CN102100818A - Quality control method for lophanthus antifebrile tablets - Google Patents
Quality control method for lophanthus antifebrile tablets Download PDFInfo
- Publication number
- CN102100818A CN102100818A CN 200910244825 CN200910244825A CN102100818A CN 102100818 A CN102100818 A CN 102100818A CN 200910244825 CN200910244825 CN 200910244825 CN 200910244825 A CN200910244825 A CN 200910244825A CN 102100818 A CN102100818 A CN 102100818A
- Authority
- CN
- China
- Prior art keywords
- solution
- lophanthus
- antifebrile
- thin layer
- layer chromatography
- 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.)
- Granted
Links
Images
Landscapes
- Medicines Containing Plant Substances (AREA)
Abstract
The invention relates to a quality control method for lophanthus antifebrile tablets, which comprises the following steps of: identifying whether the lophanthus antifebrile tablets in a prescription contains components such as angelica dahurica, officinal magnolia bark, swordlike atractylodes rhizome, perilla leaf oil and the like or not by thin layer chromatography, and detecting tangerine peel content in the lophanthus antifebrile tablets in the prescription by taking naringin as a reference substance through liquid chromatography. In the quality control method, specific requirements of a Chinese patent medicament variety amendment item task table in an action plan are improved according to national medicine standard. In the quality control method, the standard for the lophanthus antifebrile tablets is improved, in the original standard, officinal magnolia bark is only identified, so on the basis of the original standard, a thin layer identifying method for angelica dahurica and swordlike atractylodes rhizome is added; and a method for measuring the tangerine peel content is formulated by taking hesperidin as a reference substance, so by the amended quality standard, the quality control of medicines is improved.
Description
Technical field
The invention belongs to technical field of Chinese medicines, relate to the detection method of Chinese medicine, especially a kind of method of quality control of lophanthus antifebrile tablet.
Background technology
Lophanthus antifebrile tablet is made up of Rhizoma Atractylodis, Pericarpium Citri Reticulatae, Cortex Magnoliae Officinalis (processed with Rhizoma Zingiberis Recens), the Radix Angelicae Dahuricae, Poria, Pericarpium Arecae, Rhizoma Pinelliae, Radix Glycyrrhizae extractum, patchouli oil, Folium perillae acutae oil, preparation method: above ten flavors, the Radix Angelicae Dahuricae becomes fine powder with the Rhizoma Pinelliae pulverize separately, sieving for standby, Pericarpium Citri Reticulatae extracts and dissolves in right amount with ethanol after volatile oil mixes with patchouli oil, Folium perillae acutae oil, and is standby; Pericarpium Citri Reticulatae medicinal residues decocting boils once, and the time is 1 hour, and Pericarpium Arecae, Poria decocting boil twice, and 2 hours for the first time, 1 hour for the second time, merge above decocting liquid, filter, filtrate and Radix Glycyrrhizae extractum merge, and are concentrated into relative density 1.20～1.30 (50～60 ℃) cream; The Radix Angelicae Dahuricae, Rhizoma Atractylodis, Cortex Magnoliae Officinalis be with 60% alcohol reflux three times, and 6 hours for the first time, 4 hours for the second time, 2 hours for the third time, merge above ethanol extract, filter, filtrate recycling ethanol is condensed into cream; Water, pure condensed cream are merged, add fine powder and adjuvants such as Rhizoma Pinelliae, the Radix Angelicae Dahuricae, mixing is made granule, and drying is blended into the alcoholic solution of patchouli oil, Folium perillae acutae oil, Oleum Citri Reticulatae, mixing, compacting in flakes, or bag film-coat, promptly.
This product was " huoxiang zhengqi powder " of Song's prescription of peaceful benevolent dispensary originally, change system into tablet in nineteen fifty-five, 1964 annual incomes " Tianjin Chinese patent medicine standard " additional copy, " Tianjin Chinese patent medicine standard " recorded this medicine in 1978, the 15th in 1998 annual income Ministry of Public Health Chinese traditional patent formulation preparations, because this product is traditional Cheng Fang " huoxiang zhengqi powder " change dosage form, and of the same name with the side with HUOXIANG ZHENGQI SHUI, ageratum granule and HUOXIANG ZHENGQI RUANJIAONANG etc., factory thinks that this product should not the change of title still.
