CN102608250B - Rapid detection method for Jinfangganmao granules - Google Patents
Rapid detection method for Jinfangganmao granules Download PDFInfo
- Publication number
- CN102608250B CN102608250B CN201210063430.9A CN201210063430A CN102608250B CN 102608250 B CN102608250 B CN 102608250B CN 201210063430 A CN201210063430 A CN 201210063430A CN 102608250 B CN102608250 B CN 102608250B
- Authority
- CN
- China
- Prior art keywords
- solution
- methyl alcohol
- reference substance
- paracetamol
- chlorogenic acid
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Landscapes
- Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)
- Investigating Or Analysing Biological Materials (AREA)
Abstract
The invention relates to a rapid detection method for Jinfangganmao granules. The rapid detection method for the Jinfangganmao granules is characterized in that: the identification on paracetamol, ledebouriella root and chlorogenic acid is realized on the same thin-layer plates by adopting a thin-layer chromatography (TLC) and using the same testing solution; the fluorescent identification on the ledebouriella root is reported for the first time; the ordinary isocratic elution is adopted, a mixture of acetonitrile, carbinol and 0.1% phosphoric acid which are in a volume ratio of (5.5-6.5):(5-4.5):(90-89.5) is taken as a mobile phase, and the contents of the paracetamol and the chlorogenic acid in a sample are simultaneously determined at the position of 295+/-1 nm, so that the determined indicators which are originally finished through twice quantitative determination can be finished by using once quantitative determination; and the quantitative chromatograms of the two ingredients are excellent in crest separation, the crest retention time for the paracetamol is about 7 minutes, and the crest retention time for the chlorogenic acid is about 15 minutes. The rapid detection method has the advantages of simplicity, convenience, rapidness, accuracy, repeatability and easiness in popularization and grasping, the detection efficiency is effectively increased, the detection cost is lowered, and the environmental pollution is reduced.
Description
Technical field
The present invention relates to a kind of method for quick of Jinfanggnmao Granules.
Background technology
Jinfanggnmao Granules (Sugarless type) is for there being sugared type to change drug specifications kind, and former specification is every bag of 15g, once a bag, 3 times on the one, after changing into Sugarless type, every bag of 5g, once a bag, 3 times on the one.Every day to take crude drug amount constant, but taking dose significantly reduces, and is applicable to diabetic to take.Jinfanggnmao Granules prescription composition and the method for making of Sugarless type are as follows:
The windproof 233.1g hawthorn of [prescription] mountain honeysuckle flower 233.1g 233.1g ginger 233.1g paracetamol 56.1g
[method for making] above five kinds of Chinese medicine, gets mountain honeysuckle flower, windproof, hawthorn, adds 8 times of water gagings and decocts secondary, each 1.5 hours, collecting decoction, filters, and filtrate is concentrated into the clear cream that relative density is 1.05～1.10 (50 DEG C), let cool, add ethanol and make to reach 60% containing alcohol amount, stir evenly, leave standstill 24 hours, filter, filtrate recycling ethanol is also concentrated into the thick paste that relative density is 1.30～1.35 (50 DEG C); Ginger is thinly sliced, and adds 5 times of amount alcohol dipping three times, and each 24 hours, merge maceration extract, filter, decompression filtrate recycling ethanol is also concentrated into the thick paste that relative density is 1.30～1.35 (50 DEG C); Get paracetamol, the mode of progressively increasing with equivalent and Steviosin 18g, dextrin 780g～800g, after mixing, add above-mentioned thick paste, stirs evenly, with alcohol granulation, dry, makes 1000g, to obtain final product.
By the Jinfanggnmao Granules prescription of sugared type form and method for making as follows:
The windproof 77.7g hawthorn of [prescription] mountain honeysuckle flower 77.7g 77.7g ginger 77.7g paracetamol 18.7g
[method for making] above five kinds of Chinese medicine, gets mountain honeysuckle flower, windproof, hawthorn, adds 8 times of water gagings and decocts secondary, each 1.5 hours, collecting decoction, filters, and filtrate is concentrated into the clear cream that relative density is 1.05～1.10 (50 DEG C), let cool, add ethanol and make to reach 60% containing alcohol amount, stir evenly, leave standstill 24 hours, filter, filtrate recycling ethanol is also concentrated into the thick paste that relative density is 1.30～1.35 (50 DEG C); Ginger is thinly sliced, and adds 5 times of amount alcohol dipping three times, and each 24 hours, merge maceration extract, filter, decompression filtrate recycling ethanol is also concentrated into the thick paste that relative density is 1.30～1.35 (50 DEG C); Paracetamol, adds 83% ethanol and makes to dissolve, and adds above-mentioned thick paste and sucrose, stir evenly, and granulation 1000g, dry, to obtain final product.
Original sugared type quality standard is recorded in national standard for traditional Chinese medicines compilation internal medicine lung system (), and standard No. is: WS-11474 (ZD-1474) 2002.Prescription is made up of honeysuckle, windproof, hawthorn, ginger, paracetamol.Chinese Pharmacopoeia Commission in 2011, has carried out to standard the revision of becoming a full member, and in May, 2011 in online publicity, in the revised draft of becoming a full member by prescription in honeysuckle be changed to mountain honeysuckle flower; Chlorogenic Acid of Flos Lonicerae assay is changed to mountain honeysuckle flower Content of Chlorogenic Acid and measures, and is acetonitrile-water-phosphoric acid (11: 89: 0.04) by acetonitrile-water-phosphoric acid (50: 400: 0.2) specification writing, and other are all unchanged.Revised standard number is: WS-11474 (ZD-1474) 2002-2011Z.
That primary standard has been recorded is windproof, the assay of the discriminating of chlorogenic acid thin layer and chlorogenic acid and paracetamol.Differentiate for two and need 2 kinds of need testing solutions, on two blocks of thin layer plates, adopt two kinds of developping agents, launched respectively, toxic solvents consumption is large, time-consuming length, contaminated environment; The assay of chlorogenic acid and paracetamol, although mobile phase is identical, detects wavelength different with Sample Dilution multiple, must complete by 2 high efficiency liquid phases.Because under the detection wavelength 326nm of chlorogenic acid, paracetamol is without absorbing (seeing Fig. 1), and under the detection wavelength 244nm of paracetamol, and the crest of chlorogenic acid very little (seeing Fig. 2).
