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Picris L.are annual,biennial to perennial herbs of Compositae.They are distributed in Europe,Asia and North Africa,and there are 5 species in China. The chemical composition mainly contains flavonoids, organic acids, terpenoids, and polysaccharides.The actions were antipyretic,antidotal,antiphlogistic and analgesic.So was commonly used in the treatment of some diseases such as mastitis,mumps and hepatitis in civil. In contemporary research, hypoglycemic, hypolipidemic and anti-inflammatory,antioxidant and other physiological activities were found.In addition,Its super collection capacity of metal ions like Zn,Cd,Pb and etc may be used for the recovery of heavy metal contaminated soil and environmental protection.
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Objective:To improve the identification and determination methods in the original quality standard for belladonna oral solution.Methods:Belladonna oral solution was identified by a specific chromatogram of HPLC,and scopoletin and hyoscyamine sulfate in belladonna oral solution were detected by dual wavelength spectrophotometry.The detection of fingerprints was performed on a Waters SunFire C18 (250 mm×4.6mm,5 μm) column.The mobile phase was methanol-0.05% phosphoric acid solution at a flow rate of 1.0 ml·min-1.The detection wavelength was 344 nm and the column temperature was 30℃.The detection of scopoletin and hyoscyamine sulfate was performed on the same C18 column.The mobile phase was 10 mmol·L-1 heptanesulfonate sodiumat (pH value was 3.3 adjusted by glacial acetic acid)-absolute ethanol-acetonitrile (68.75∶6.25∶25) at a flow rate of 1.0 ml·min-1.The detection wavelengths were 344 nm and 210 nm,and the column temperature was 30℃.Results:The specific chromatogram of belladonna oral solution was accordance with that of belladonna tincture raw material.The retention time and relative peak area of each characteristic peak and reference peak all met requirements of Chinese Pharmacopoeia.Scopoletin and hyoscyamine sulfate were completely separated from the other compositions under the above mentioned conditions.The calibration curves were linear within the range of 5.168-103.360 μg·ml-1 (r=1.000 0) for scopoletin and 50.560-758.400 μg·ml-1 (r=0.999 9) for hyoscyamine sulfate.The average recovery was 101.79% (RSD=1.05%,n=6) and 100.92% (RSD=0.97%,n=6),respectively.Conclusion:After the quality control method improvement,the identification shows high specificity and the quality of belladonna oral solution can be better controlled by the two selected index components.The method is easy and accurate,which can provide a reliable way to control the quality.
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Objective: To establish HPLC fingerprint chromatogram analysis for Mahuang Xuanfei Zhike syrup. Methods: The separation was performed on a Waters SunFire C18 column (250 mm × 4. 6 mm,5 μm), the mobile phase consisted of acetonitrile-0. 2% phosphoric acid with gradient elution at the flow rate of 1. 0 ml·min-1 , the detection wavelength was at 277 nm,the column temperature was at 30℃, and the sample size was 10 μl. Results: The precision, repeatability and stability of the fingerprint were measured. The fingerprints of 10 samples of Mahuang Xuanfei Zhike syrup revealed that there were twenty-four common peaks, and a-mong them, eight peaks were identified to Chinese, chlorogenic acid, caffeic acid, forsythin A, luteolin, apigenin, carotene and wild iris. Conclusion:The repeatability and information of chromatogram peaks of the method are satisfied, which provides a credible meth-od for controlling the quality of Mahuang Xuanfei Zhike syrup.
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Objective To establish a specific HPLC method for simultaneous determination of three components ( baicalin, linarin and rhein) in Cuochuang Xiaoyan lotion. Methods The three components in Cuochuang Xiaoyan lotion were assayed by HPLC gradient elution method.The assay was performed with Waters Xterra MS C18(4.6 mm×250 mm,5 μm) column, with acetonitrile (A) and 0.2% phosphoric acid solution (B) as mobile phase in gradient elution.The flow rate was 1.0 mL·min-1.The detection wave length was 277 nm and column temperature was 30 ℃. Results Three components were completely separated from the adjacent peaks and a good linear relationship between each sample concentration and integral area was obtained.The linear equations were as follows:Ybaicalin=9.208X-0.0994(R2=0.9999, 83.97-839.70 μg·mL-1);Ylinarin=3.0628X-0.0038 ( R2 = 0. 9999, 34. 75-347. 49 μg · mL-1 );Yrhein = 1. 0225X-0. 0286 ( R2 = 0. 9998, 63. 20-632.00 μg·mL-1 ) . Conclusion The HPLC method is simple, accurate and reproducible, which is effective in controlling the quality of Cuochuang Xiaoyan lotion.