Though still there is not the international standard of plant medicine at present in the world, the trend of Chinese medicine standard but the south east asia of the U.S., European Union, China and tradition outlet Chinese medicine is improved, in the case, need to propose to be fit to the standard of China's product quality to adapt to international standard, it is historical that China has the Chinese medicine in thousands of years to use, countries in the world are many Chinese medicine standards with reference to China in working out corresponding plant amedica target level of product quality, so quality standard perfect, that improve Chinese medicine is more extremely urgent.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art part, a kind of method of quality control of lophanthus antifebrile tablet that can the qualitative and quantitative analysis ingredient is provided, this method has that detection means is simple, the testing result characteristic of accurate.
The objective of the invention is to be achieved through the following technical solutions:
A kind of method of quality control of lophanthus antifebrile tablet, step is:
(1) thin layer chromatography differentiates in the lophanthus antifebrile tablet whether contain Radix Angelicae Dahuricae composition;
(2) thin layer chromatography differentiates in the lophanthus antifebrile tablet whether contain the Cortex Magnoliae Officinalis composition;
(3) thin layer chromatography differentiates in the lophanthus antifebrile tablet whether contain the Rhizoma Atractylodis composition;
(4) liquid chromatography detects Pericarpium Citri Reticulatae content in the lophanthus antifebrile tablet.
And the method that the thin layer chromatography of the described Radix Angelicae Dahuricae is differentiated is as follows:
1. the preparation of need testing solution: get for examination lophanthus antifebrile tablet sample, remove coating, porphyrize, the 30ml that adds diethyl ether flooded 1 hour, and constantly jolting is centrifugal, gets supernatant, flings to ether, and residue adds ethyl acetate 1ml makes dissolving, as need testing solution;
2. the preparation of reference substance solution: get the imperatorin reference substance, add ethyl acetate and make the solution that every 1ml contains 1mg, in contrast product solution;
3. thin layer chromatography condition and result: thin layer chromatography test, draw need testing solution and each 5-10 μ l of reference substance solution, put respectively on same silica gel g thin-layer plate, with petroleum ether: ether=3: 2 is developing solvent, launches, and takes out, dry, put under the 365nm ultra-violet lamp and inspect, inspect the test sample chromatograph with the corresponding position of reference substance chromatograph on whether show the fluorescence speckle of same color, and then whether contain Radix Angelicae Dahuricae composition in definite sample.
And the method that the thin layer chromatography of described Cortex Magnoliae Officinalis is differentiated is as follows:
1. the preparation of need testing solution: get the need testing solution in the Radix Angelicae Dahuricae discriminating, volatilize ethyl acetate, residue adds methanol 2ml makes dissolving, as need testing solution;
2. the preparation of reference substance solution: get magnolol and honokiol reference substance and add dehydrated alcohol and make the solution that every 1ml contains 1mg, in contrast product solution;
3. thin layer chromatography condition and result: thin layer chromatography test, draw need testing solution and each 5-10 μ l of reference substance solution, put respectively on same silica gel g thin-layer plate, with petroleum ether: ethyl acetate: methanol=80: 20: 2 is developing solvent, launches, take out, dry, spray is with 5% vanillin sulfuric acid solution, and it is clear to be heated to the speckle colour developing, inspect the speckle that on the corresponding position of reference substance chromatograph, whether shows same color in the test sample chromatograph, and then determine for whether containing the Cortex Magnoliae Officinalis composition in the examination.
And the method that the thin layer chromatography of described Rhizoma Atractylodis is differentiated is as follows:
1. the preparation of need testing solution: get for examination lophanthus antifebrile tablet sample, film-coat is removed coating, and porphyrize adds normal hexane, and supersound process filters, and filtrate evaporate to dryness, residue add normal hexane 2ml makes dissolving, as need testing solution;
2. the preparation of control medicinal material solution: get Rhizoma Atractylodis control medicinal material 0.5g, add normal hexane 2ml, supersound process 15 minutes filters, and filtrate is medical material solution in contrast;
3. thin layer chromatography condition and result: thin layer chromatography test, draw need testing solution, each 5～10 μ l of control medicinal material solution, put respectively on same silica gel g thin-layer plate, with petroleum ether: ethyl acetate=20: 1 is developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid of 5% paradime thylaminobenzaldehyde, it is clear to be heated to the speckle colour developing, inspect in the test sample chromatograph with the corresponding position of control medicinal material chromatograph on whether show the speckle of same color, and then whether contain the Rhizoma Atractylodis composition in definite sample.
