CN105606756A - Antibacterial anti-inflammatory capsule quality detection method - Google Patents
Antibacterial anti-inflammatory capsule quality detection method Download PDFInfo
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Abstract
The invention discloses an antibacterial anti-inflammatory capsule quality detection method. Antibacterial anti-inflammatory capsules are prepared from honeysuckle flowers, radix stemonae, Chinese rhubarb, folium isatidis, radix scutellariae, rhizoma anemarrhenae and a christina loosestrife herb. The antibacterial anti-inflammatory capsule quality detection method comprises the four steps of suitability test on chromatographic conditions and a system, preparation of a reference substance solution, preparation of a test sample solution and determination. In addition, the radix stemonae, the Chinese rhubarb, the radix scutellariae, the rhizoma anemarrhenae and the honeysuckle flowers are subjected to thin-layer identification. The antibacterial anti-inflammatory capsule quality detection method has the advantages of being simple and easy to operate and capable of effectively controlling the product quality.
Description
Technical field
The invention belongs to Chinese medicine preparation Quality Control Technology field, be specifically related to a kind of quality testing of Antibicrobial anti inflammatory capsuleMethod.
Background technology
Antibicrobial anti inflammatory capsule is for recording changing of in the drug standards promulgated by the ministries or commissions of the Central Government the 7th (WS3-B-1339-93) anti-inflammation sheetBecome formulation kind, formed by honeysuckle, the tuber of stemona, rheum officinale, folium isatidis, the root of large-flowered skullcap, the wind-weed, desmodium seven flavor medicine thing, there is heat-clearing, rush downEffect of fire, removing toxic substances, can be used for anemopyretic cold, abscess of throat, excess fire toothache. Antibicrobial anti inflammatory capsule has the treatment of its uniqueness and doesWith, can partly replace chemobiotic, the phenomenon that reduces China's Western medicine abuse of antibiotics is had to certain facilitation.
Fang Zhong: honeysuckle is clearing heat and detoxicating, wind-heat dissipating; The cough-relieving of tuber of stemona moistening lung to lower qi, desinsection; The rheum officinale logical intestines that purge heat, cool bloodRemoving toxic substances, stimulates the menstrual flow by the stasis of blood; Folium isatidis is clearing heat and detoxicating, blood cooling and ecchymoses removing; Root of large-flowered skullcap heat-clearing and damp-drying drug, purging intense heat and detonicating, hemostasis, antiabortive; The wind-weed is clearHot purging intense heat, promotes the production of body fluid and moisturizes; Desmodium eliminating dampness and heat, treating stranguria, detumescence. And former anti-inflammation sheet standard is not to any in prescriptionThe active ingredient of medicine is carried out quantitative and qualitative analysis monitoring, can not carry out effective quality testing to product.
Summary of the invention
The object of the invention is to overcome above-mentioned shortcoming and provide a kind of simple, can effective control for product quality anti-The quality determining method of bacterium antiphlogistic capsule.
The quality determining method of a kind of Antibicrobial anti inflammatory capsule of the present invention, described Antibicrobial anti inflammatory capsule by honeysuckle, the tuber of stemona,Rheum officinale, folium isatidis, the root of large-flowered skullcap, the wind-weed and desmodium prepare, and comprise the following steps:
(1) chromatographic condition and system suitability experiment: with polarity silica gel be filler; With water, methyl alcohol, glacial acetic acid by volume51-55:45-49:2-5, PH=2.5-3.5 are mobile phase; Detection wavelength is 275-285nm; Theoretical cam curve is by scutelloside peakCalculation should be not less than 2000;
(2) preparation of reference substance solution: it is appropriate that precision takes scutelloside reference substance, adds methyl alcohol and makes molten containing 0.04mg of every 1mlLiquid, for subsequent use;
(3) preparation of need testing solution: get this product 70-90 order fine powder 0.25g, accurately weighed, precision adds mass percent denseDegree is the ethanol 25ml of 60-80%, and weighed weight, adds hot reflux 3 hours, let cool to room temperature, more weighed weight, use quality percentageSpecific concentration is the weight that the ethanol of 60-80% is supplied less loss, shakes up, and filters, and precision measures filtrate 2ml, put in 10ml volumetric flask,Add methyl alcohol to scale, shake up, for subsequent use;
(4) precision is drawn reference substance solution and the each 10 μ l of need testing solution respectively, and injection liquid chromatography is measured; Wherein, this productEvery should be no less than 3.7mg containing the root of large-flowered skullcap in scutelloside.