The method for quick of Jinfanggnmao Granules of the present invention, is on the basis of differentiating at original windproof and chlorogenic acid thin layer, by windproof fat-soluble distinctive compound, be changed to water soluble ingredient according to operational characteristic, and first passage increasing fluorescence is differentiated; Increased the discriminating of paracetamol simultaneously; Three ultrasonic sample solutions of same methyl alcohol for discriminating complete on two blocks of thin layer plates.Paracetamol and windproofly (see Fig. 3,4) on a thin layer plate, chlorogenic acid is on another piece thin layer plate (seeing Fig. 5).Select chlorogenic acid and paracetamol to have the 295nm (seeing Fig. 6,7,8) of absorption for detecting wavelength, by the chlorogenic acid in primary standard and paracetamol single quantitative measurement separately, combine Simultaneous Determination, and former mobile phase is carried out to restructuring research, solve former chromatographic column durability undesirable, the coated impurity peaks problem of crest of part chromatographic column paracetamol, has improved specificity and the accuracy of quantitative measurement.
Summary of the invention
The present invention is directed to the quality determining method of current Chinese medicine, sample pre-treatments is more loaded down with trivial details, time-consuming, murder by poisoning solvent load is large, environmental pollution is serious, the present situation that detection speed cannot match with the large production of mechanization, invent and adopted the ultrasonic need testing solution of same methyl alcohol and each control medicinal material solution, on 2 blocks of thin layer plates, the thin layer that completes paracetamol, windproof and chlorogenic acid is differentiated.Three thin layers are differentiated, only need sample 2g, extract solvent 10ml, 10 minutes time.And by the mode of isocratic elution, paracetamol and chlorogenic acid have been measured at 295nm simultaneously.Make the testing index that originally second metering has been measured, can complete with quantitative measurement once.Reduce cost, saved the time, improved efficiency.The quantitative chromatogram of binary, crest separates good, and the crest retention time of paracetamol is about 7 minutes, and the crest retention time of chlorogenic acid is about 15 minutes.
According to extraction process feature, the present invention has created the thin-layer identification method of windproof water soluble ingredient increasing fluorescence, has widened windproof discriminating scope.
Water-soluble much larger than fat-soluble character according to paracetamol and chlorogenic acid, pass through Data Comparison, by former extraction solvent absolute ethyl alcohol, be changed to 70% methyl alcohol, make the content of chlorogenic acid improve approximately 30%, measure the real content (in table 1) that numerical value is tending towards sample, effectively improved the accuracy of method.
By methodological study, chlorogenic acid sample size is at 0.0926～0.926 μ g, is good linear relationship with peak area, and regression equation is: Y=2931322.4X-5113, γ=0.999999 (in table 2, Fig. 9); Paracetamol sample size is at 0.9576～9.576 μ g, is good linear relationship with peak area, and regression equation is: Y=271998.7X+18054, γ=0.99997 (in table 3, Figure 10).Adopt application of sample recovery experiment, result shows: the average recovery rate that paracetamol is measured for 9 times is that 99.76%, RSD is 1.17% (in table 4); The average recovery rate that chlorogenic acid is measured for 9 times is that 98.97%, RSD is 1.95% (in table 5).Precision (in table 6), stability (in table 7), repeatability (in table 8), specificity (seeing Figure 11,12,13) all meet methodology requirement with post durability (in table 9, Figure 14,15,16) experiment.Be applicable to the Simultaneous Determination of paracetamol and chlorogenic acid in Jinfanggnmao Granules.
The technical solution adopted for the present invention to solve the technical problems is:
(1) quick thin-layer identification method
1. get Jinfanggnmao Granules 2～4g, add methyl alcohol 5ml, ultrasonic processing 10 minutes, filters, and filtrate is as need testing solution.Separately get paracetamol reference substance, add methyl alcohol and make the solution of every 1ml containing 5mg, product solution in contrast; Get again windproof control medicinal material 0.3g, add methyl alcohol 3ml, ultrasonic processing 10 minutes, supernatant is medicinal material solution in contrast; Draw each 4～8 μ l of above-mentioned three kinds of solution, put respectively on same silica GF254 thin layer plate, taking volume ratio as 10～12: 2～1: 4～2: methenyl choloride-ethyl acetate-methyl alcohol-dense ammonia of 1～0.5 is developping agent, launch, take out, dry, put under ultraviolet lamp 254nm and inspect, in test sample chromatogram, with the corresponding position of reference substance chromatogram on, aobvious same color spot; Spray with 10% ethanol solution of sulfuric acid, 105 DEG C of bakings 1～2 minute, put under ultraviolet lamp 365nm and inspect again, in test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, aobvious identical bright blue look fluorescence principal spot;
2. get chlorogenic acid reference substance, add methyl alcohol and make the solution of every 1ml containing 2mg, product solution in contrast; Draw reference substance solution 5 μ l and differentiate 1. under need testing solution 2～5 μ l, put respectively on same silica gel g thin-layer plate, taking volume ratio as 15～13: 5～3: the upper solution of butyl acetate-formic acid-water of 5～3 is developping agent, launch, take out hot blast drying, put under ultraviolet lamp 365nm and inspect, in test sample chromatogram, with the corresponding position of reference substance chromatogram on, aobvious same color fluorescence spot;
(2). chlorogenic acid and paracetamol Simultaneous Determination method
A. chromatographic condition and system suitability are taking octadecylsilane chemically bonded silica as filling agent; Taking volume ratio as 5.5～6.5: 5～4.5: 90～89.5 acetonitrile-methyl alcohol-0.1% phosphoric acid is mobile phase; Detection wavelength is 295nm; Number of theoretical plate calculates and should be not less than 3000 by chlorogenic acid peak;
B. reference substance solution preparation is got chlorogenic acid with paracetamol reference substance is appropriate, accurately weighed, adds methyl alcohol and makes every 1ml and contain chlorogenic acid 0.02mg, and the solution of paracetamol 0.45mg, to obtain final product;
C. Jinfanggnmao Granules 5g is got in need testing solution preparation, and porphyrize, gets 0.2～0.6g, accurately weighed, to put in tool plug conical flask, precision adds 70% methyl alcohol 25ml, weighed weight, with power 250w, frequency 50kHz, ultrasonic processing 10 minutes, let cool, weighed weight again, supplies the weight of less loss with 70% methyl alcohol, shake up, filter, to obtain final product;
D. determination method accurate reference substance solution and the each 5 μ l of need testing solution of drawing respectively, injection liquid chromatography, measures, and to obtain final product;
Every bag of this product containing mountain honeysuckle flower with chlorogenic acid C
16h
18o
9meter, must not be less than 10.0mg; Containing paracetamol C
8h
9nO
2should be 90.0%～110.0% of labelled amount.