And the method for the content of described liquid chromatography for measuring Pericarpium Citri Reticulatae is:
1. chromatographic condition: with octadecylsilane chemically bonded silica is filler; Acetonitrile: 0.05mol/L sodium dihydrogen phosphate=13: 70 is a mobile phase; The detection wavelength is 284nm; Flow velocity: 1.0ml/min, 30 ℃ of column temperatures, number of theoretical plate should be not less than 2000 by the Hesperidin peak;
2. the preparation of control medicinal material solution: it is an amount of that precision takes by weighing the Hesperidin reference substance, adds methanol and make the solution that every 1ml contains Hesperidin 60 μ g, and product solution is gone into Liquid Detection in contrast;
3. the preparation of need testing solution: get 20 of this product, Film coated tablets is removed coating, and accurate the title decides, porphyrize is got 0.75g, and accurate the title decides, put in the 25ml tool plug conical flask, the accurate methanol 25ml that adds claims to decide weight, supersound process 30 minutes is put coldly, claims to decide weight again, supply the weight that subtracts mistake with methanol, mixing filters, get subsequent filtrate, that is, go into Liquid Detection;
4. interpretation of result: contain the quantifier regulation according to the tentative standard WS-10057 of State Food and Drug Administration (ZD-0057)-2002 HUOXIANG ZHENGQI PIAN, every of this product contains Pericarpium Citri Reticulatae in Determination of Hesperidin Content, must not be less than 0.35mg, wherein plain sheet: every heavy 0.3g; Film coated tablets: every heavy 0.31g.
Advantage of the present invention and good effect are:
1, improves the specific requirement that action plan Chinese patent medicine kind increases revision project task table according to the national drug standards, the present invention has carried out raising, perfect to the HUOXIANG ZHENGQI PIAN standard, the discriminating of having only Cortex Magnoliae Officinalis is arranged in primary standard, on the primary standard basis, increased the thin layer discrimination method of the Radix Angelicae Dahuricae, Rhizoma Atractylodis; With the Hesperidin is reference substance, has formulated the content assaying method of Pericarpium Citri Reticulatae, and revised quality standard has improved the quality control of medicine.
2, have only the thin layer of Cortex Magnoliae Officinalis to differentiate in the primary standard, can not the better controlled product quality, the present invention has all carried out the thin layer discrimination test to the Radix Angelicae Dahuricae, Rhizoma Atractylodis, Folium perillae acutae oil, patchouli oil in the prescription on the basis of primary standard, filtering out that favorable reproducibility, specificity are strong, the speckle colour developing is clear, Cortex Magnoliae Officinalis, the Radix Angelicae Dahuricae, Rhizoma Atractylodis, Folium perillae acutae oil method that the result easily judges are included in the standard, is that the discriminating of this important preparation is more accurate.
Description of drawings
Fig. 1 is a Radix Angelicae Dahuricae thin layer chromatography identification color spectrogram of the present invention, be followed successively by from left to right: 1 HUOXIANG ZHENGQI PIAN (lot number 0704001), 2 HUOXIANG ZHENGQI PIAN (lot number 0704002), 3 HUOXIANG ZHENGQI PIAN (lot number 0704003), imperatorin, HUOXIANG ZHENGQI PIAN Radix Angelicae Dahuricae negative sample;
Fig. 2 is a Cortex Magnoliae Officinalis thin layer chromatography identification color spectrogram of the present invention, is followed successively by from left to right: 1 HUOXIANG ZHENGQI PIAN (lot number 0704001), 2 HUOXIANG ZHENGQI PIAN (lot number 0704002), 3 HUOXIANG ZHENGQI PIAN (lot number 0704003), 4 Cortex Magnoliae Officinalis reference substances, 5 magnolia obovata reference substances, 6 HUOXIANG ZHENGQI PIAN Cortex Magnoliae Officinalis negative samples;
Fig. 3 is a Rhizoma Atractylodis thin layer chromatography identification color spectrogram of the present invention, is followed successively by from left to right: 1 HUOXIANG ZHENGQI PIAN (lot number 0704001), 2 HUOXIANG ZHENGQI PIAN (lot number 0704002), 3 HUOXIANG ZHENGQI PIAN (lot number 0704003), Rhizoma Atractylodis control medicinal material, 5 HUOXIANG ZHENGQI PIAN Rhizoma Atractylodis negative samples;
Fig. 4 is a Folium perillae acutae oil thin layer chromatography identification color spectrogram of the present invention, is followed successively by from left to right: 1. Folium perillae acutae oil A, 2. Folium perillae acutae oil B, 3. Folium perillae acutae oil C, 4. Folium Perillae control medicinal material;
Fig. 5 is a Hesperidin reference substance solution of the present invention;
Fig. 6 is negative sample spectrogram in the naringin detection of the present invention;
Fig. 7 is for supplying the detection chromatogram of test agent HUOXIANG ZHENGQI PIAN (sample 0704001) in the naringin detection of the present invention.