The quality determining method of above-mentioned a kind of Antibicrobial anti inflammatory capsule, wherein: the thin-layer identification method of the described tuber of stemona is:
(1) take this product content 2g, add ammonia solution 2ml, chloroform 20ml, ultrasonic processing 30min, takes out, and filters, and filtrate is wavedDry, residue adds the hydrochloric acid solution 1ml that mass percent concentration is 2-5%, is stirred to dissolve, and supernatant is put in test tube, uses dense ammoniaIt is 9-11 that water regulates pH, adds 0.5ml chloroform, shake well, and stratification, gets chloroform layer as need testing solution;
(2) separately get tuber of stemona control medicinal material 0.1g, add ammonia solution 0.1ml, chloroform 1ml, ultrasonic processing 20min, gets chloroform solution conductControl medicinal material solution;
(3) according to " Chinese pharmacopoeia " 2010 editions one thin-layered chromatography annex VI B test, draw respectively need testing solution and rightAccording to the each 2.5-5 μ of medicinal material solution l, put on same silica gel g thin-layer plate, taking toluene, ethyl acetate, chloroform by volume 2:8:2 asSolvent, launches, and takes out, and dries iodine colour developing; In test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, aobvious identicalColor spot.
The quality determining method of above-mentioned a kind of Antibicrobial anti inflammatory capsule, wherein: the thin-layer identification method of described rheum officinale is:
(1) take this product content 0.5g, put in tool plug test tube, add ethanol 1ml, ultrasonic processing 30min, takes out, and stirs evenly, and leaves standstillClarification, gets supernatant as need testing solution;
(2) separately get rheum officinale control medicinal material 0.05g, be made in the same way of control medicinal material solution with need testing solution;
(3) according to " Chinese pharmacopoeia " 2010 editions one thin-layered chromatography annex VI B test, draw respectively need testing solution and rightAccording to the each 5 μ l of medicinal material solution, put on same silica gel g thin-layer plate, taking toluene, ethyl acetate, formic acid by volume 8:1:0.1 as exhibitionOpen agent, launch, take out, dry, put under the ultraviolet lamp that wavelength is 365nm and inspect; In test sample chromatogram, with control medicinal material lookCompose on corresponding position, aobvious same color fluorescence spot.
The quality determining method of above-mentioned a kind of Antibicrobial anti inflammatory capsule, wherein: the thin layer of the described root of large-flowered skullcap is differentiated:
(1) get this product capsule 's content 1g, in the triangular flask of 50ml, add the ultrasonic processing of methyl alcohol 10ml 10min, leave standstill clarification, getSupernatant is as need testing solution;
(2) separately get root of large-flowered skullcap control medicinal material 0.5g, be made in the same way of control medicinal material solution with need testing solution;
(3) get again scutelloside reference substance, add methyl alcohol and make the solution of every 1ml containing 0.5-1.0mg, product solution in contrast;
(4) according to " Chinese pharmacopoeia " 2010 editions one thin-layered chromatography annex VI B test, draw respectively need testing solution, contrastMedicinal material solution, the each 5ul of reference substance solution, put on same polyamide film, the ice vinegar that is 35-37% with mass percent concentrationAcid, as solvent, launches, and takes out, and dries, and the ferric trichloride ethanolic solution of spray taking mass percent concentration as 5-10%, makes spotPoint colour developing is clear; In test sample chromatogram, with control medicinal material chromatogram and the corresponding position of reference substance chromatogram on, aobvious same color spotPoint.
The quality determining method of above-mentioned a kind of Antibicrobial anti inflammatory capsule, wherein: the thin layer of the described wind-weed is differentiated:
(1) get this product capsule 's content 1g, in the triangular flask of 50ml, adding mass percent concentration is the acetone 10ml of 25-35%,Ultrasonic 30min, leaves standstill clarification, gets supernatant as need testing solution;
(2) separately getting rhizoma anemarrhenae saponin BII reference substance, to add mass percent concentration be that the acetone of 25-35% is made every 1ml containing 0.5mg'sSolution, in contrast product solution;
(3) according to " Chinese pharmacopoeia " 2010 editions one thin-layered chromatography annex VI B test, draw respectively need testing solution and rightAccording to the each 5ul of product solution, put on same silica G plate, with n-butanol, glacial acetic acid, the water upper solution conduct of 4:1:5 by volumeSolvent launches, and takes out, and dries, and the phosphomolybdic acid ethanol solution of spray taking mass percent concentration as 5-10%, puts into 105-110 DEG CBaking oven, until spot clear display; In test sample chromatogram, with the corresponding principal spot of reference substance chromatogram position on, aobvious identicalColor spot.