For the preferred determination techniques scheme of sucrose free Jinfanggnmao Granules be:
(1) quick thin-layer identification method
1. get sucrose free Jinfanggnmao Granules 2g, add methyl alcohol 5ml, ultrasonic processing 10 minutes, filters, and filtrate is as need testing solution; Separately get paracetamol reference substance, add methyl alcohol and make the solution of every 1ml containing 5mg, product solution in contrast; Get again windproof control medicinal material 0.3g, add methyl alcohol 3ml, ultrasonic processing 10 minutes, supernatant is medicinal material solution in contrast; Draw the each 4 μ l of above-mentioned three kinds of solution, put respectively in same silica G F
254on thin layer plate, taking volume ratio as 10: 2: 4: methenyl choloride-ethyl acetate-methyl alcohol-dense ammonia of 1 is developping agent, launch, take out, dry, put under ultraviolet lamp 254nm and inspect, in test sample chromatogram, with the corresponding position of reference substance chromatogram on, aobvious same color spot; Spray with 10% ethanol solution of sulfuric acid, 105 DEG C of bakings 1～2 minute, put under ultraviolet lamp 365nm and inspect again, in test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, aobvious identical bright blue look fluorescence principal spot;
2. get chlorogenic acid reference substance, add methyl alcohol and make the solution of every 1ml containing 2mg, product solution in contrast; Draw reference substance solution 5 μ l and differentiate 1. under need testing solution 2～5 μ l, put respectively on same silica gel g thin-layer plate, upper solution taking volume ratio as the butyl acetate-formic acid-water of 15: 5: 5 is as developping agent, launch, take out hot blast drying, put under ultraviolet lamp 365nm and inspect, in test sample chromatogram, with the corresponding position of reference substance chromatogram on, aobvious same color fluorescence spot;
(2). chlorogenic acid and paracetamol Simultaneous Determination method
A. chromatographic condition and system suitability are taking octadecylsilane chemically bonded silica as filling agent; Taking volume ratio as acetonitrile-methyl alcohol-0.1% phosphoric acid of 5.5: 4.5: 90 is as mobile phase; Detection wavelength is 295nm; Number of theoretical plate calculates and should be not less than 3000 by chlorogenic acid peak;
B. reference substance solution preparation is got chlorogenic acid with paracetamol reference substance is appropriate, accurately weighed, adds methyl alcohol and makes every 1ml and contain chlorogenic acid 0.02mg, and the solution of paracetamol 0.45mg, to obtain final product;
C. sucrose free Jinfanggnmao Granules 5g is got in need testing solution preparation, and porphyrize, gets 0.2g, accurately weighed, to put in tool plug conical flask, precision adds 70% methyl alcohol 25ml, weighed weight, with power 250w, frequency 50kHz, ultrasonic processing 10 minutes, let cool, weighed weight again, supplies the weight of less loss with 70% methyl alcohol, shake up, filter, to obtain final product;
D. determination method accurate reference substance solution and the each 5 μ l of need testing solution of drawing respectively, injection liquid chromatography, measures, and to obtain final product;
Every bag of this product containing mountain honeysuckle flower with chlorogenic acid C
16h
18o
9meter, must not be less than 10.0mg; Containing paracetamol C
8h
9nO
2should be 90.0%～110.0% of labelled amount.
For the preferred determination techniques scheme of Jinfanggnmao Granules containing sucrose be:
(1) quick thin-layer identification method
1. get the Jinfanggnmao Granules 4g containing sucrose, add methyl alcohol 5ml, ultrasonic processing 10 minutes, filters, and filtrate is as need testing solution; Separately get paracetamol reference substance, add methyl alcohol and make the solution of every 1ml containing 5mg, product solution in contrast; Get again windproof control medicinal material 0.3g, add methyl alcohol 3ml, ultrasonic processing 10 minutes, supernatant is medicinal material solution in contrast; Draw reference substance solution and the each 4 μ l of control medicinal material solution, need testing solution 8 μ l, put respectively in same silica G F
254on thin layer plate, taking volume ratio as 12: 1.5: 4: methenyl choloride-ethyl acetate-methyl alcohol-dense ammonia of 0.5 is developping agent, launch, take out, dry, put under ultraviolet lamp 254nm and inspect, in test sample chromatogram, with the corresponding position of reference substance chromatogram on, aobvious same color spot; Spray with 10% ethanol solution of sulfuric acid, 105 DEG C of bakings 1～2 minute, put under ultraviolet lamp 365nm and inspect again, in test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, aobvious identical bright blue look fluorescence principal spot;
2. get chlorogenic acid reference substance, add methyl alcohol and make the solution of every 1ml containing 2mg, product solution in contrast; Draw reference substance solution 5 μ l and differentiate 1. under need testing solution 2～5 μ l, put respectively on same silica gel g thin-layer plate, upper solution taking volume ratio as the butyl acetate-formic acid-water of 14: 4: 4 is as developping agent, launch, take out hot blast drying, put under ultraviolet lamp 365nm and inspect, in test sample chromatogram, with the corresponding position of reference substance chromatogram on, aobvious same color fluorescence spot;
(2). chlorogenic acid and paracetamol Simultaneous Determination method
A. chromatographic condition and system suitability are taking octadecylsilane chemically bonded silica as filling agent; Taking volume ratio as acetonitrile-methyl alcohol-0.1% phosphoric acid of 6: 4.5: 89.5 is as mobile phase; Detection wavelength is 295nm; Number of theoretical plate calculates and should be not less than 3000 by chlorogenic acid peak;
B. reference substance solution preparation is got chlorogenic acid with paracetamol reference substance is appropriate, accurately weighed, adds methyl alcohol and makes every 1ml and contain chlorogenic acid 0.02mg, and the solution of paracetamol 0.45mg, to obtain final product;
C. the Jinfanggnmao Granules 5g containing sucrose is got in need testing solution preparation, and porphyrize, gets 0.6g, accurately weighed, to put in tool plug conical flask, precision adds 70% methyl alcohol 25ml, weighed weight, with power 250w, frequency 50kHz, ultrasonic processing 10 minutes, let cool, weighed weight again, supplies the weight of less loss with 70% methyl alcohol, shake up, filter, to obtain final product;
D. determination method accurate reference substance solution and the each 5 μ l of need testing solution of drawing respectively, injection liquid chromatography, measures, and to obtain final product;
Every bag of this product containing mountain honeysuckle flower with chlorogenic acid C
16h
18o
9meter, must not be less than 10.0mg; Containing paracetamol C
8h
9nO
2should be 90.0%～110.0% of labelled amount.