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Objective To establish a specific HPLC method for simultaneous determination of three components ( baicalin, linarin and rhein) in Cuochuang Xiaoyan lotion. Methods The three components in Cuochuang Xiaoyan lotion were assayed by HPLC gradient elution method.The assay was performed with Waters Xterra MS C18(4.6 mm×250 mm,5 μm) column, with acetonitrile (A) and 0.2% phosphoric acid solution (B) as mobile phase in gradient elution.The flow rate was 1.0 mL·min-1.The detection wave length was 277 nm and column temperature was 30 ℃. Results Three components were completely separated from the adjacent peaks and a good linear relationship between each sample concentration and integral area was obtained.The linear equations were as follows:Ybaicalin=9.208X-0.0994(R2=0.9999, 83.97-839.70 μg·mL-1);Ylinarin=3.0628X-0.0038 ( R2 = 0. 9999, 34. 75-347. 49 μg · mL-1 );Yrhein = 1. 0225X-0. 0286 ( R2 = 0. 9998, 63. 20-632.00 μg·mL-1 ) . Conclusion The HPLC method is simple, accurate and reproducible, which is effective in controlling the quality of Cuochuang Xiaoyan lotion.
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Objective:To prepare Cuochuang Xiaoyan lotion and establish HPLC fingerprint chromatogram for the quality control . Methods:The separation was performed on a Waters XTerra MS C 18column(250 mm ×4.6 mm, 5μm).The mobile phase consisted of acetonitrile-0.2%phosphoric acid with gradient elution at a flow rate of 1.0 ml· min-1 , the eluent was monitored by a UV detector at 277 nm, and the column temperature was at 30℃.Results: There were sixteen common peaks for the sample , and among them, three ones were identified as baicalin , linarin and rhein , respectively .Conclusion:The repeatability and information of chromatogram peaks of the method are satisfied , which can provide credible quality control method for Cuochuang Xiaoyan lotion .
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Objective:To compare the contents of notoginsenoside R1 , ginsenoside Rg1 and ginsenoside Rb1 between Notoginseng Radix et Rhizoma and its formula granules. Methods:An HPLC method was used with a SunFire C18 column (250mm × 4. 6 mm, 5μm),the flow rate was 1. 0 ml·min-1, the detection wavelength was set at 203 nm, and the column temperature was at 30 ℃. The mobile phase was acetonitrile( A)-water( B) with gradient elution. An HPLC was used to determine the contents of the three ingredi-ents between Notoginseng Radix et Rhizoma and its formula granules, and compare the differences. Results: The total content of the three ingredients in Notoginseng Radix et Rhizoma and its formula granules was 9. 214% and 8. 646%, respectively. The total content of the three ingredients was equivalent and the daily amount of the major components in the commercial formula granules was equivalent with that in the decoction of Notoginseng Radix et Rhizoma. Conclusion:The production process of the original formula granules is re-liable, and the quality of formula granules of Notoginseng Radix et Rhizoma is stable.
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The endogenous microorganism in paridis rhizoma mainly includes bacteria and fungi,and shows different physiological activities,such as microorganism inhibition and anti-tumor activity. The principal active substance steroid saponin in paridis rhizoma can be generated from the fermentation liquor of some endogenous bacteria,and the chemical structure of vancomycin and progesterone can be transformed by the endophyte. It is supposed that paridis rhizoma may benefit from the attributions of the endogenous bacteria against illness and environment changes. It would also benefit in productivity, transformation and modification of the other active sub-metabolites and compounds in paridis rhizoma. Thus,it is valuable in drug development and source insufficiency alleviation of Chinese medicines through separation,identification,screening and clone of the endogenous microorganism in paridis rhizoma.
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Objective To establish the fingerprint of Forsythia suspensa dispensing granule by HPLC. Methods The total of 10 samples of Forsythia suspensa were analyzed by HPLC on a Waters SunFire C18 column(4. 6 mm×250 mm,5 μm) with mobile phase of A:acetonitrile and mobile phase B:0. 4% acetic acid solution as gradient elution, with flow rate at 1. 0 mL·min-1 , wavelength at 277 nm and column temperature at 30 ℃. Results There were 13 characteristic common peaks in the Forsythia suspensa dispensing granule, in which two peaks identified as forsythoside A and forsythin, the similarities were more than 0. 999. Conclusion The HPLC fingerprint of Forsythia suspensa dispensing granule is stable, and is easy to manipulate, which can provide more information for the quality control of Forsythia suspensa dispensing granule.
