granule of sculellaria barbata medicinal material - Google Patents
Content determination method for scutellarin and scutellarein in sculellaria barbata medicinal material and formula granule of sculellaria barbata medicinal material Download PDFInfo
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- CN105353053A CN105353053A CN201510917013.XA CN201510917013A CN105353053A CN 105353053 A CN105353053 A CN 105353053A CN 201510917013 A CN201510917013 A CN 201510917013A CN 105353053 A CN105353053 A CN 105353053A
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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
- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
- G01N2030/027—Liquid chromatography
Abstract
The invention relates to a content determination method for scutellarin and scutellarein in sculellaria barbata medicinal material and formula granule of sculellaria barbata medicinal material. The content determination method is characterized in that common isocratic elution is adopted, acetonitrile-methyl alcohol-0.1 percent phosphoric acid of which the volume ratio is 12.5:(15 to 16.2):(71.3 to 72.5) is taken as a mobile phase, and the contents of the scutellarin and the scutellarein in the sculellaria barbata medicinal material and the formula granule of the sculellaria barbata medicinal material are simultaneously determined at a wavelength of 340+/-2nm. The method is simple, convenient, fast, and easy to popularize and master; the separations of wave crests on three different chromatographic columns are good. Compared with a method of recording under a sculellaria barbata medicinal material item of the first part of the pharmacopeia, the prominent improvement is that a sample treatment process is simplified, the time and cost are saved, the determination is advanced from single component determination of the scutellarin to the simultaneous determination of the two components, the quality controllability is improved, and the defects that impurity peaks exist and the content results are inaccurate are overcome.
Description
Technical field
The content assaying method of scutellarin and scutellarin in a kind of Sculellaria barbata medicinal material and granule thereof.
Background technology
Sculellaria barbata is the dry herb of labiate ScutellariabarbataD.Don.Be a kind of conventional Chinese medicine, tool is clearing heat and detoxicating, effect of stagnation resolvation diuresis.For furuncle swelling toxin, abscess of throat, falls and flutters the pain of injury, oedema, jaundice, snake bite and insect sting.Main containing flavones ingredient, as baicalein, wogonin, apiolin, cyanidenon, naringenin, scutellarin, 7-hydroxyl-5,8 dimethoxy flavones, 7-hydroxyl-5,8 dimethoxy flavone-7-O-β-D-Glucose glycosides, 5,7,8,2-kaempferol-7-O-β-D-Glucose glycosides etc., also containing some diterpene and triterpene lactone class etc.Its quality standard does not record TLC distinguish project under Chinese Pharmacopoeia version in 2015 Sculellaria barbata medicinal material item, and recorded 2 assays, one is take scutellarin as index, adopts spectrophotometric method, measures the general flavone content in medicinal material; Another adopts HPLC method, with the content of methanol-water-acetic acid (35: 61: 4) for mobile phase mensuration scutellarin.By consulting literatures is learnt, be all be index with scutellarin, adopt the mobile phase of pharmacopeia in current Sculellaria barbata medicinal material and preparation thereof, measures Content Measurement of Scutellarin.Also find the report of Simultaneously test scutellarin, Luteolin and apiolin, but employing is gradient elution, its relative content is all lower.Also do not find employing isocratic elution, the report of Simultaneously test scutellarin and scutellarin at present.In above-mentioned background situation, be the quality of easy, quick, multi-objective control Sculellaria barbata medicinal material and granule thereof, invented the common chromatograph of employing, isocratic elution, the scutellarin in Simultaneously test Sculellaria barbata and granule thereof and the content of scutellarin.
The preparation method of Sculellaria barbata medicinal material granule gets Sculellaria barbata medicine materical crude slice 13000-14000g, add water 8 times amount respectively, decocts and extract secondary, each 1-2 hour, filter, filtrate 70 DEG C of reduced pressure concentrations, concentrate spraying dry or 70 DEG C of drying under reduced pressure, add dextrin appropriate, mixing, be granulation into 1000g, packing, obtain Sculellaria barbata granule.