The specific embodiment
Below in conjunction with embodiment, the present invention is further described, and following embodiment is illustrative, is not determinate, can not limit protection scope of the present invention with following embodiment.
The method of quality control of lophanthus antifebrile tablet, the step of its method is:
(1) thin layer chromatography of the Radix Angelicae Dahuricae is differentiated
1. the preparation of need testing solution: get for 20 in examination lophanthus antifebrile tablet sample, remove coating, porphyrize, the 30ml that adds diethyl ether flooded 1 hour, and constantly jolting is centrifugal, gets supernatant, flings to ether, and residue adds ethyl acetate 1ml makes dissolving, as need testing solution;
2. the preparation of reference substance solution: get the imperatorin reference substance, add ethyl acetate and make the solution that every 1ml contains 1mg, in contrast product solution;
3. the preparation of negative sample solution: by the prescription proportioning, get and remove other flavor medical materials of the Radix Angelicae Dahuricae, make sample, make negative sample solution by above-mentioned need testing solution preparation method again by the preparation technology of former medicine;
4. thin layer chromatography condition and result: according to thin layer chromatography (2005 editions appendix VIB of Chinese Pharmacopoeia) test, draw need testing solution, negative control product solution and each 5-10 μ l of reference substance solution, put respectively on same silica gel g thin-layer plate, with petroleum ether (60～90 ℃): ether=3: 2 is developing solvent, launch, take out, dry, put under the ultra-violet lamp (365nm) and inspect.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color, negative noiseless, testing result is seen Fig. 1.
(2) thin layer chromatography of Cortex Magnoliae Officinalis is differentiated
1. the preparation of need testing solution: get the need testing solution under discriminating (1) item, volatilize ethyl acetate, residue adds methanol 2ml makes dissolving, as need testing solution;
2. the preparation of reference substance solution: get magnolol and honokiol reference substance and add dehydrated alcohol and make the solution that every 1ml contains 1mg, in contrast product solution;
3. the preparation of negative sample solution: by the prescription proportioning, get other flavor medical materials of removing Cortex Magnoliae Officinalis, make sample, make negative sample solution by above-mentioned need testing solution preparation method again by former medicine preparation technology;
4. thin layer chromatography condition and result: according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005) test, draw need testing solution, negative sample solution and each 5-10 μ l of reference substance solution, put respectively on same silica gel g thin-layer plate, with petroleum ether (60～90 ℃): ethyl acetate: methanol=80: 20: 2 is developing solvent, launch, take out, dry, spray is with 5% vanillin sulfuric acid solution, and it is clear to be heated to the speckle colour developing.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color, and negative noiseless, testing result is seen Fig. 2.
(3) thin layer chromatography of Rhizoma Atractylodis is differentiated
1. the preparation of need testing solution: get for 6 in examination lophanthus antifebrile tablet sample, film-coat is removed coating, and porphyrize adds normal hexane 20ml, and supersound process 15 minutes filters, and filtrate evaporate to dryness, residue add normal hexane 2ml makes dissolving, as need testing solution.
2. the preparation of control medicinal material solution: get Rhizoma Atractylodis control medicinal material 0.5g, add normal hexane 2ml, supersound process 15 minutes filters, and filtrate is medical material solution in contrast.
3. the preparation of negative sample solution: by the prescription proportioning, get other flavor medical materials of removing Rhizoma Atractylodis, make sample, make negative sample solution by above-mentioned need testing solution preparation method again by former medicine preparation technology.