Principle of the present invention is as follows:
1. by the performance of methyl alcohol solubilized polarity and nonpolar Multiple components, taking methyl alcohol as extracting solvent, extract the sample and the control medicinal material solution that obtain perfect information amount.According to effective constituent chemical constitution and polarity separately, under specific unfolding condition, utilize the attached ability of its Adsorption and desorption on thin layer plate different again, each effective constituent is separated.The approximate effective constituent of polarity like this, on same thin layer plate, different inspects under condition, can present the spot colors that Rf value is different, and for detecting without interfering with each other several compositions simultaneously.
2. all present the character of absorption in ultraviolet region according to chlorogenic acid and paracetamol, for increasing the chlorogenic acid peak area of low content, reduce the paracetamol peak area that content is high, select chlorogenic acid and paracetamol to have the 295nm of absorption as measuring wavelength, make the crest size of chlorogenic acid and paracetamol suitable, and crest area separately, in certain scope, present good linear relationship with sample size again, and for quantitative measurement.Component by mobile phase and ratio discussion again, make chlorogenic acid and paracetamol not only crest separate well, and crest retention time is suitable, the crest retention time of paracetamol approximately 7 minutes, the crest retention time of chlorogenic acid approximately 15 minutes.
Innovative point of the present invention and beneficial effect are as follows:
(1) adopt first common isocratic elution, reverse-phase chromatographic column, taking volume ratio as 5.5～6.5: 5～4.5: 90～89.5 acetonitrile-methyl alcohol-0.1% phosphoric acid is mobile phase; At 295nm place, Jinfanggnmao Granules Content of Chlorogenic Acid and Determination Paracetamol in Paracetamol have been measured simultaneously.Make the workload of 2 days originally, shorten to one day and complete, and saved mobile phase and sample preparation reagent at double.
(2) water-soluble much larger than fat-soluble character according to paracetamol and chlorogenic acid, pass through Data Comparison, methyl alcohol with 70% replaces absolute ethyl alcohol, having solved former method can not extract chlorogenic acid completely, cause measuring the problem that numerical value departs from real content, make the content of chlorogenic acid improve approximately 30%, improved the accuracy of method.
(3) the present invention adopts the means that increase fluorescence first, windproof water soluble ingredient has been carried out to TLC-Fluorescence discriminating, the novel identification method of windproof medicinal material water soluble ingredient in compound preparation is not only provided, and solved former thin layer identification beacon and water extraction process disconnection, cannot bring into play the effect of monitoring.
(4) three thin layers of the present invention are differentiated and are only needed sample 2g, and sample, control medicinal material and reference substance pre-treatment, are all that methyl alcohol is ultrasonic, easy, quick, only need methyl alcohol 10ml, 10 minutes time.Compared with differentiating with former binomial, in the situation that increasing a discriminating, also save solvent 42ml, 1.3 hours time.Make thin layer differentiate the control extraction process effect of having brought into play simultaneously.
(5) appearance of the inventive method, not merely for the fast detecting of Jinfanggnmao Granules provides method, but also is content great disparity, detects the different different compound Simultaneous Determinations of wavelength, provides Research Thinking, tool table general and exemplary role.
Brief description of the drawings
The HPLC chromatogram that Fig. 1 detects with a collection of Jinfanggnmao Granules 326nm
The HPLC chromatogram that Fig. 2 detects with a collection of Jinfanggnmao Granules 244nm
The paracetamol spot of inspecting under Figure 32 54nm
The windproof fluorescence spot that after Figure 41 0% sulfuric acid colour developing, 365nm inspects
The chlorogenic acid fluorescence spot that Figure 53 65nm inspects
The spectral scan figure of Fig. 6 paracetamol
The spectral scan figure of Fig. 7 chlorogenic acid
The HPLC chromatogram that Fig. 8 detects with a collection of Jinfanggnmao Granules 295nm
The linear relationship chart of Fig. 9 chlorogenic acid
The linear relationship chart of Figure 10 paracetamol
Figure 11 chlorogenic acid and paracetamol reference substance HPLC chromatogram
Figure 12 is Jinfanggnmao Granules HPLC chromatogram
Figure 13 is the Jinfanggnmao Granules HPLC chromatogram that does not contain paracetamol and mountain honeysuckle flower
The sample HPLC chromatogram of Figure 14 serviceability test-Shimadzu Shimadzu VP-ODS post (4.6 × 150mm)
The sample HPLC chromatogram of Figure 15 serviceability test-Di Ma dimonsil post (4.6 × 150mm)
The sample HPLC chromatogram of Figure 16 serviceability test-GraceSmart RP post (4.6 × 250mm)
Fig. 1, Fig. 2, Fig. 8, Figure 11, Figure 12, Figure 14, Figure 15, Tu16Zhong, 1 is paracetamol peak, 2 is chlorogenic acid peak
Fig. 3, Fig. 4 are same thin layer plate, Fig. 3 is the paracetamol spot of inspecting under uviol lamp 254nm, after Fig. 4 is 10% ethanol solution of sulfuric acid colour developing, the windproof increasing fluorescence spot of inspecting under uviol lamp 365nm, the sample label of Fig. 3, Fig. 4 is the same, and 1 is windproof control medicinal material, 2 is windproof blank, 3,4,5 is sample, and 6 is paracetamol, and 7 is paracetamol blank
In Fig. 5,1 is chlorogenic acid, and 2 is that blank 3.4.5 is sample
Fig. 9, Tu10Zhong, ordinate is peak area; Horizontal ordinate is that (μ g) for sample size
The specific embodiment of the invention
Embodiment 1 sucrose free Jinfanggnmao Granules method for quick
(1) quick thin-layer identification method
1. get sucrose free Jinfanggnmao Granules 2g, add methyl alcohol 5ml, ultrasonic processing 10 minutes, filters, and filtrate is as need testing solution; Separately get paracetamol reference substance, add methyl alcohol and make the solution of every 1ml containing 5mg, product solution in contrast; Get again windproof control medicinal material 0.3g, add methyl alcohol 3ml, ultrasonic processing 10 minutes, supernatant is medicinal material solution in contrast; Draw the each 4 μ l of above-mentioned three kinds of solution, put respectively in same silica G F