Summary of the invention
Adopting common isocratic elution, is that acetonitrile-methanol-0.1% phosphoric acid of 12.5: 15-16.2: 71.3-72.5 is for mobile phase with volume ratio; Column temperature: 30 DEG C; At 340 ± 2nm place; The content of scutellarin and scutellarin in Simultaneously test Sculellaria barbata medicinal material and granule thereof.Method is easy, quick, is easy to universal and grasps; In three kinds of different chromatographic columns, each crest is separated good, and baseline is steady, goes out peak complete in 44 minutes.
By methodological study, the sample size of scutellarin is at 0.0744 ~ 0.744 μ g, and be good linear relationship (see table 1, Fig. 1) with peak area, regression equation is: Y=44.173X-0.9457, r=0.9999; Scutellarin sample size is at 0.0516 ~ 0.3612 μ g, and be good linear relationship (see table 2, Fig. 2) with peak area, regression equation is: Y=51.554X-0.184, r=0.9999.Adopt application of sample recovery experiment, result shows: the average recovery rate of scutellarin is 101.18% (n=9), RSD is 2.67% (see table 3); The average recovery rate of scutellarin is 101.08% (n=9), RSD is 1.94% (see table 4).Precision (see table 5), stability (see table 6), repeatability (see table 7), specificity (see Fig. 3,4,5) are tested with post durability (see table 8, Fig. 6,7,8) and are all met methodology requirement.Be applicable to the quantitative measurement of scutellarin and scutellarin in Sculellaria barbata medicinal material and granule thereof.
The technical solution adopted for the present invention to solve the technical problems is:
(1) chromatographic condition and system suitability are that acetonitrile-methanol-0.1% phosphoric acid of 12.5: 15-16.2: 71.3-72.5 is for mobile phase with volume ratio; Column temperature: 30 DEG C; Determined wavelength is 340 ± 2nm; Number of theoretical plate calculates should be not less than 3000 by scutellarin peak;
(2) to get scutellarin and scutellarin reference substance respectively appropriate, accurately weighed in the preparation of reference substance solution, and put in brown measuring bottle, add 70% methyl alcohol and make every 1ml containing scutellarin 40 μ g, scutellarin is the solution of 12 μ g, in contrast product solution;
(3) Sculellaria barbata fine medicinal material powder 0.5g is got in the preparation of need testing solution, accurately weighed; Or Sculellaria barbata granule 0.1g, accurately weighed; Put in tool plug conical flask respectively, precision adds 70% methyl alcohol 25ml, close plug, weighed weight, fine medicinal material powder was with the ultrasonic process of power 250W, frequency 33kHz 30 minutes, granule, with the ultrasonic process of power 250W, frequency 33kHz 10 minutes, lets cool, weighed weight again, supply the weight of less loss with 70% methyl alcohol, shake up, filter, get filtrate to filter with the miillpore filter of 0.45 μm, subsequent filtrate is 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, injection liquid chromatography, measures the content of scutellarin and scutellarin.
With Shimadzu WondasilC
18with Di Madima DiamonsilC
18chromatographic column, the determination techniques scheme of preferred Sculellaria barbata medicinal material and granule thereof is:
(1) chromatographic condition and system suitability are that acetonitrile-methanol-0.1% phosphoric acid of 12.5: 15: 72.5 is for mobile phase with volume ratio; Column temperature: 30 DEG C; Determined wavelength is 340 ± 2nm; Number of theoretical plate calculates should be not less than 3000 by scutellarin peak;
(2) to get scutellarin and scutellarin reference substance respectively appropriate, accurately weighed in the preparation of reference substance solution, and put in brown measuring bottle, add 70% methyl alcohol and make every 1ml containing scutellarin 40 μ g, scutellarin is the solution of 12 μ g, in contrast product solution;
(3) Sculellaria barbata fine medicinal material powder 0.5g is got in the preparation of need testing solution, accurately weighed; Or Sculellaria barbata granule 0.1g, accurately weighed; Put in tool plug conical flask respectively, precision adds 70% methyl alcohol 25ml, close plug, weighed weight, fine medicinal material powder was with the ultrasonic process of power 250W, frequency 33kHz 10 minutes, granule, with the ultrasonic process of power 250W, frequency 33kHz 30 minutes, lets cool, weighed weight again, supply the weight of less loss with 70% methyl alcohol, shake up, filter, get filtrate to filter with the miillpore filter of 0.45 μm, subsequent filtrate is 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, injection liquid chromatography, measures the content of scutellarin and scutellarin.