4. thin layer chromatography condition and result: according to thin layer chromatography (2005 editions appendix VIB of Chinese Pharmacopoeia) test, draw need testing solution, each 5～10 μ l of control medicinal material solution, put respectively on same silica gel g thin-layer plate, with petroleum ether (60～90 ℃): ethyl acetate=20: 1 is developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid of 5% paradime thylaminobenzaldehyde, and it is clear to be heated to the speckle colour developing.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color, and negative noiseless, see Fig. 3.
(4) thin layer chromatography of Folium perillae acutae oil is differentiated
1. the preparation of reference substance solution: other gets Folium Perillae control medicinal material 0.7g, puts in the 500ml round-bottomed flask, adds water 250ml, mixing, connect volatile oil determination apparatus, add water to scale from the determinator upper end, and till overflow goes in the flask, add petroleum ether (60 ℃～90 ℃) 1.5ml again, connect reflux condensing tube, be heated to and boil, and keep little and boiled 2 hours, put coldly, divide and to get petroleum ether layer product solution in contrast;
2. the preparation of test solution: get for examination lophanthus antifebrile tablet sample and make need testing solution according to method method 1.;
3. test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with petroleum ether (60 ℃～90 ℃): ethyl acetate=19: 1 is developing solvent, launch, take out, dry, spray is placed with the dinitrophenylhydrazine test solution.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
(5) assay of liquid chromatography Pericarpium Citri Reticulatae
Chromatographic condition: with octadecylsilane chemically bonded silica is filler; Acetonitrile: 0.05mol/L sodium dihydrogen phosphate=13: 70 is a mobile phase, and wherein sodium dihydrogen phosphate is with phosphoric acid adjust pH to 3; Wavelength is 284nm; Flow velocity: 1.0ml/min, 30 ℃ of column temperatures, number of theoretical plate should be not less than 2000 by the Hesperidin peak;
1. the preparation of control medicinal material solution: it is an amount of that precision takes by weighing the Hesperidin reference substance, adds methanol and make the solution that every 1ml contains Hesperidin 60 μ g, and product solution is gone into Liquid Detection in contrast, and testing result as shown in Figure 5;
2. the preparation of negative sample solution: by the prescription proportioning, get other medical materials except that Pericarpium Citri Reticulatae, make tablet by former medicine preparation technology, 1. need testing solution preparation method set by step makes negative sample solution again, goes into Liquid Detection, and testing result as shown in Figure 6;
3. the preparation of need testing solution: get 20 of this product, Film coated tablets is removed coating, and accurate the title decided porphyrize, get 0.75g, the accurate title, decide, and puts in the 25ml tool plug conical flask, the accurate methanol 25ml that adds claims to decide weight, supersound process 30 minutes, put coldly, claim again to decide weight, supply the weight that subtracts mistake with methanol, mixing filters, and gets subsequent filtrate, that is, go into liquid phase, testing result as shown in Figure 7;
4. interpretation of result: negative need testing solution does not have the Hesperidin Interference Peaks and exists, this detection method specificity is good, contain the quantifier regulation according to the tentative standard WS-10057 of State Food and Drug Administration (ZD-0057)-2002 HUOXIANG ZHENGQI PIAN, every (plain sheet: every heavy 0.3g of this product; Film coated tablets: every heavy 0.31g) contain Pericarpium Citri Reticulatae, must not be less than 0.35mg in Determination of Hesperidin Content.
Claims (5)
1. the method for quality control of a lophanthus antifebrile tablet, it is characterized in that: the step of its method is:
(1) thin layer chromatography differentiates in the lophanthus antifebrile tablet whether contain Radix Angelicae Dahuricae composition;
(2) thin layer chromatography differentiates in the lophanthus antifebrile tablet whether contain the Cortex Magnoliae Officinalis composition;
(3) thin layer chromatography differentiates in the lophanthus antifebrile tablet whether contain the Rhizoma Atractylodis composition;
(4) liquid chromatography detects Pericarpium Citri Reticulatae content in the lophanthus antifebrile tablet.