The quality determining method of above-mentioned a kind of Antibicrobial anti inflammatory capsule, wherein: the thin layer of described honeysuckle is differentiated:
(1) get this product capsule 's content 1g, add methyl alcohol 10ml in the triangular flask of 50ml, ultrasonic processing 20min, leaves standstill clarification,Get supernatant as need testing solution;
(2) another extracting honeysuckle control medicinal material 0.5g, is made in the same way of control medicinal material solution with need testing solution;
(3) get again chlorogenic acid reference substance, add methyl alcohol and make the solution of every 1ml containing 0.5mg, product solution in contrast;
(4) according to " Chinese pharmacopoeia " 2010 editions one thin-layered chromatography annex VI B test, draw respectively need testing solution, contrastMedicinal material solution, the each 5ul of reference substance solution, put on same silica gel H plate, uses butyl acetate, formic acid, water 7:2.5 by volume:2.5 upper solution is launched as solvent, takes out, and dries, and under the ultraviolet lamp that is 365nm, inspects at wavelength; Test sample lookIn spectrum, with control medicinal material chromatogram and the corresponding position of reference substance chromatogram on, the fluorescence spot of aobvious same color.
The present invention compared with prior art, has obvious beneficial effect, as can be known from the above technical solutions: provided by the present inventionThe quality determining method of Antibicrobial anti inflammatory capsule, original standard not to prescription in any effective ingredient carry out qualitativeIn the situation of quantitative monitoring, adopt with the root of large-flowered skullcap index composition root of large-flowered skullcap in high effective liquid chromatography for measuring Antibicrobial anti inflammatory capsuleThe quality control of glycosides, the thin layer that has increased honeysuckle, the tuber of stemona, rheum officinale, the root of large-flowered skullcap, the wind-weed differentiates, quantitatively detect accuracy high, measureContent is accurate, and qualitative discriminating specificity is strong, identification result is clear, simple, energy effective control for product quality; The present invention can haveEffect is controlled the quality of this Chinese medicinal capsule, ensures the security of medication, thereby guarantees its clinical efficacy.
Brief description of the drawings
Fig. 1: Antibicrobial anti inflammatory capsule solvent high-efficiency liquid chromatogram;
Fig. 2: Antibicrobial anti inflammatory capsule lacks the negative high-efficient liquid phase chromatogram of the root of large-flowered skullcap;
Fig. 3: Antibicrobial anti inflammatory capsule sample high-efficient liquid phase chromatogram;
Fig. 4: Antibicrobial anti inflammatory capsule scutelloside reference substance high-efficient liquid phase chromatogram;
Fig. 5: scutelloside linear graph.
Detailed description of the invention
Further illustrate beneficial effect of the present invention below by experimental example and embodiment.
Experimental example: content determination of Baicalin
(1) selection of mobile phase:
Mobile phase 1: acetonitrile-1% glacial acetic acid (25: 75);
Mobile phase 2: acetonitrile-1% glacial acetic acid (20: 80);
Mobile phase 3: acetonitrile-0.02% phosphoric acid (25: 75);
Mobile phase 4: methanol-water-glacial acetic acid (53: 47: 1)
Mobile phase 5: methanol-water-glacial acetic acid (53: 47: 3)
By the analysis of above comparative test result, it is suitable that mobile phase 5 has retention time, effective, the negative nothing of sample separationThe features such as interference; Meanwhile, analyze and sum up according to follow-up test, the theoretical cam curve of sample is between 2000-9000 scope, thereforeThe theoretical cam curve of regulation scutelloside is not less than 2000.