With Agilent AgilentEclipsePlusC
18chromatographic column, the determination techniques scheme of preferred Sculellaria barbata medicinal material and granule thereof is:
(1) chromatographic condition and system suitability are that acetonitrile-methanol-0.1% phosphoric acid of 12.5: 16.2: 71.3 is for mobile phase with volume ratio; Column temperature: 30 DEG C; Determined wavelength is 340 ± 2nm; Number of theoretical plate calculates should be not less than 3000 by scutellarin peak;
(2) to get scutellarin and scutellarin reference substance respectively appropriate, accurately weighed in the preparation of reference substance solution, and put in brown measuring bottle, add 70% methyl alcohol and make every 1ml containing scutellarin 40 μ g, scutellarin is the solution of 12 μ g, in contrast product solution;
(3) Sculellaria barbata fine medicinal material powder 0.5g is got in the preparation of need testing solution, accurately weighed; Or Sculellaria barbata granule 0.1g, accurately weighed; Put in tool plug conical flask respectively, precision adds 70% methyl alcohol 25ml, close plug, weighed weight, fine medicinal material powder was with the ultrasonic process of power 250W, frequency 33kHz 30 minutes, granule, with the ultrasonic process of power 250W, frequency 33kHz 10 minutes, lets cool, weighed weight again, supply the weight of less loss with 70% methyl alcohol, shake up, filter, get filtrate to filter with the miillpore filter of 0.45 μm, subsequent filtrate is 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, injection liquid chromatography, measures the content of scutellarin and scutellarin.
Principle of the present invention is as follows:
Scutellarin and scutellarin are the relations of glycosides and aglycon, it is all flavone compound, containing multiple polyphenol hydroxyl, be soluble in aqueous alcohol, the two spectral absorption figure is consistent, all have absorption maximum (see Fig. 9,10) at 288 ± 2nm and 340 ± 2nm, but 340nm place is highly sensitive, so be determined wavelength with 340nm, carry out assay.Directly with the scutellarin in the ultrasonic extraction medicinal material of aqueous methanol or granule and scutellarin, after filtration, sample introduction.Without extraction, without evaporate to dryness, easy, quick, practical.By adjusting the volume ratio of acetonitrile, methyl alcohol and 0.1% phosphoric acid, making 2 kinds of compositions in 3 kinds of different chromatographic columns, going out peak in 44 minutes complete.Again according to these 2 kinds of compositions sample size within the specific limits, present good linear relationship with its peak area, and for quantitative measurement.
Innovative point of the present invention and beneficial effect as follows:
(1) adopting common isocratic elution, reverse-phase chromatographic column, is that acetonitrile-methanol-0.1% phosphoric acid of 12-12.5: 15-16.2: 71.3-72.5 is mobile phase with volume ratio; Scutellarin in Simultaneously test Sculellaria barbata medicinal material and granule thereof and the content of scutellarin.By adjusting the ratio of mobile phase, make 2 kinds of compositions in three kinds of different chromatographic columns, within 44 minutes, go out peak complete, each crest is separated good.The Simultaneous Determination of scutellarin and scutellarin still belongs to the first time report.Achieve easy, quick, that science, specification, Two indices control medicinal material and its granule quality hope.