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Objective:To establish an HPLC method for the fingerprint determination of glycyrrhizae dispensing granules. Meth-ods:Twelve samples were analyzed by HPLC with glycyrrhizic acid as the reference. The analysis was performed on a Waters SunFire C18 column(250 mm × 4. 6 mm,5 μm) with the mobile phase A of acetonitrile and the mobile phase B of 0. 1% phosphoric acid solu-tion with gradient elution. The flow rate was 1. 0 ml·min-1 , the detection wavelength was 237nm, and the column temperature was 30℃. Results:By analyzing the fingerprint, 21 peaks existed including the peak of liquiritin and glycyrrhizic acid. The similarity of the samples was more than 0. 97. Conclusion:The established HPLC fingerprint of glycyrrhizae dispensing granules is dependable and simple. The method can provide scientific basis for the quality control of glycyrrhizae dispensing granules.
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Objective:To compare the content of total saponins in Paridis Rhizome from Wudang mountain area to explore the cor-relation between the quality of medicinal materials and the production areas and species. Methods: The content of total saponins in Paridis Rhizome was determined by an ultraviolet-visible spectrophotometer at 406nm with perchloric acid as the chromogenic reagent. Results:The saponins content in Paridis Rhizome from Wudang mountain area had obvious differences:the minimum was 1. 29%, and the maximum was up to 10. 22%. The content of total saponins had no obvious correlation with species, production area and altitude. Conclusion:The quality of Paridis Rhizome is unstable in Wudang mountain area, and that will affect the effectiveness and safety of the clinical medication. Only by promoting the standardized planting of Chinese medicine materials, the stable quality of Paridis Rhizo-me can be ensured.
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Objective: To optimize the conditions of semi-bionic extraction for Kanggan Liyan syrups. Methods: The samples were extracted by water with different pH values under the same conditions of formula composition and dosage, extraction temperature, filtration method, water voulme, centrifugal time and concentration multiple. The best conditions of the semi-bionic extraction for Kang-gan Liyan syrups were screened by uniform design with the content of forsythoside A, polydatin, baicalin and emodin and the dried ex-tract weight as the indices. Results:The best technical conditions were as follows:the pH value of water for the 1st, 2nd and 3rd de-coction was 4. 9, 7. 5 and 9. 0, respectively, and the total extraction time was 2h. Conclusion:According to the industrial production conditions, the pH value of water for the 1st, 2nd and 3rd decoction is 5. 0, 7. 5 and 9. 0 with the extraction time of 1h,0. 5h and 0. 5h, respectively.
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Objective:To establish the HPLC fingerprint for Polygonum cuspidatum dispensing granules. Methods:The HPLC fin-gerprint of 12 batches of Polygonum cuspidatum from different manufacturers were determined. The analysis was performed on a Waters SunFire C18 column(250 mm × 4. 6 mm,5μm)with acetonitrile as the mobile phase A and 0. 05% phosphoric acid solution as the mo-bile phase B with gradient elution. The flow rate was 1. 0 ml·min-1 ,the detection wavelength was 230 nm,the column temperature was 30℃,and the injection volume was 10μl. Results:The results were calculated according to“similarity evaluation system for tradi-tional Chinese medicine chromatographic fingerprint”nominated by CFDA combined with the analysis of the HPLC fingerprints. Totally 14 common peaks with similarity above 0. 98 were found in the HPLC fingerprint of Polygonum cuspidatum,including the peak respec-tively for polydatin and emodin. Conclusion:The method can provide more information for the quality control of Polygonum cuspidatum dispensing granules.
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Objective: To optimize the alcohol concentration for Jinyin Qingre oral liquids extracted by semi-bionic extraction (SBE). Methods:Using proportional division method to set up 5 alcohol concentration 30%,55%,61. 25%,67. 5%,80% for the ex-periment . The dried extract yield and the contents of chlorogenic acid ,geniposide,salviandic acid B and total phenolic acid were set up as indexes which were standardized as the comprehensive evaluation value ( Y) ,using the weighting coefficient had been set. Choosing the appropriate concentration by comparing the value of Y. Results:The order of comprehensive evaluation value was as follows:30%>61. 25% >55% >80% >67. 5%. Conclusion:Combining the clarity of the oral liquids, the best alcohol concentration in SBE for Jinyin Qingre oral liquids is 61. 25%.