(2) need testing solution preparation method screening:
In this product, the root of large-flowered skullcap is that primary medicinal powder adds, and adopts respectively 50% methyl alcohol, 70% methyl alcohol, 50% ethanol, 70% ethanol to extractMethod screening, 70% alcohol extract best results. That is: get this product fine powder 0.25g, accurately weighed, precision adds 70% ethanol25ml, weighed weight, adds hot reflux 3 hours, lets cool, more weighed weight, supplies the weight of less loss with 70% ethanol, shakes up filterCross, precision measures filtrate 2ml, puts in 10ml volumetric flask, adds methyl alcohol to scale, shakes up, and to obtain final product;
(3) mensuration of negative control experiment and solvent peak:
Get and lack the negative preparation of the root of large-flowered skullcap, according to need testing solution, be made in the same way of and lack root of large-flowered skullcap negative control product solution. Get respectively methyl alcohol, lackThe each 10 μ l of root of large-flowered skullcap negative control product, test sample and reference substance solution, injection liquid chromatography, the results are shown in Figure 1,2,3,4.
Above result of the test shows: negative control solution with reference substance, the corresponding position of test sample chromatographic peak on noiseless, sideMethod is feasible.
(4) linear relationship is investigated:
Precision measures scutelloside reference substance solution (0.01,0.02,0.04,0.08,0.16mg/ml) the 10 μ l notes of variable concentrationsEnter liquid chromatograph, carry out scutelloside mensuration, with scutelloside peak area, A carries out linear regression, linearity to Determination of baicalin CRegression equation: A=43887599.5x-4893.8, the range of linearity: 0.1-1.6 μ g, correlation coefficient r=0.9999, matchingCross former point equation A=43843110.7C, enter full scale equation and former point equation is crossed in matching with minimum point (0.01mg/ml) peak area generation,Relative deviation is 0.63%, and because relative standard deviation is less than 1%, therefore visual full scale equation intercept levels off to zero, outside can usingMark one point method calculates content.
According to experimental result, Determination of baicalin is within the scope of 0.1-1.6 μ g, and peak area and sample size are good linearityRelation. The results are shown in following table and Fig. 5.
(5) precision test
Precision measures scutelloside reference substance solution (0.04mg/ml) 10 μ l injection liquid chromatographies, repeats sample introduction 5 times, with the root of large-flowered skullcapThe calculated by peak area of glycosides, RSD=0.70%. The results are shown in following table:
| Measure number of times | 1 | 2 | 3 | 4 | 5 | On average | RSD（%） |
| Peak area | 1753287 | 1729518 | 1756404 | 1744936 | 1732110 | 1743251 | 0.70% |
(6) replica test
Get same lot number test sample, prepare 5 parts of need testing solutions according to [assay] method, with the calculated by peak area of scutelloside,RSD=1.11%. The results are shown in following table.
(7) stability test
Precision measures same need testing solution, and according to the form below official hour sample introduction is surveyed 6 times altogether, with scutelloside calculated by peak area, and knotReally show, test sample is in 10h, and scutelloside peak area integrated value front and back are without significant change. The results are shown in following table.
(8) average recovery test
Get this product 0.125g, 6 parts, accurately weighed, precision adds scutelloside reference substance solution (0.08mg/ml) 25ml (70% methyl alcoholPreparation), weighed weight, adds hot reflux 3 hours, lets cool, more weighed weight, supplies the weight of less loss with 70% ethanol, shakes up, and filtersCross, precision measures filtrate 2ml, puts in 10ml volumetric flask, adds methyl alcohol to scale, is need testing solution, according to [assay] sideMethod, carries out content determination of Baicalin, the results are shown in following table.
Result of the test shows, application of sample average recovery rate is that 98.56%, RSD is 1.01%, reaches standard-required, and method is feasible.
(9) ten batch sample assays
Press assay operation, measure the content of baicalin of 10 lot number Antibicrobial anti inflammatory capsules and medicinal material, the results are shown in following table.
According to the assay result of ten batch samples, content of baicalin limit in Antibicrobial anti inflammatory capsule (mg/ the grain)=root of large-flowered skullcap is thrownMinimum content × average yield (%) ÷ output (g)=45g × 90mg/g of scutelloside in material amount (g) × radix scutellariae medicinal materials ×91.13% ÷ 300g=12.30mg/g, i.e. 3.69mg/ grain. According to calculating, every of this product contains the root of large-flowered skullcap with scutelloside（C21H18O11) meter should be no less than 3.7mg.