(2) Sculellaria barbata medicinal material is because of the flavonoids be similar to containing multiple character, obtain the chromatographic peak of the good multiple flavone component of degree of separation, must by the multifactor serviceability test research of chromatographic column.The present invention obtains in three kinds of different chromatographic columns, is all separated good chromatographic condition (see Fig. 6,7,8).The assay condition recorded under overcoming pharmacopeia Sculellaria barbata medicinal material item, scutellarin and scutellarin crest effectively cannot be separated (see Figure 11), and cause cannot accurate quantitative analysis measure drawback, ensure that accuracy and the reappearance of content results.
(3) the sample pre-treatments program under the present invention and Chinese Pharmacopoeia version in 2015 Sculellaria barbata medicinal material item compares, and official method is more loaded down with trivial details, time-consuming, and only sample extraction just needs 6-7 hour, cost sherwood oil and methyl alcohol 225ml; And medicinal material extract of the present invention spends 0.5 hour, 70% methyl alcohol 25ml; Granule spends 10 minutes, 70% methyl alcohol 25ml.Replace sherwood oil and methyl alcohol with aqueous methanol, not only decrease liposoluble constituent and propose, and be beneficial to after mensuration terminates, the flushing protection of chromatographic column.Progress of the present invention and significant practical function are fully demonstrated.
(4) on the content of scutellarin and scutellarin, the liquid chromatograph of the band UV-detector that this method only needs a Daepori to lead to, just can easy, carry out quantitative measurement fast and accurately.
Accompanying drawing explanation
The linear relationship chart of Fig. 1 scutellarin
The linear relationship chart of Fig. 2 scutellarin
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 test-Shimadzu WondasilC
18the sample HPLC chromatogram of (4.6 × 250mm)
The sample HPLC chromatogram of Fig. 7 serviceability test-Di Ma dimonsil post (4.6 × 250mm)
Fig. 8 Agilent AgilentEclipsePlusC
18the sample HPLC chromatogram of post (4.6 × 250mm)
The spectral scan figure of Fig. 9 scutellarin
The spectral scan figure of Figure 10 scutellarin
Figure 11 pharmacopeia records the granule HPLC chromatogram that mobile phase is separated
Fig. 1, Fig. 2 ordinate is peak area; Horizontal ordinate is sample size (μ g)
Fig. 9,10 ordinates are absorption intensity (mAU); Horizontal ordinate is absorbing wavelength (nm)
Fig. 3, Fig. 4, Fig. 5, Fig. 6, Fig. 7, Fig. 8, Tu11Zhong, 1. scutellarin 2. scutellarin
The specific embodiment of the invention
Embodiment 1:
(1) chromatographic condition and system suitability are that acetonitrile-methanol-0.1% phosphoric acid of 12.5: 15: 72.5 is for mobile phase with volume ratio; Column temperature: 30 DEG C; Determined wavelength is 340 ± 2nm; Number of theoretical plate calculates should be not less than 3000 by scutellarin peak;
(2) to get scutellarin and scutellarin reference substance respectively appropriate, accurately weighed in the preparation of reference substance solution, and put in brown measuring bottle, add 70% methyl alcohol and make every 1ml containing scutellarin 40 μ g, scutellarin is the solution of 12 μ g, in contrast product solution;
(3) Sculellaria barbata fine medicinal material powder 0.5g is got in the preparation of need testing solution, accurately weighed; Or Sculellaria barbata granule 0.1g, accurately weighed; Put in tool plug conical flask respectively, precision adds 70% methyl alcohol 25ml, close plug, weighed weight, fine medicinal material powder was with the ultrasonic process of power 250W, frequency 33kHz 30 minutes, granule, with the ultrasonic process of power 250W, frequency 33kHz 10 minutes, lets cool, weighed weight again, supply the weight of less loss with 70% methyl alcohol, shake up, filter, get filtrate to filter with the miillpore filter of 0.45 μm, subsequent filtrate is 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, injection liquid chromatography, measures the content of scutellarin and scutellarin.Determine 3 batches of commercially available Sculellaria barbata medicinal materials and three batches of granule content, the results are shown in Table 9.