254on thin layer plate, taking volume ratio as 10: 2: 4: methenyl choloride-ethyl acetate-methyl alcohol-dense ammonia of 1 is developping agent, launch, take out, dry, put under ultraviolet lamp 254nm and inspect, in test sample chromatogram, with the corresponding position of reference substance chromatogram on, aobvious same color spot; Spray with 10% ethanol solution of sulfuric acid, 105 DEG C of bakings 1～2 minute, put under ultraviolet lamp 365nm and inspect again, in test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, aobvious identical bright blue look fluorescence principal spot;
2. get chlorogenic acid reference substance, add methyl alcohol and make the solution of every 1ml containing 2mg, product solution in contrast; Draw reference substance solution 5 μ l and differentiate 1. under need testing solution 2～5 μ l, put respectively on same silica gel g thin-layer plate, upper solution taking volume ratio as the butyl acetate-formic acid-water of 15: 5: 5 is as developping agent, launch, take out hot blast drying, put under ultraviolet lamp 365nm and inspect, in test sample chromatogram, with the corresponding position of reference substance chromatogram on, aobvious same color fluorescence spot;
(2). chlorogenic acid and paracetamol Simultaneous Determination method
A. chromatographic condition and system suitability are taking octadecylsilane chemically bonded silica as filling agent; Taking volume ratio as acetonitrile-methyl alcohol-0.1% phosphoric acid of 5.5: 4.5: 90 is as mobile phase; Detection wavelength is 295nm.Number of theoretical plate calculates and should be not less than 3000 by chlorogenic acid peak;
B. reference substance solution preparation is got chlorogenic acid with paracetamol reference substance is appropriate, accurately weighed, adds methyl alcohol and makes every 1ml and contain chlorogenic acid 0.02mg, and the solution of paracetamol 0.45mg, to obtain final product;
C. sucrose free Jinfanggnmao Granules 5g is got in need testing solution preparation, and porphyrize, gets 0.2g, accurately weighed, to put in tool plug conical flask, precision adds 70% methyl alcohol 25ml, weighed weight, with power 250w, frequency 50kHz, ultrasonic processing 10 minutes, let cool, weighed weight again, supplies the weight of less loss with 70% methyl alcohol, shake up, filter, to obtain final product;
D. determination method accurate reference substance solution and the each 5 μ l of need testing solution of drawing respectively, injection liquid chromatography, measures, and to obtain final product;
Every bag of this product containing mountain honeysuckle flower with chlorogenic acid C
16h
18o
9meter, must not be less than 10.0mg; Containing paracetamol C
8h
9nO
2should be 90.0%～110.0% of labelled amount.The measurement result of three batch samples is in table 10.
Embodiment 2 is containing the Jinfanggnmao Granules method for quick of sucrose
(1) quick thin-layer identification method
1. get the Jinfanggnmao Granules 4g containing sucrose, add methyl alcohol 5ml, ultrasonic processing 10 minutes, filters, and filtrate is as need testing solution; Separately get paracetamol reference substance, add methyl alcohol and make the solution of every 1ml containing 5mg, product solution in contrast; Get again windproof control medicinal material 0.3g, add methyl alcohol 3ml, ultrasonic processing 10 minutes, supernatant is medicinal material solution in contrast; Draw reference substance solution and the each 4 μ l of control medicinal material solution, need testing solution 8 μ l, put respectively in same silica G F
254on thin layer plate, taking volume ratio as 12: 1.5: 4: methenyl choloride-ethyl acetate-methyl alcohol-dense ammonia of 0.5 is developping agent, launch, take out, dry, put under ultraviolet lamp 254nm and inspect, in test sample chromatogram, with the corresponding position of reference substance chromatogram on, aobvious same color spot; Spray with 10% ethanol solution of sulfuric acid, 105 DEG C of bakings 1～2 minute, put under ultraviolet lamp 365nm and inspect again, in test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, aobvious identical bright blue look fluorescence principal spot;
2. get chlorogenic acid reference substance, add methyl alcohol and make the solution of every 1ml containing 2mg, product solution in contrast; Draw reference substance solution 5 μ l and differentiate 1. under need testing solution 2～5 μ l, put respectively on same silica gel g thin-layer plate, upper solution taking volume ratio as the butyl acetate-formic acid-water of 14: 4: 4 is as developping agent, launch, take out hot blast drying, put under ultraviolet lamp 365nm and inspect, in test sample chromatogram, with the corresponding position of reference substance chromatogram on, aobvious same color fluorescence spot;
(2). chlorogenic acid and paracetamol Simultaneous Determination method
A. chromatographic condition and system suitability are taking octadecylsilane chemically bonded silica as filling agent; Taking volume ratio as acetonitrile-methyl alcohol-0.1% phosphoric acid of 6: 4.5: 89.5 is as mobile phase; Detection wavelength is 295nm; Number of theoretical plate calculates and should be not less than 3000 by chlorogenic acid peak;
B. reference substance solution preparation is got chlorogenic acid with paracetamol reference substance is appropriate, accurately weighed, adds methyl alcohol and makes every 1ml and contain chlorogenic acid 0.02mg, and the solution of paracetamol 0.45mg, to obtain final product;
C. the Jinfanggnmao Granules 5g containing sucrose is got in need testing solution preparation, and porphyrize, gets 0.6g, accurately weighed, to put in tool plug conical flask, precision adds 70% methyl alcohol 25ml, weighed weight, with power 250w, frequency 50kHz, ultrasonic processing 10 minutes, let cool, weighed weight again, supplies the weight of less loss with 70% methyl alcohol, shake up, filter, to obtain final product.
D. determination method accurate reference substance solution and the each 5 μ l of need testing solution of drawing respectively, injection liquid chromatography, measures, and to obtain final product;
Every bag of this product containing mountain honeysuckle flower with chlorogenic acid C
16h
18o
9meter, must not be less than 10.0mg; Containing paracetamol C
8h
9nO
2should be 90.0%～110.0% of labelled amount.The measurement result of three batch samples is in table 10.