2. the method for quality control of lophanthus antifebrile tablet according to claim 1 is characterized in that: the method that the thin layer chromatography of the described Radix Angelicae Dahuricae is differentiated is as follows:
1. the preparation of need testing solution: get for examination lophanthus antifebrile tablet sample, remove coating, porphyrize, the 30ml that adds diethyl ether flooded 1 hour, and constantly jolting is centrifugal, gets supernatant, flings to ether, and residue adds ethyl acetate 1ml makes dissolving, as need testing solution;
2. the preparation of reference substance solution: get the imperatorin reference substance, add ethyl acetate and make the solution that every 1ml contains 1mg, in contrast product solution;
3. thin layer chromatography condition and result: thin layer chromatography test, draw need testing solution and each 5-10 μ l of reference substance solution, put respectively on same silica gel g thin-layer plate, with petroleum ether: ether=3: 2 is developing solvent, launches, and takes out, dry, put under the 365nm ultra-violet lamp and inspect, inspect the test sample chromatograph with the corresponding position of reference substance chromatograph on whether show the fluorescence speckle of same color, and then whether contain Radix Angelicae Dahuricae composition in definite sample.
3. the method for quality control of lophanthus antifebrile tablet according to claim 1 is characterized in that: the method that the thin layer chromatography of described Cortex Magnoliae Officinalis is differentiated is as follows:
1. the preparation of need testing solution: get the need testing solution in the Radix Angelicae Dahuricae discriminating, volatilize ethyl acetate, residue adds methanol 2ml makes dissolving, as need testing solution;
2. the preparation of reference substance solution: get magnolol and honokiol reference substance and add dehydrated alcohol and make the solution that every 1ml contains 1mg, in contrast product solution;
3. thin layer chromatography condition and result: thin layer chromatography test, draw need testing solution and each 5-10 μ l of reference substance solution, put respectively on same silica gel g thin-layer plate, with petroleum ether: ethyl acetate: methanol=80: 20: 2 is developing solvent, launches, take out, dry, spray is with 5% vanillin sulfuric acid solution, and it is clear to be heated to the speckle colour developing, inspect the speckle that on the corresponding position of reference substance chromatograph, whether shows same color in the test sample chromatograph, and then determine for whether containing the Cortex Magnoliae Officinalis composition in the examination.
4. the method for quality control of lophanthus antifebrile tablet according to claim 1 is characterized in that: the method that the thin layer chromatography of described Rhizoma Atractylodis is differentiated is as follows:
1. the preparation of need testing solution: get for examination lophanthus antifebrile tablet sample, film-coat is removed coating, and porphyrize adds normal hexane, and supersound process filters, and filtrate evaporate to dryness, residue add normal hexane 2ml makes dissolving, as need testing solution;
2. the preparation of control medicinal material solution: get Rhizoma Atractylodis control medicinal material 0.5g, add normal hexane 2ml, supersound process 15 minutes filters, and filtrate is medical material solution in contrast;
3. thin layer chromatography condition and result: thin layer chromatography test, draw need testing solution, each 5～10 μ l of control medicinal material solution, put respectively on same silica gel g thin-layer plate, with petroleum ether: ethyl acetate=20: 1 is developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid of 5% paradime thylaminobenzaldehyde, it is clear to be heated to the speckle colour developing, inspect in the test sample chromatograph with the corresponding position of control medicinal material chromatograph on whether show the speckle of same color, and then whether contain the Rhizoma Atractylodis composition in definite sample.