Embodiment 2:
(1) chromatographic condition and system suitability are that acetonitrile-methanol-0.1% phosphoric acid of 12.5: 16.2: 71.3 is for mobile phase with volume ratio; Column temperature: 30 DEG C; Determined wavelength is 340 ± 2nm; Number of theoretical plate calculates should be not less than 3000 by scutellarin peak;
(2) to get scutellarin and scutellarin reference substance respectively appropriate, accurately weighed in the preparation of reference substance solution, and put in brown measuring bottle, add 70% methyl alcohol and make every 1ml containing scutellarin 40 μ g, scutellarin is the solution of 12 μ g, in contrast product solution;
(3) Sculellaria barbata fine medicinal material powder 0.5g is got in the preparation of need testing solution, accurately weighed; Or Sculellaria barbata granule 0.1g, accurately weighed; Put in tool plug conical flask respectively, precision adds 70% methyl alcohol 25ml, close plug, weighed weight, fine medicinal material powder was with the ultrasonic process of power 250W, frequency 33kHz 30 minutes, granule, with the ultrasonic process of power 250W, frequency 33kHz 10 minutes, lets cool, weighed weight again, supply the weight of less loss with 70% methyl alcohol, shake up, filter, get filtrate to filter with the miillpore filter of 0.45 μm, subsequent filtrate is 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, injection liquid chromatography, measures the content of scutellarin and scutellarin.
Table 1 scutellarin sample size and peak area
Table 2 scutellarin sample size and peak area
The recovery test result of scutellarin in table 3 sample
The recovery test result of scutellarin in table 4 sample
Table 5 Precision Experiment result (peak area)
Table 6 stability experiment result (peak area)
Table 7 replica test result (mg/g)
Table 8 serviceability test-different chromatographic column is to the assay result (mg/g) of same sample
Note: in upper table, chromatographic column specification is all 4.6 × 250mm.
The assay result (mg/g) of table 9 Sculellaria barbata medicinal material and granule
Claims (4)
1. the content assaying method of scutellarin and scutellarin in Sculellaria barbata medicinal material and granule thereof, is characterized in that:
(1) chromatographic condition and system suitability are that acetonitrile-methanol-0.1% phosphoric acid of 12.5: 15-16.2: 71.3-72.5 is for mobile phase with volume ratio; Column temperature: 30 DEG C; Determined wavelength is 340 ± 2nm; Number of theoretical plate calculates should be not less than 3000 by scutellarin peak;
(2) to get scutellarin and scutellarin reference substance respectively appropriate, accurately weighed in the preparation of reference substance solution, and put in brown measuring bottle, add 70% methyl alcohol and make every 1ml containing scutellarin 40 μ g, scutellarin is the solution of 12 μ g, in contrast product solution;
(3) Sculellaria barbata fine medicinal material powder 0.5g is got in the preparation of need testing solution, accurately weighed; Or Sculellaria barbata granule 0.1g, accurately weighed; Put in tool plug conical flask respectively, precision adds 70% methyl alcohol 25ml, close plug, weighed weight, fine medicinal material powder was with the ultrasonic process of power 250W, frequency 33kHz 30 minutes, granule, with the ultrasonic process of power 250W, frequency 33kHz 10 minutes, lets cool, weighed weight again, supply the weight of less loss with 70% methyl alcohol, shake up, filter, get filtrate to filter with the miillpore filter of 0.45 μm, subsequent filtrate is 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, injection liquid chromatography, measures the content of scutellarin and scutellarin.
2. the content assaying method of scutellarin and scutellarin in a kind of Sculellaria barbata medicinal material according to claim 1 and granule thereof, is characterized in that the described suitable primary crude drug 13 ~ 14g of the every 1g of Sculellaria barbata granule.