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Objective:To analyze the current situation of sulfur dioxide residues in Chinese herb pieces through determining the residues in Chinese herb pieces purchased by our hospital to provide the information for the quality control of Chinese herb pieces in our hospital and ensure the clinical medication safety. Methods:The methods for the detection of sulfur dioxide residues described in Chi-nese Pharmacopoeia 2010 edition and the relative literatures were adopted. Totally 100 batches of Chinese herb pieces were selected randomly from the storage waiting products, including 10 categories of 36 batches with the limitation of 400 mg·kg-1 and the other categories of 64 batches with the limitation of 150 mg·kg-1 . Results: The sulfur dioxide residues in 14 batches were out of limits, and among them, 7 batches were over 400 mg·kg-1 and the other 7 ones were over 150 mg·kg-1 . The unqualified rate was 19. 4%and 10. 9% for the samples with the limitation of 400 mg·kg-1 and 150 mg·kg-1 , respectively. Conclusion:The detection method is simple, reproducible and rapid in determining sulfur dioxide residues in Chinese herb pieces. The exceeding standard situation of sulfur dioxide residues in Chinese herb pieces is serious, and the management on Chinese herb medicines with sulphur fumigation should be strengthened by manufacturers. Hospitals should implement the determination of sulfur dioxide residues before storage to en-sure drug safety.
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Objective:To optimize the conditions of semi-bionic extraction for Jinyin Qingre oral liquids. Methods:The best con-ditions of the semi-bionic extraction for Jinyin Qingre oral liquids was optimized by uniform design with the yield of chlorogenic acid, geniposide and total phenolic acid, and the dried extract weight as the indices in a comprehensive evaluation. Results:The optimal pH of water for the three-time decoction was 2. 89, 6. 50 and 8. 43, respectively, and the total extraction time was 2. 0 h. Conclusion:Combined with the actual production, the pH value of water is 3. 0, 6. 5 and 8. 5 with the decoction time of 1. 0, 0. 5 and 0. 5h, re-spectively.
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Objective:To establish the HPLC fingerprints of chemical constituents in Forsytiae suspensa Fructus from Shiyan dis-trict to provide scientific evidence for the quality control of Forsytiae suspensa Fructus. Methods: HPLC was performed on a Waters SunFire C18 (250 mm × 4. 6 mm, 5 μm) column and a Diamonsil C18 guard column, and the mobile phase consisted of acetonitrile-0. 4% acetic acid solution with gradient elution. The flow rate was 1 ml·min-1 , the detection wavelength was 277 nm, and the col-umn temperature was 30℃. Results:There were 14 common peaks in the HPLC fingerprints of chemical constituents in 12 batches of Forsytiae suspensa Fructus from Shiyan. The 14 characteristic peaks of Forsytiae suspensa Fructus from different habitats were under clustering analysis, and the similarity showed little difference. The contents of forsythoside A and forsythin exhibited significant differ-ence in the samples. Conclusion:The HPLC fingerprint method is simple, rapid and feasible in the quality control of Forsytiae suspen-sa Fructus.
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Objective To investigate the stability of jinyin qingre oral liquid. Methods According to the stability test guidelines for pharmaceutical preparations,the appearance,pH and relative density of jinyin qingre oral liquid were detected, the contents of geniposide,chlorogenic acid and salvia acid B were determined by HPLC. The chromatographic conditions were as follows:AtlantisT3 column(150 mm×4. 6 mm,3 μm),mobile phase A:0. 05% phosphoric acid,mobile phase B:acetonitrle, gradient elution at the flow rate of 0. 8 mL · min-1 ,and column temperature at 35 ℃. The detection wavelength was set at 254 nm. Results The appearance,pH,and relative density of jinyin qingre oral liquid did not change significantly with the acceleration test,but the contents of geniposide,chlorogenic acid and salvia acid B decreased time dependently. Conclusion Light and high temperature could decrease the stability of the jinyin qingre oral liquid.
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Objective:To optimize semi-bionic extraction(SBE)of Forsythia suspensa. Methods: The best conditions of semi-bionic extraction of Forsythia suspense were screened by uniform design with the total content of forsythoside A,and forsythin and dried extract weight as the indices. Results:The results of the uniform design were analyzed by DPS data, and combined with the industrial production conditions, the optimal extraction technology was as follows:the pH value of water in the three-time extraction was 2. 0,7. 0 and 10. 0 with the extraction time of 1. 0h,0. 5h and 0. 5h, respectively. Conclusion: The technology provides a theoretical basis for the extraction optimization of Forsythia suspensa.
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Objective:To study the effect of artificial gastric juice on the dissolution of schizandrin A to provide the parameters for the best extraction method of Schisandra chinensis. Methods:Schisandra chinensis was respectively extracted by artificial gastric juice and water. Schizandrin A in the extracts was determined by HPLC, and the dissolution of schizandrin A in artificial gastric juice and water was studied and compared. Results:At 60 min, schizandrin A dissolution was 0. 483% in artificial gastric juice, and 0. 362%in water. Conclusion:The dissolution of schizandrin A in artificial gastric juice is 33. 4% higher than that in water, suggesting artifi-cial gastric juice can significantly improve the dissolution of schisandrin A.