Embodiment
A quality determining method for Antibicrobial anti inflammatory capsule, described Antibicrobial anti inflammatory capsule by honeysuckle, the tuber of stemona, rheum officinale, folium isatidis,The root of large-flowered skullcap, the wind-weed and desmodium prepare, and comprise the following steps:
(1) chromatographic condition and system suitability experiment: with polarity silica gel be filler; With water, methyl alcohol, glacial acetic acid by volume51:45:2, PH=2.5 are mobile phase; Detection wavelength is 275nm; Theoretical cam curve is calculated and should be not less than 2000 by scutelloside peak;
(2) preparation of reference substance solution: it is appropriate that precision takes scutelloside reference substance, adds methyl alcohol and makes molten containing 0.04mg of every 1mlLiquid, for subsequent use;
(3) preparation of need testing solution: get this product 70 order fine powder 0.25g, accurately weighed, precision adds mass percent concentration to be60% ethanol 25ml, weighed weight, adds hot reflux 3 hours, lets cool to room temperature, more weighed weight, use mass percent concentrationBe the weight that 60% ethanol is supplied less loss, shake up, filter, precision measures filtrate 2ml, puts in 10ml volumetric flask, adds methyl alcohol extremelyScale, shakes up, for subsequent use;
(4) precision is drawn reference substance solution and the each 10 μ l of need testing solution respectively, and injection liquid chromatography is measured; Wherein, this productEvery should be no less than 3.7mg containing the root of large-flowered skullcap in scutelloside.
Wherein: the thin-layer identification method of the described tuber of stemona is:
(1) take this product content 2g, add ammonia solution 2ml, chloroform 20ml, ultrasonic processing 30min, takes out, and filters, and filtrate is wavedDry, it is 2% hydrochloric acid solution 1ml that residue adds mass percent concentration, is stirred to dissolve, and supernatant is put in test tube, uses concentrated ammonia liquorRegulating pH is 9, adds 0.5ml chloroform, shake well, and stratification, gets chloroform layer as need testing solution;
(2) separately get tuber of stemona control medicinal material 0.1g, add ammonia solution 0.1ml, chloroform 1ml, ultrasonic processing 20min, gets chloroform solution conductControl medicinal material solution;
(3) according to " Chinese pharmacopoeia " 2010 editions one thin-layered chromatography annex VI B test, draw respectively need testing solution and rightAccording to the each 2.5 μ l of medicinal material solution, put on same silica gel g thin-layer plate, taking toluene, ethyl acetate, chloroform by volume 2:8:2 as exhibitionOpen agent, launch, take out, dry, iodine colour developing; In test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, aobvious identical faceColor spot point.
The thin-layer identification method of described rheum officinale is:
(1) take this product content 0.5g, put in tool plug test tube, add ethanol 1ml, ultrasonic processing 30min, takes out, and stirs evenly, and leaves standstillClarification, gets supernatant as need testing solution;
(2) separately get rheum officinale control medicinal material 0.05g, be made in the same way of control medicinal material solution with need testing solution;
(3) according to " Chinese pharmacopoeia " 2010 editions one thin-layered chromatography annex VI B test, draw respectively need testing solution and rightAccording to the each 5 μ l of medicinal material solution, put on same silica gel g thin-layer plate, taking toluene, ethyl acetate, formic acid by volume 8:1:0.1 as exhibitionOpen agent, launch, take out, dry, put under the ultraviolet lamp that wavelength is 365nm and inspect; In test sample chromatogram, with control medicinal material lookCompose on corresponding position, aobvious same color fluorescence spot.
The thin layer of the described root of large-flowered skullcap is differentiated:
(1) get this product capsule 's content 1g, in the triangular flask of 50ml, add the ultrasonic processing of methyl alcohol 10ml 10min, leave standstill clarification, getSupernatant is as need testing solution;
(2) separately get root of large-flowered skullcap control medicinal material 0.5g, be made in the same way of control medicinal material solution with need testing solution;
(3) get again scutelloside reference substance, add methyl alcohol and make the solution of every 1ml containing 0.5mg, product solution in contrast;
(4) according to " Chinese pharmacopoeia " 2010 editions one thin-layered chromatography annex VI B test, draw respectively need testing solution, contrastMedicinal material solution, the each 5ul of reference substance solution, put on same polyamide film, and the glacial acetic acid that is 35% with mass percent concentration is doneFor solvent, launch, take out, dry, the ferric trichloride ethanolic solution of spray taking mass percent concentration as 5%, makes spot colour developing clearClear; In test sample chromatogram, with control medicinal material chromatogram and the corresponding position of reference substance chromatogram on, aobvious same color spot.