Table 1 same batch sample different solvents chlorogenic acid and Determination Paracetamol in Paracetamol result (mg/g)
Table 2 chlorogenic acid sample size and peak area
Table 3 paracetamol sample size and peak area
The recovery test result of paracetamol in table 4 sample
The recovery test result of table 5 sample Content of Chlorogenic Acid
Note: for saving reference substance, the cumulative volume of sample is not 25ml, is 15ml, in the consistent situation of concentration, sampling amount reduces.
Table 6 Precision Experiment result (peak area)
Table 7 stability experiment result
Table 8 replica test result
The content of the same sample that the different chromatographic columns of table 9 are measured
Paracetamol and determination of chlorogenic acid result in table 10 Jinfanggnmao Granules
Claims (4)
1. a method for quick for Jinfanggnmao Granules, is characterized in that:
(1) quick thin-layer identification method
1. get Jinfanggnmao Granules 2～4g, porphyrize, adds methyl alcohol 5ml, and ultrasonic processing 10 minutes filters, and filtrate is as need testing solution; Separately get paracetamol reference substance, add methyl alcohol and make the solution of every 1ml containing 5mg, product solution in contrast; Get again windproof control medicinal material 0.3g, add methyl alcohol 3ml, ultrasonic processing 10 minutes, supernatant is medicinal material solution in contrast; Draw each 4～8 μ l of above-mentioned three kinds of solution, put respectively in same silica G F
254on thin layer plate, taking volume ratio as 10～12: 2～1: 4～2: methenyl choloride-ethyl acetate-methyl alcohol-dense ammonia of 1～0.5 is developping agent, launch, take out, dry, put under ultraviolet lamp 254nm and inspect, in test sample chromatogram, with the corresponding position of reference substance chromatogram on, aobvious same color spot; Spray with 10% ethanol solution of sulfuric acid, 105 DEG C of bakings 1～2 minute, put under ultraviolet lamp 365nm and inspect again, in test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, aobvious identical bright blue look fluorescence principal spot;
2. get chlorogenic acid reference substance, add methyl alcohol and make the solution of every 1ml containing 2mg, product solution in contrast; Draw reference substance solution 5 μ l and differentiate 1. under need testing solution 2～5 μ l, put respectively on same silica gel g thin-layer plate, taking volume ratio as 15～13: 5～3: the upper solution of butyl acetate-formic acid-water of 5～3 is developping agent, launch, take out hot blast drying, put under ultraviolet lamp 365nm and inspect, in test sample chromatogram, with the corresponding position of reference substance chromatogram on, aobvious same color fluorescence spot;
(2). chlorogenic acid and paracetamol Simultaneous Determination method
A. chromatographic condition and system suitability are taking octadecylsilane chemically bonded silica as filling agent; Taking volume ratio as 5.5～6.5: 5～4.5: 90～89.5 acetonitrile-methyl alcohol-0.1% phosphoric acid is mobile phase; Detection wavelength is 295nm; Number of theoretical plate calculates and should be not less than 3000 by chlorogenic acid peak;
B. reference substance solution preparation is got chlorogenic acid with paracetamol reference substance is appropriate, accurately weighed, adds methyl alcohol and makes every 1ml and contain chlorogenic acid 0.02mg, and the solution of paracetamol 0.45mg, to obtain final product;
C. Jinfanggnmao Granules 5g is got in need testing solution preparation, and porphyrize, gets 0.2～0.6g, accurately weighed, to put in tool plug conical flask, precision adds 70% methyl alcohol 25ml, weighed weight, with power 250w, frequency 50kHz, ultrasonic processing 10 minutes, let cool, weighed weight again, supplies the weight of less loss with 70% methyl alcohol, shake up, filter, to obtain final product;
D. determination method accurate reference substance solution and the each 5 μ l of need testing solution of drawing respectively, injection liquid chromatography, measures, and to obtain final product.
2. the method for quick of a kind of Jinfanggnmao Granules according to claim 1, is characterized in that described Jinfanggnmao Granules refers to containing two kinds of the Jinfanggnmao Granules of sucrose and sucrose free Jinfanggnmao Granules.
3. the method for quick of a kind of Jinfanggnmao Granules according to claim 1, is further characterized in that:
(1) quick thin-layer identification method
1. get sucrose free Jinfanggnmao Granules 2g, porphyrize, adds methyl alcohol 5ml, and ultrasonic processing 10 minutes filters, and filtrate is as need testing solution; Separately get paracetamol reference substance, add methyl alcohol and make the solution of every 1ml containing 5mg, product solution in contrast; Get again windproof control medicinal material 0.3g, add methyl alcohol 3ml, ultrasonic processing 10 minutes, supernatant is medicinal material solution in contrast; Draw the each 4 μ l of above-mentioned three kinds of solution, put respectively in same silica G F
254on thin layer plate, taking volume ratio as 10: 2: 4: methenyl choloride-ethyl acetate-methyl alcohol-dense ammonia of 1 is developping agent, launch, take out, dry, put under ultraviolet lamp 254nm and inspect, in test sample chromatogram, with the corresponding position of reference substance chromatogram on, aobvious same color spot; Spray with 10% ethanol solution of sulfuric acid, 105 DEG C of bakings 1～2 minute, put under ultraviolet lamp 365nm and inspect again, in test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, aobvious identical bright blue look fluorescence principal spot;
2. get chlorogenic acid reference substance, add methyl alcohol and make the solution of every 1ml containing 2mg, product solution in contrast; Draw reference substance solution 5 μ l and differentiate 1. under need testing solution 2～5 μ l, put respectively on same silica gel g thin-layer plate, upper solution taking volume ratio as the butyl acetate-formic acid-water of 15: 5: 5 is as developping agent, launch, take out hot blast drying, put under ultraviolet lamp 365nm and inspect, in test sample chromatogram, with the corresponding position of reference substance chromatogram on, aobvious same color fluorescence spot;
(2). chlorogenic acid and paracetamol Simultaneous Determination method
A. chromatographic condition and system suitability are taking octadecylsilane chemically bonded silica as filling agent; Taking volume ratio as acetonitrile-methyl alcohol-0.1% phosphoric acid of 5.5: 4.5: 90 is as mobile phase; Detection wavelength is 295nm; Number of theoretical plate calculates and should be not less than 3000 by chlorogenic acid peak;
B. reference substance solution preparation is got chlorogenic acid with paracetamol reference substance is appropriate, accurately weighed, adds methyl alcohol and makes every 1ml and contain chlorogenic acid 0.02mg, and the solution of paracetamol 0.45mg, to obtain final product;
C. need testing solution preparation is got not containing sucrose Jinfanggnmao Granules 5g, and porphyrize, gets 0.2g, accurately weighed, to put in tool plug conical flask, precision adds 70% methyl alcohol 25ml, weighed weight, with power 250w, frequency 50kHz, ultrasonic processing 10 minutes, let cool, weighed weight again, supplies the weight of less loss with 70% methyl alcohol, shake up, filter, to obtain final product;
D. determination method accurate reference substance solution and the each 5 μ l of need testing solution of drawing respectively, injection liquid chromatography, measures, and to obtain final product.