5. the method for quality control of lophanthus antifebrile tablet according to claim 1, it is characterized in that: the method for the content of described liquid chromatography for measuring Pericarpium Citri Reticulatae is:
1. chromatographic condition: with octadecylsilane chemically bonded silica is filler; Acetonitrile: 0.05mol/L sodium dihydrogen phosphate=13: 70 is a mobile phase; The detection wavelength is 284nm; Flow velocity: 1.0ml/min, 30 ℃ of column temperatures, number of theoretical plate should be not less than 2000 by the Hesperidin peak;
2. the preparation of control medicinal material solution: it is an amount of that precision takes by weighing the Hesperidin reference substance, adds methanol and make the solution that every 1ml contains Hesperidin 60 μ g, and product solution is gone into Liquid Detection in contrast;
3. the preparation of need testing solution: get 20 of this product, Film coated tablets is removed coating, and accurate the title decides, porphyrize is got 0.75g, and accurate the title decides, put in the 25ml tool plug conical flask, the accurate methanol 25ml that adds claims to decide weight, supersound process 30 minutes is put coldly, claims to decide weight again, supply the weight that subtracts mistake with methanol, mixing filters, get subsequent filtrate, that is, go into Liquid Detection;
4. interpretation of result: contain the quantifier regulation according to the tentative standard WS-10057 of State Food and Drug Administration (ZD-0057)-2002 HUOXIANG ZHENGQI PIAN, every of this product contains Pericarpium Citri Reticulatae in Determination of Hesperidin Content, must not be less than 0.35mg, wherein plain sheet: every heavy 0.3g; Film coated tablets: every heavy 0.31g.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200910244825 CN102100818B (en) | 2009-12-16 | 2009-12-16 | Quality control method for lophanthus antifebrile tablets |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200910244825 CN102100818B (en) | 2009-12-16 | 2009-12-16 | Quality control method for lophanthus antifebrile tablets |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102100818A true CN102100818A (en) | 2011-06-22 |
| CN102100818B CN102100818B (en) | 2012-12-12 |
Family
ID=44154018
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200910244825 Active CN102100818B (en) | 2009-12-16 | 2009-12-16 | Quality control method for lophanthus antifebrile tablets |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102100818B (en) |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102998411A (en) * | 2011-09-13 | 2013-03-27 | 天士力制药集团股份有限公司 | Quality detection method for Huoxiang Zhengqi dripping pills |
| CN103134883A (en) * | 2011-11-28 | 2013-06-05 | 邯郸摩罗丹药业股份有限公司 | Medicine composition and detecting method of manufacturing agent of medicine composition |
| CN106198836A (en) * | 2016-06-24 | 2016-12-07 | 中国人民解放军第三〇七医院 | Clearing brain tablet method of quality control |
| CN106370768A (en) * | 2016-10-20 | 2017-02-01 | 中悦民安（北京）科技发展有限公司 | Identification method of patchouli in traditional Chinese medicine compounds |
| CN107389821A (en) * | 2017-07-25 | 2017-11-24 | 长江师范学院 | A kind of method of active ingredient in measure ageratum oral liquid |
| CN108627588A (en) * | 2018-08-14 | 2018-10-09 | 上海和黄药业有限公司 | A kind of detection method of healthy tendency piece finger-print and its application |
| CN110927322A (en) * | 2019-11-07 | 2020-03-27 | 石药集团中奇制药技术（石家庄）有限公司 | Detection method of agastache rugosus healthy energy mixture |
| CN111665317A (en) * | 2020-07-23 | 2020-09-15 | 长春雷允上药业有限公司 | Method for simultaneously identifying pogostemon cablin, magnolia officinalis and rhizoma atractylodis |
| CN114354792A (en) * | 2021-12-24 | 2022-04-15 | 安徽誉隆亚东药业有限公司 | Detection method of yellow thick antidiarrheal dripping pills |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100367996C (en) * | 2003-12-23 | 2008-02-13 | 江苏康缘药业股份有限公司 | Quality control method of 'Jia Wei Huo Xiang' soft capsule |
-
2009
- 2009-12-16 CN CN 200910244825 patent/CN102100818B/en active Active
Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102998411A (en) * | 2011-09-13 | 2013-03-27 | 天士力制药集团股份有限公司 | Quality detection method for Huoxiang Zhengqi dripping pills |
| CN102998411B (en) * | 2011-09-13 | 2015-12-16 | 天士力制药集团股份有限公司 | A kind of detection method of ageratum dripping pill |
| CN103134883A (en) * | 2011-11-28 | 2013-06-05 | 邯郸摩罗丹药业股份有限公司 | Medicine composition and detecting method of manufacturing agent of medicine composition |
| CN103134883B (en) * | 2011-11-28 | 2015-05-13 | 邯郸制药股份有限公司 | Medicine composition and detecting method of formula of medicine composition |