The thin layer of the described wind-weed is differentiated:
(1) get this product capsule 's content 1g, in the triangular flask of 50ml, add mass percent concentration and be 25% acetone 10ml, superSound 30min, leaves standstill clarification, gets supernatant as need testing solution;
(2) separately getting rhizoma anemarrhenae saponin BII reference substance, to add mass percent concentration be that 25% acetone is made molten containing 0.5mg of every 1mlLiquid, in contrast product solution;
(3) according to " Chinese pharmacopoeia " 2010 editions one thin-layered chromatography annex VI B test, draw respectively need testing solution and rightAccording to the each 5ul of product solution, put on same silica G plate, with n-butanol, glacial acetic acid, the water upper solution conduct of 4:1:5 by volumeSolvent launches, and takes out, and dries, and the phosphomolybdic acid ethanol solution of spray taking mass percent concentration as 5%, puts into the baking oven of 105 DEG C,Until spot clear display; In test sample chromatogram, with the corresponding principal spot of reference substance chromatogram position on, aobvious same color spotPoint.
The thin layer of described honeysuckle is differentiated:
(1) get this product capsule 's content 1g, add methyl alcohol 10ml in the triangular flask of 50ml, ultrasonic processing 20min, leaves standstill clarification,Get supernatant as need testing solution;
(2) another extracting honeysuckle control medicinal material 0.5g, is made in the same way of control medicinal material solution with need testing solution;
(3) get again chlorogenic acid reference substance, add methyl alcohol and make the solution of every 1ml containing 0.5mg, product solution in contrast;
(4) according to " Chinese pharmacopoeia " 2010 editions one thin-layered chromatography annex VI B test, draw respectively need testing solution, contrastMedicinal material solution, the each 5ul of reference substance solution, put on same silica gel H plate, uses butyl acetate, formic acid, water 7:2.5 by volume:2.5 upper solution is launched as solvent, takes out, and dries, and under the ultraviolet lamp that is 365nm, inspects at wavelength; Test sample lookIn spectrum, with control medicinal material chromatogram and the corresponding position of reference substance chromatogram on, the fluorescence spot of aobvious same color.
Method of operating is constant, by the chromatographic condition in aforementioned Antibicrobial anti inflammatory capsule quality determining method and system suitability experimentThe volume ratio of water, methyl alcohol, glacial acetic acid is adjusted into 55:49:5 or 53:47:3.5, PH and is adjusted into 3.5 or 3, detects wavelength and be adjusted into285nm or 280nm, the segmentation granularity in need testing solution preparation is adjusted into the mass percent concentration of 90 orders or 80 orders, ethanolBe adjusted into 80% or 70%, all can realize scutelloside and detect, reach quality testing object of the present invention;
Method of operating is constant, by the mass percent concentration of hydrochloric acid solution in aforementioned tuber of stemona thin-layer identification method be adjusted into 5% or3.5%, the PH of concentrated ammonia liquor is adjusted into 11 or 10, the sampling amount of need testing solution and control medicinal material solution is adjusted into 5 μ l or 3.5 μ l,Also can realize the thin layer of the tuber of stemona differentiates;
Method of operating is constant, the scutelloside reference substance in aforementioned Radix Astragali thin-layer identification method is added to methyl alcohol and make every 1ml containing 1.0mgOr the mass percent concentration of the solution of 7.5mg, glacial acetic acid is adjusted into 37% or 36%, the quality percentage of ferric trichloride ethanolic solutionSpecific concentration is adjusted into 10% or 7.5%, also can realize the thin layer of the Radix Astragali and differentiate;
Method of operating is constant, by the mass percent concentration of acetone in wind-weed thin-layer identification method be adjusted into 35% or 30%, phosphorus molybdenumThe mass percent concentration of acid ethanolic solution is adjusted into 10% or 7.5%, the temperature of baking oven is adjusted into 110 DEG C or 107 DEG C, also can be realThe thin layer of the existing wind-weed is differentiated.