4. the method for quick of a kind of Jinfanggnmao Granules according to claim 1, is further characterized in that:
(1) quick thin-layer identification method
1. get the Jinfanggnmao Granules 4g containing sucrose, porphyrize, adds methyl alcohol 5ml, and ultrasonic processing 10 minutes filters, and filtrate is as need testing solution; Separately get paracetamol reference substance, add methyl alcohol and make the solution of every 1ml containing 5mg, product solution in contrast; Get again windproof control medicinal material 0.3g, add methyl alcohol 3ml, ultrasonic processing 10 minutes, supernatant is medicinal material solution in contrast; Draw reference substance solution and the each 4 μ l of control medicinal material solution, need testing solution 8 μ l, put respectively in same silica G F
254on thin layer plate, taking volume ratio as 12: 1.5: 4: methenyl choloride-ethyl acetate-methyl alcohol-dense ammonia of 0.5 is developping agent, launch, take out, dry, put under ultraviolet lamp 254nm and inspect, in test sample chromatogram, with the corresponding position of reference substance chromatogram on, aobvious same color spot; Spray with 10% ethanol solution of sulfuric acid, 105 DEG C of bakings 1～2 minute, put under ultraviolet lamp 365nm and inspect again, in test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, aobvious identical bright blue look fluorescence principal spot;
2. get chlorogenic acid reference substance, add methyl alcohol and make the solution of every 1ml containing 2mg, product solution in contrast; Draw reference substance solution 5 μ l and differentiate 1. under need testing solution 2～5 μ l, put respectively on same silica gel g thin-layer plate, upper solution taking volume ratio as the butyl acetate-formic acid-water of 14: 4: 4 is as developping agent, launch, take out hot blast drying, put under ultraviolet lamp 365nm and inspect, in test sample chromatogram, with the corresponding position of reference substance chromatogram on, aobvious same color fluorescence spot;
(2). chlorogenic acid and paracetamol Simultaneous Determination method
A. chromatographic condition and system suitability are taking octadecylsilane chemically bonded silica as filling agent; Taking volume ratio as acetonitrile-methyl alcohol-0.1% phosphoric acid of 6: 4.5: 89.5 is as mobile phase; Detection wavelength is 295nm; Number of theoretical plate calculates and should be not less than 3000 by chlorogenic acid peak;
B. reference substance solution preparation is got chlorogenic acid with paracetamol reference substance is appropriate, accurately weighed, adds methyl alcohol and makes every 1ml and contain chlorogenic acid 0.02mg, and the solution of paracetamol 0.45mg, to obtain final product;
C. the Jinfanggnmao Granules 5g containing sucrose is got in need testing solution preparation, and porphyrize, gets 0.6g, accurately weighed, to put in tool plug conical flask, precision adds 70% methyl alcohol 25ml, weighed weight, with power 250w, frequency 50kHz, ultrasonic processing 10 minutes, let cool, weighed weight again, supplies the weight of less loss with 70% methyl alcohol, shake up, filter, to obtain final product;
D. determination method accurate reference substance solution and the each 5 μ l of need testing solution of drawing respectively, injection liquid chromatography, measures, and to obtain final product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210063430.9A CN102608250B (en) | 2012-03-13 | 2012-03-13 | Rapid detection method for Jinfangganmao granules |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210063430.9A CN102608250B (en) | 2012-03-13 | 2012-03-13 | Rapid detection method for Jinfangganmao granules |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102608250A CN102608250A (en) | 2012-07-25 |
| CN102608250B true CN102608250B (en) | 2014-07-23 |
Family
ID=46525792
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201210063430.9A Active CN102608250B (en) | 2012-03-13 | 2012-03-13 | Rapid detection method for Jinfangganmao granules |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102608250B (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108982720B (en) * | 2018-10-08 | 2021-10-08 | 湖南省中医药研究院 | Construction method and application of HPLC standard fingerprint of compound Ganmaoling granules |
| CN110133138A (en) * | 2019-05-22 | 2019-08-16 | 贵州天楼生物发展有限公司 | The detection method of stauntonvine Content of Chlorogenic Acid |
| CN110455976A (en) * | 2019-08-30 | 2019-11-15 | 广西壮族自治区药用植物园 | A kind of thin-layer chromatography detection method of " radix scutellariae adds taste disinfectant soup " extract |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101797277A (en) * | 2010-04-01 | 2010-08-11 | 贵州百灵企业集团制药股份有限公司 | Method for detecting Jingan capsule |
| CN101961430A (en) * | 2010-09-13 | 2011-02-02 | 广州市香雪制药股份有限公司 | Quality analysis method of compound Ganmaoling tablets |
| CN102085220A (en) * | 2010-11-02 | 2011-06-08 | 河北以岭医药研究院有限公司 | Thin-layer identification method with fluorescence intensifier detection for traditional Chinese medicines |
| CN102100850A (en) * | 2009-12-16 | 2011-06-22 | 天津中新药业集团股份有限公司隆顺榕制药厂 | Quality control method for refined fructus forsythiae antidotal tablets |
| CN102297926A (en) * | 2011-07-12 | 2011-12-28 | 刘金伶 | Rapid TLC identification and three-component simultaneous quantitative determination method for antitussive tablets |
| CN102507769A (en) * | 2011-10-25 | 2012-06-20 | 承德燕峰药业有限责任公司 | Quantitative determination method of chlorogenic acid and three kinds of isochlorogenic acid in lonicera flower medicinal material and preparation thereof |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2000050887A1 (en) * | 1999-02-22 | 2000-08-31 | Evotec Biosystems Ag | Utilization of supporting material in capillary electrochromatography |