| CN106198836A (en) * | 2016-06-24 | 2016-12-07 | 中国人民解放军第三〇七医院 | Clearing brain tablet method of quality control |
| CN106370768A (en) * | 2016-10-20 | 2017-02-01 | 中悦民安（北京）科技发展有限公司 | Identification method of patchouli in traditional Chinese medicine compounds |
| CN107389821A (en) * | 2017-07-25 | 2017-11-24 | 长江师范学院 | A kind of method of active ingredient in measure ageratum oral liquid |
| CN108627588A (en) * | 2018-08-14 | 2018-10-09 | 上海和黄药业有限公司 | A kind of detection method of healthy tendency piece finger-print and its application |
| CN108627588B (en) * | 2018-08-14 | 2024-03-12 | 上海和黄药业有限公司 | Detection method of Zhengqi tablet fingerprint and application thereof |
| CN110927322A (en) * | 2019-11-07 | 2020-03-27 | 石药集团中奇制药技术（石家庄）有限公司 | Detection method of agastache rugosus healthy energy mixture |
| CN110927322B (en) * | 2019-11-07 | 2022-05-17 | 石药集团中奇制药技术（石家庄）有限公司 | Detection method of Huoxiang Zhengqi mixture |
| CN111665317A (en) * | 2020-07-23 | 2020-09-15 | 长春雷允上药业有限公司 | Method for simultaneously identifying pogostemon cablin, magnolia officinalis and rhizoma atractylodis |
| CN114354792A (en) * | 2021-12-24 | 2022-04-15 | 安徽誉隆亚东药业有限公司 | Detection method of yellow thick antidiarrheal dripping pills |
| CN114354792B (en) * | 2021-12-24 | 2023-12-08 | 安徽誉隆亚东药业有限公司 | Detection method of yellow thick antidiarrheal drop pills |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102100818B (en) | 2012-12-12 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102100818B (en) | Quality control method for lophanthus antifebrile tablets | |
| CN103197027A (en) | Quality control method of astragalus-leech capsules capable of regulating collaterals | |
| CN101028388B (en) | Quality inspection of Chinese-medicinal preparation for treating shortsighness and asthenopia | |
| CN102139008A (en) | Quality control method of Xiaoer daochi tablet | |
| CN104758515A (en) | Traditional Chinese medicinal composition for treating nephropathy as well as preparation method and detection method thereof | |
| CN105301168B (en) | The detection method of dredging collateral resolving sputum capsule | |
| CN102335402A (en) | Detection method of Chinese preparation mixture for invigorating the spleen and replenishing qi | |
| CN102038908B (en) | Detection method of tambac depression-alleviating pill as traditional Chinese medical preparation | |
| CN104407092A (en) | Quality detection method of traditional Chinese medicinal composition with efficacy of appetizing and invigorating spleen | |
| CN102426205A (en) | Detection method of thrombus sumalin capsules | |
| CN102139067A (en) | Quality control method for antipyretic and antitoxic tablet | |
| CN103308644A (en) | Quality detection method for miscarriage-preventing leonurus preparation | |
| CN100542523C (en) | Capsule with hairy vein agrimony and arenobufagin and preparation method thereof, method of quality control | |
| CN101385808B (en) | Detection method of Zhubai tranquilizing pill | |
| CN102552515A (en) | Quality detection method for blood-nourishing Chinese angelica syrup | |
| CN102139040A (en) | Quality control method of tablet capable of clearing lung and inhibiting fire | |
| CN101716270B (en) | Method for detecting quality of traditional Chinese herbal medicament compound preparation for invigorating blood and regulating menses | |
| CN100522205C (en) | Method for detecting infant's rhinitis granule | |
| CN103211907A (en) | Siwu decoction formulated particles, and preparation method and detection method thereof | |
| CN100515476C (en) | Compound capsule with pseudo-ginseng and Chinese fanpalm seed, its preparation process and quality control method | |
| CN101601855B (en) | Analysis method of Guilong kechuanning tablet | |
| CN102068566B (en) | Detection method for Yinchen Wudan pills for treating damp-heat jaundice | |
| CN102507842A (en) | Testing method for Xueshuan xinmaining tablet | |
| CN101574477A (en) | Method for controlling quality of menstruation regulation and macula removal tablet | |
| CN102507844A (en) | Testing method for Xueshuan xinmaining tablet |
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 | ||
| CP03 | Change of name, title or address | ||
| CP03 | Change of name, title or address |
Address after: No.21, 10th Street, Binhai New Area Economic and Technological Development Zone, Tianjin 300457 Patentee after: Jinyao Darentang Group Co.,Ltd. Longshunrong Pharmaceutical Factory Address before: 300457 No. tenth, 21 Avenue, Tianjin economic and Technological Development Zone Patentee before: Longshunrong Pharmaceutical Factory, Tianjin Zhongxin Pharmaceutical Group Co.,Ltd. |