The above, be only preferred embodiment of the present invention, not the present invention made to any pro forma restriction, Ren HeweiDisengaging technical solution of the present invention content, any simple modification of above embodiment being done according to technical spirit of the present invention, etc.With changing and modifying, all still belong in the scope of technical solution of the present invention.
Claims (6)
1. a quality determining method for Antibicrobial anti inflammatory capsule, described Antibicrobial anti inflammatory capsule is by honeysuckle, the tuber of stemona, rheum officinale, smaltLeaf, the root of large-flowered skullcap, the wind-weed and desmodium prepare, and comprise the following steps:
The experiment of chromatographic condition and system suitability: with polarity silica gel be filler; With water, methyl alcohol, glacial acetic acid 51-by volume55:45-49:2-5, PH=2.5-3.5 are mobile phase; Detection wavelength is 275-285nm; Theoretical cam curve is pressed scutelloside peak and is calculatedShould be not less than 2000;
(2) preparation of reference substance solution: it is appropriate that precision takes scutelloside reference substance, adds methyl alcohol and makes molten containing 0.04mg of every 1mlLiquid, for subsequent use;
(3) preparation of need testing solution: get this product 70-90 order fine powder 0.25g, accurately weighed, precision adds mass percent denseDegree is the ethanol 25ml of 60-80%, and weighed weight, adds hot reflux 3 hours, let cool to room temperature, more weighed weight, use quality percentageSpecific concentration is the weight that the ethanol of 60-80% is supplied less loss, shakes up, and filters, and precision measures filtrate 2ml, put in 10ml volumetric flask,Add methyl alcohol to scale, shake up, for subsequent use;
(4) precision is drawn reference substance solution and the each 10 μ l of need testing solution respectively, and injection liquid chromatography is measured; Wherein, this productEvery should be no less than 3.7mg containing the root of large-flowered skullcap in scutelloside.
2. the quality determining method of a kind of Antibicrobial anti inflammatory capsule as claimed in claim 1, wherein: the thin layer of the described tuber of stemona is differentiatedMethod is:
(1) take this product content 2g, add ammonia solution 2ml, chloroform 20ml, ultrasonic processing 30min, takes out, and filters, and filtrate is wavedDry, residue adds the hydrochloric acid solution 1ml that mass percent concentration is 2-5%, is stirred to dissolve, and supernatant is put in test tube, uses dense ammoniaIt is 9-11 that water regulates pH, adds 0.5ml chloroform, shake well, and stratification, gets chloroform layer as need testing solution;
(2) separately get tuber of stemona control medicinal material 0.1g, add ammonia solution 0.1ml, chloroform 1ml, ultrasonic processing 20min, gets chloroform solution conductControl medicinal material solution;
(3) according to " Chinese pharmacopoeia " 2010 editions one thin-layered chromatography annex VI B test, draw respectively need testing solution and rightAccording to the each 2.5-5 μ of medicinal material solution l, put on same silica gel g thin-layer plate, taking toluene, ethyl acetate, chloroform by volume 2:8:2 asSolvent, launches, and takes out, and dries iodine colour developing; In test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, aobvious identicalColor spot.
3. the quality determining method of a kind of Antibicrobial anti inflammatory capsule as claimed in claim 1, wherein: the thin layer of described rheum officinale is differentiatedMethod is:
Take this product content 0.5g, put in tool plug test tube, add ethanol 1ml, ultrasonic processing 30min, takes out, and stirs evenly, and leaves standstill clearGet supernatant as need testing solution clearly;
(2) separately get rheum officinale control medicinal material 0.05g, be made in the same way of control medicinal material solution with need testing solution;
(3) according to " Chinese pharmacopoeia " 2010 editions one thin-layered chromatography annex VI B test, draw respectively need testing solution and rightAccording to the each 5 μ l of medicinal material solution, put on same silica gel g thin-layer plate, taking toluene, ethyl acetate, formic acid by volume 8:1:0.1 as exhibitionOpen agent, launch, take out, dry, put under the ultraviolet lamp that wavelength is 365nm and inspect; In test sample chromatogram, with control medicinal material lookCompose on corresponding position, aobvious same color fluorescence spot.
4. the quality determining method of a kind of Antibicrobial anti inflammatory capsule as claimed in claim 1, wherein: the thin layer mirror of the described root of large-flowered skullcapOther:
Get this product capsule 's content 1g, in the triangular flask of 50ml, add the ultrasonic processing of methyl alcohol 10ml 10min, leave standstill clarification, getClear liquid is as need testing solution;
Separately get root of large-flowered skullcap control medicinal material 0.5g, be made in the same way of control medicinal material solution with need testing solution;
Get again scutelloside reference substance, add methyl alcohol and make the solution of every 1ml containing 0.5-1.0mg, product solution in contrast;
(4) according to " Chinese pharmacopoeia " 2010 editions one thin-layered chromatography annex VI B test, draw respectively need testing solution, contrastMedicinal material solution, the each 5ul of reference substance solution, put on same polyamide film, the ice vinegar that is 35-37% with mass percent concentrationAcid, as solvent, launches, and takes out, and dries, and the ferric trichloride ethanolic solution of spray taking mass percent concentration as 5-10%, makes spotPoint colour developing is clear; In test sample chromatogram, with control medicinal material chromatogram and the corresponding position of reference substance chromatogram on, aobvious same color spotPoint.
5. the quality determining method of a kind of Antibicrobial anti inflammatory capsule as claimed in claim 1, wherein: the thin layer mirror of the described wind-weedOther:
Get this product capsule 's content 1g, in the triangular flask of 50ml, adding mass percent concentration is the acetone 10ml of 25-35%, superSound 30min, leaves standstill clarification, gets supernatant as need testing solution;
Separately getting rhizoma anemarrhenae saponin BII reference substance, to add mass percent concentration be that the acetone of 25-35% is made molten containing 0.5mg of every 1mlLiquid, in contrast product solution;
(3) according to " Chinese pharmacopoeia " 2010 editions one thin-layered chromatography annex VI B test, draw respectively need testing solution and rightAccording to the each 5ul of product solution, put on same silica G plate, with n-butanol, glacial acetic acid, the water upper solution conduct of 4:1:5 by volumeSolvent launches, and takes out, and dries, and the phosphomolybdic acid ethanol solution of spray taking mass percent concentration as 5-10%, puts into 105-110 DEG CBaking oven, until spot clear display; In test sample chromatogram, with the corresponding principal spot of reference substance chromatogram position on, aobvious identicalColor spot.
6. the quality determining method of a kind of Antibicrobial anti inflammatory capsule as claimed in claim 1, wherein: the thin layer mirror of described honeysuckleOther:
Get this product capsule 's content 1g, add methyl alcohol 10ml in the triangular flask of 50ml, ultrasonic processing 20min, leaves standstill clarification, getsSupernatant is as need testing solution;
Another extracting honeysuckle control medicinal material 0.5g, is made in the same way of control medicinal material solution with need testing solution;
Get again chlorogenic acid reference substance, add methyl alcohol and make the solution of every 1ml containing 0.5mg, product solution in contrast;
According to " Chinese pharmacopoeia " 2010 editions one thin-layered chromatography annex VI B test, draw respectively need testing solution, contrast medicineMaterial solution, the each 5ul of reference substance solution, put on same silica gel H plate, with butyl acetate, formic acid, water 7:2.5:2.5 by volumeUpper solution launch as solvent, take out, dry, under the ultraviolet lamp that is 365nm at wavelength, inspect; Test sample chromatogramIn, with control medicinal material chromatogram and the corresponding position of reference substance chromatogram on, the fluorescence spot of aobvious same color.
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| CN107045021A (en) * | 2017-01-19 | 2017-08-15 | 山东省食品药品检验研究院 | It is a kind of at the same differentiate anti-inflammation piece in honeysuckle, radix scutellariae and the wind-weed detection method |
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| CN109771596A (en) * | 2019-03-25 | 2019-05-21 | 广东在田药业有限公司 | A kind of Antibicrobial anti inflammatory capsule and preparation method thereof |
| CN109771596B (en) * | 2019-03-25 | 2021-07-20 | 广东在田药业股份有限公司 | Antibacterial and anti-inflammatory capsule and preparation method thereof |
| CN110031588A (en) * | 2019-03-26 | 2019-07-19 | 浙江金大康动物保健品有限公司 | An a kind of quick thin-layer identification method of plate multiple medicine taste of livestock and poultry antiviral granule |
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