| JP2010151529A (en) * | 2008-12-24 | 2010-07-08 | Kao Corp | Method for analyzing chlorogenic acid |
-
2012
- 2012-03-13 CN CN201210063430.9A patent/CN102608250B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102100850A (en) * | 2009-12-16 | 2011-06-22 | 天津中新药业集团股份有限公司隆顺榕制药厂 | Quality control method for refined fructus forsythiae antidotal tablets |
| CN101797277A (en) * | 2010-04-01 | 2010-08-11 | 贵州百灵企业集团制药股份有限公司 | Method for detecting Jingan capsule |
| CN101961430A (en) * | 2010-09-13 | 2011-02-02 | 广州市香雪制药股份有限公司 | Quality analysis method of compound Ganmaoling tablets |
| CN102085220A (en) * | 2010-11-02 | 2011-06-08 | 河北以岭医药研究院有限公司 | Thin-layer identification method with fluorescence intensifier detection for traditional Chinese medicines |
| CN102297926A (en) * | 2011-07-12 | 2011-12-28 | 刘金伶 | Rapid TLC identification and three-component simultaneous quantitative determination method for antitussive tablets |
| CN102507769A (en) * | 2011-10-25 | 2012-06-20 | 承德燕峰药业有限责任公司 | Quantitative determination method of chlorogenic acid and three kinds of isochlorogenic acid in lonicera flower medicinal material and preparation thereof |
Non-Patent Citations (13)
| Title |
|---|
| High-performance liquid chromatographic analysis for quantitation of marker compounds of artemisia capillaris thunb;Kyung Min Park 等;《Archives of Pharmacal Research》;20121231;第35卷(第12期);全文 * |
| HPLC同时测定维C银翘片中绿原酸、对乙酰氨基酚、维生素C、马来酸氯苯那敏的含量;高光伟等;《中成药》;20080229;第30卷(第2期);全文 * |
| JP特开2010-151529A 2010.07.08 |
| Kyung Min Park 等.High-performance liquid chromatographic analysis for quantitation of marker compounds of artemisia capillaris thunb.《Archives of Pharmacal Research》.2012,第35卷(第12期),2153-2162. |
| Method of screening and quantitative determination of serum levels of salicylic acid,acetaminophen,theophylline,phenobarbital,bromvalerylurea,pentobarbital,and amobarbital using liquid chromatography/electrospray mass spectrometry;Yasushi Hori 等;《Pharmaceutical Society of Japan》;20060131;第29卷(第1期);全文 * |
| Yasushi Hori 等.Method of screening and quantitative determination of serum levels of salicylic acid,acetaminophen,theophylline,phenobarbital,bromvalerylurea,pentobarbital,and amobarbital using liquid chromatography/electrospray mass spectrometry.《Pharmaceutical Society of Japan》.2006,第29卷(第1期),7-13. |
| 天香丹胶囊质量标准研究;姜林等;《中成药》;20090831;第31卷(第8期);全文 * |
| 姜林等.天香丹胶囊质量标准研究.《中成药》.2009,第31卷(第8期),1214-1218. |
| 小儿咽扁颗粒质量控制方法的简化研究;董占军等;《河北中医》;20110831;第33卷(第8期);全文 * |
| 董占军等.小儿咽扁颗粒质量控制方法的简化研究.《河北中医》.2011,第33卷(第8期),1224-1226. |
| 连防感冒颗粒中防风薄层鉴别方法改进;黄兰芷等;《中南药学》;20070430;第5卷(第2期);全文 * |
| 高光伟等.HPLC同时测定维C银翘片中绿原酸、对乙酰氨基酚、维生素C、马来酸氯苯那敏的含量.《中成药》.2008,第30卷(第2期),207-210. |
| 黄兰芷等.连防感冒颗粒中防风薄层鉴别方法改进.《中南药学》.2007,第5卷(第2期),149-150. |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102608250A (en) | 2012-07-25 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| WO2021073175A1 (en) | Method for identifying various ingredients in traditional chinese medicine composition and measuring contents | |
| CN102998411B (en) | A kind of detection method of ageratum dripping pill | |
| CN104398642A (en) | Preparation and quality detection method of compound prescription cortex phellodendri chinensis fluid | |
| CN105259295A (en) | Quality detection method for ginseng, cassia twig and poria cocos oral solution | |
| CN101701945B (en) | Method for determining anthocyanin composition spectrum and content in germplasm and seed coat of black soyabean by utilizing HPLC | |
| CN102608250B (en) | Rapid detection method for Jinfangganmao granules | |
| CN104251889B (en) | The measuring method of Phenylephrine Hydrochloride, chlorpheniramine maleate and Ibuprofen BP/EP three kinds of component contents in compound flu tablet | |
| CN102520103B (en) | Quantitative determination method of component in pill of six ingredients with rehmannia | |
| CN104764820A (en) | Method for determining content of active ingredients such as ephedrine hydrochloride and pseudoephedrine hydrochloride in pinellia ternata syrup | |
| CN109142588A (en) | A kind of LianZhixiaoyan Capsule HPLC characteristic spectrum and its construction method and application | |
| CN101520444A (en) | Method for identifying Lonicera confusa and honeysuckle flower and application thereof | |
| CN109085285B (en) | Quality control method of changyanning granules | |
| CN108037200B (en) | Quality detection method of kidney nourishing and tranquilizing pills | |
| CN104833736A (en) | Fast qualitative and quantitative detection method for 25-ingredient coral pills through quantitative analysis of multi-components by single-marker | |
| CN103926332A (en) | Ultra performance liquid chromatography method for simultaneously determining contents of uridine, guanosine and adenosine in rhizoma pinelliae extract | |
| CN102139067A (en) | Quality control method for antipyretic and antitoxic tablet | |
| CN108956843A (en) | A kind of quick multi information thin-layer identification method of banxia baizhu tianma decoction freeze-dried powder | |
| CN106596777B (en) | The method of quality control of Dandengtongnao preparation | |
| CN115808473A (en) | Novel method for quality control of Chinese herbal compound angelica Sini decoction | |
| CN106680414A (en) | Detection method of compound ardisia japonica tablet | |
| CN101703610A (en) | Quality detection method of Qingnao antihypertensive tablet | |
| CN103163272A (en) | Quality control method of infant spleen tonifying medicament | |
| CN100540037C (en) | A kind of detection method of infantile lung clearing phlegm transforming preparation | |
| CN111948331B (en) | Quality detection method of sugar-free liver-clearing granules | |
| CN102166264A (en) | Shenshitong quality control method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |