2009 Vol. 27, No. 1
Display Method:
2009, 27(1): 31-32,45.
Abstract:
Objective : To improve the synthetic process of tenofovir. Methods : P-toluenesulfonic acid diethoxyphosphorylmethyl ester(4) was prepared from diethyl phosphate and paraformaldehyde by condensation and esterification.9-(2-hydroxy-propyl)adenine(7) was synthesized by reaction of adenine and propylene carbonate.In presence of(CH3)3CONa,compound(7) was connected with compound(4),and then hydrolyzed to tenofovir. Results :The technique was successfully improved due to its low cost,easier operation and less pollution to the environment. Conclusion : The overall yield of the improved synthetic process was 30%,which is more suitable for industrial production.
Objective : To improve the synthetic process of tenofovir. Methods : P-toluenesulfonic acid diethoxyphosphorylmethyl ester(4) was prepared from diethyl phosphate and paraformaldehyde by condensation and esterification.9-(2-hydroxy-propyl)adenine(7) was synthesized by reaction of adenine and propylene carbonate.In presence of(CH3)3CONa,compound(7) was connected with compound(4),and then hydrolyzed to tenofovir. Results :The technique was successfully improved due to its low cost,easier operation and less pollution to the environment. Conclusion : The overall yield of the improved synthetic process was 30%,which is more suitable for industrial production.
2009, 27(1): 33-37.
Abstract:
Objective : To develop a method for purity test and enantioseparation of ephedrine levorotatory by capillary electrophoresis(CE). Methods : The cyclodextrin,concentration,pH,organic solvent were studied,and the results indicated that the enantiomer of ephedrin and ephedrine levorotatory were baseline separated under the following experimental conditions:uncoated fused silica capillary(75 μm × 68 cm),25 mmol/L Tris,2% HP-β-CD and 1% SBE-β-CD,pH was adjusted at 3.0 by phosphoric acid,and 15 kV separation voltage.The detection wavelength was set at 214 nm with the column temperature of 15 ℃. Results : Under the experimental conditions adopted,the baseline separation of ephedrin and ephedrine levorotatory was obtained. Conclusions : The proposed method is simple,reliable and can be used for routine purity test and chiral separation.
Objective : To develop a method for purity test and enantioseparation of ephedrine levorotatory by capillary electrophoresis(CE). Methods : The cyclodextrin,concentration,pH,organic solvent were studied,and the results indicated that the enantiomer of ephedrin and ephedrine levorotatory were baseline separated under the following experimental conditions:uncoated fused silica capillary(75 μm × 68 cm),25 mmol/L Tris,2% HP-β-CD and 1% SBE-β-CD,pH was adjusted at 3.0 by phosphoric acid,and 15 kV separation voltage.The detection wavelength was set at 214 nm with the column temperature of 15 ℃. Results : Under the experimental conditions adopted,the baseline separation of ephedrin and ephedrine levorotatory was obtained. Conclusions : The proposed method is simple,reliable and can be used for routine purity test and chiral separation.
2009, 27(1): 38-39,57.
Abstract:
Objective : To study the chemical constituents of Semen Allii Fistulosi. Methods :Isolation and purification were carried out by macroporous absorption resin,silica gel,Sephadex LH-20 and RP-silica.The compounds of Semem Allii Fistulosi were identified and elucidated by spectral and chemical methods. Results :Seven compounds were obtained from water extract of Semen Allii Fistulosi and their structures were determined as adenosine(Ⅰ),2,3,4,5,6-pentahydroxyhexanoic acid(Ⅱ),2-methoxyhydroquinone(Ⅲ),S-(cis-1-propenyl)-L-cysteine(Ⅳ),S-(trans-1-propenyl)-L-cysteine(Ⅴ),trans-hinokiresinol(Ⅵ),and β-sitosterol(Ⅶ). Conclusion :All the compounds are found in Semen Allii Fistulosi for the first time,and compound Ⅵ is found in Allium for the first time.
Objective : To study the chemical constituents of Semen Allii Fistulosi. Methods :Isolation and purification were carried out by macroporous absorption resin,silica gel,Sephadex LH-20 and RP-silica.The compounds of Semem Allii Fistulosi were identified and elucidated by spectral and chemical methods. Results :Seven compounds were obtained from water extract of Semen Allii Fistulosi and their structures were determined as adenosine(Ⅰ),2,3,4,5,6-pentahydroxyhexanoic acid(Ⅱ),2-methoxyhydroquinone(Ⅲ),S-(cis-1-propenyl)-L-cysteine(Ⅳ),S-(trans-1-propenyl)-L-cysteine(Ⅴ),trans-hinokiresinol(Ⅵ),and β-sitosterol(Ⅶ). Conclusion :All the compounds are found in Semen Allii Fistulosi for the first time,and compound Ⅵ is found in Allium for the first time.
2009, 27(1): 40-42.