3. the content assaying method of scutellarin and scutellarin in a kind of Sculellaria barbata medicinal material according to claim 1 and granule thereof, is further characterized in that:
(1) chromatographic condition and system suitability are that acetonitrile-methanol-0.1% phosphoric acid of 12.5: 15: 72.5 is for mobile phase with volume ratio; Column temperature: 30 DEG C; Determined wavelength is 340 ± 2nm; Number of theoretical plate calculates should be not less than 3000 by scutellarin peak;
(2) to get scutellarin and scutellarin reference substance respectively appropriate, accurately weighed in the preparation of reference substance solution, and put in brown measuring bottle, add 70% methyl alcohol and make every 1ml containing scutellarin 40 μ g, scutellarin is the solution of 12 μ g, in contrast product solution;
(3) Sculellaria barbata fine medicinal material powder 0.5g is got in the preparation of need testing solution, accurately weighed; Or Sculellaria barbata granule 0.1g, accurately weighed; Put in tool plug conical flask respectively, precision adds 70% methyl alcohol 25ml, close plug, weighed weight, fine medicinal material powder was with the ultrasonic process of power 250W, frequency 33kHz 30 minutes, granule, with the ultrasonic process of power 250W, frequency 33kHz 10 minutes, lets cool, weighed weight again, supply the weight of less loss with 70% methyl alcohol, shake up, filter, get filtrate to filter with the miillpore filter of 0.45 μm, subsequent filtrate is 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, injection liquid chromatography, measures the content of scutellarin and scutellarin.
4. the content assaying method of scutellarin and scutellarin in a kind of Sculellaria barbata medicinal material according to claim 1 and granule thereof, is further characterized in that:
(1) chromatographic condition and system suitability are that acetonitrile-methanol-0.1% phosphoric acid of 12.5: 16.2: 71.3 is for mobile phase with volume ratio; Column temperature: 30 DEG C; Determined wavelength is 340 ± 2nm; Number of theoretical plate calculates should be not less than 3000 by scutellarin peak;
(2) to get scutellarin and scutellarin reference substance respectively appropriate, accurately weighed in the preparation of reference substance solution, and put in brown measuring bottle, add 70% methyl alcohol and make every 1ml containing scutellarin 40 μ g, scutellarin is the solution of 12 μ g, in contrast product solution;
(3) Sculellaria barbata fine medicinal material powder 0.5g is got in the preparation of need testing solution, accurately weighed; Or Sculellaria barbata granule 0.1g, accurately weighed; Put in tool plug conical flask respectively, precision adds 70% methyl alcohol 25ml, close plug, weighed weight, fine medicinal material powder was with the ultrasonic process of power 250W, frequency 33kHz 30 minutes, granule, with the ultrasonic process of power 250W, frequency 33kHz 10 minutes, lets cool, weighed weight again, supply the weight of less loss with 70% methyl alcohol, shake up, filter, get filtrate to filter with the miillpore filter of 0.45 μm, subsequent filtrate is 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, injection liquid chromatography, measures the content of scutellarin and scutellarin.
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| CN106950318A (en) * | 2017-04-20 | 2017-07-14 | 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 baicalin in Scutellaria baicalensis Georgi content |
| CN108051535A (en) * | 2017-12-22 | 2018-05-18 | 广东方制药有限公司 | A kind of method of UPLC-MS-MS rapid screenings Sculellaria barbata different sources otherness |
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| CN106918662A (en) * | 2017-03-20 | 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 Content Measurement of Scutellarin in Sculellaria barbata |
| CN106950318A (en) * | 2017-04-20 | 2017-07-14 | 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 baicalin in Scutellaria baicalensis Georgi content |
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| CN114028344A (en) * | 2021-12-14 | 2022-02-11 | 四川新绿色药业科技发展有限公司 | Preparation method and detection method of sculellaria barbata formula granules |
| CN114527218A (en) * | 2022-02-24 | 2022-05-24 | 北京五和博澳药业股份有限公司 | Method for detecting components of scutellaria baicalensis |
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