Abstract:
Objective : To analyze the chemical constituents of hawthorn leaves by high-performance liquid chromatography(HPLC)-diode array detector/electrospray ionization-mass spectrometry(HPLC-DAD/ESI-MS). Methods : Dried hawthorn leaves were extracted under reflux with 60% ethanol and purified by D101 macroporous resin again.The chromatographic separation was performed on a YMC ODS-C18 column(250 mm×4.6 mm i.d.;5 μm) with a mobile phase composed of aceonitrile-0.1% formic acid(1585 v/v),eluted at a flow rate of 0.6 mL/min,and UV detection was set at 254 nm.The negative ionization mode with needle voltage 3 500 V,capillary voltage-20V,gas(N2)press 21 psi and temperature of the capillary 300 ℃ was selected.Relative molecular mass data acquisition was performed from m/z 300 to 800 in full MS scan mode. Results :Eleven of the major chemical constituents of hawthorn leaves were characterized based on their retention behavior obtained on-line by their UV spectra and the HPLC-DAD/ESI-MS. Conclusion :A rapid and efficient method for studying the chemical constituents of hawthorn leaves by HPLC-DAD/ESI-MS was established.
Objective : To analyze the chemical constituents of hawthorn leaves by high-performance liquid chromatography(HPLC)-diode array detector/electrospray ionization-mass spectrometry(HPLC-DAD/ESI-MS). Methods : Dried hawthorn leaves were extracted under reflux with 60% ethanol and purified by D101 macroporous resin again.The chromatographic separation was performed on a YMC ODS-C18 column(250 mm×4.6 mm i.d.;5 μm) with a mobile phase composed of aceonitrile-0.1% formic acid(1585 v/v),eluted at a flow rate of 0.6 mL/min,and UV detection was set at 254 nm.The negative ionization mode with needle voltage 3 500 V,capillary voltage-20V,gas(N2)press 21 psi and temperature of the capillary 300 ℃ was selected.Relative molecular mass data acquisition was performed from m/z 300 to 800 in full MS scan mode. Results :Eleven of the major chemical constituents of hawthorn leaves were characterized based on their retention behavior obtained on-line by their UV spectra and the HPLC-DAD/ESI-MS. Conclusion :A rapid and efficient method for studying the chemical constituents of hawthorn leaves by HPLC-DAD/ESI-MS was established.
2009, 27(1): 43-45.
Abstract:
Objective : To establish a nitrogen determination method for determining capsaicin in rotenone-capsaicin suspension. Methods : The capsaicin of suspension was determined by the nitrogen determination method.The results were regulated by blank control and protein control. Results :The content in suspension was 0.25 g/100 mL and RSD was 1.77%.The mean average recovery of the method was 100.67% and RSD was 1.65%.The error of the protein influence was in control. Conclusion :The method was simple and accurate.It could be used to quality control of the rotenone-capsaicin suspension.
Objective : To establish a nitrogen determination method for determining capsaicin in rotenone-capsaicin suspension. Methods : The capsaicin of suspension was determined by the nitrogen determination method.The results were regulated by blank control and protein control. Results :The content in suspension was 0.25 g/100 mL and RSD was 1.77%.The mean average recovery of the method was 100.67% and RSD was 1.65%.The error of the protein influence was in control. Conclusion :The method was simple and accurate.It could be used to quality control of the rotenone-capsaicin suspension.
2009, 27(1): 46-48,50.
Abstract:
Objective : To optimize the extraction methods and GC-MS analysis of volatile oil in Rhizoma Zingiberis. Methods : The distilled water volume,ultrasonic time,soaking time and extraction time were optimized by orthogonal design and GC-MS chromatogram was obtained. Results :The yield of volatile oil was 1.89% by orthogonal design.Also,a stable,reliable chromatogram was obtained under optimized GC-MS conditions. Conclusion :The design can be applied for optimizing the extraction condition of volatile oil in Rhizoma Zingiberis and 49 compounds were identified by GC-MS analysis.
Objective : To optimize the extraction methods and GC-MS analysis of volatile oil in Rhizoma Zingiberis. Methods : The distilled water volume,ultrasonic time,soaking time and extraction time were optimized by orthogonal design and GC-MS chromatogram was obtained. Results :The yield of volatile oil was 1.89% by orthogonal design.Also,a stable,reliable chromatogram was obtained under optimized GC-MS conditions. Conclusion :The design can be applied for optimizing the extraction condition of volatile oil in Rhizoma Zingiberis and 49 compounds were identified by GC-MS analysis.
2009, 27(1): 49-50.
Abstract:
Objective : To identify Semen Celosiae from different districts and its adulterant C.cristata L.. Methods : TG/DTA and thermal analyser were both used to scan and analyse the thermal map of Semen Celosiae from different districts and its adulterant Celosia cristata L.The experiment conditions are: asensitivity of ±50 uV,a calefactive rate of 15 ℃/min,an ambience of nitrogen and velocity of flow is 50 mL/min. Results :The thermal curves of Semen Celosiae and its adulterant Celosia.cristata L.represent that there were significant differences between them and each with characteristics,which means this experience has achieved an obverious differentiating effect. Conclusion :Differential thermal analysis method for accurate identification of traditional chinese medicine is simple,rapid and worthy of application.
Objective : To identify Semen Celosiae from different districts and its adulterant C.cristata L.. Methods : TG/DTA and thermal analyser were both used to scan and analyse the thermal map of Semen Celosiae from different districts and its adulterant Celosia cristata L.The experiment conditions are: asensitivity of ±50 uV,a calefactive rate of 15 ℃/min,an ambience of nitrogen and velocity of flow is 50 mL/min. Results :The thermal curves of Semen Celosiae and its adulterant Celosia.cristata L.represent that there were significant differences between them and each with characteristics,which means this experience has achieved an obverious differentiating effect. Conclusion :Differential thermal analysis method for accurate identification of traditional chinese medicine is simple,rapid and worthy of application.
The analyses of the trends and effect factors about drug expenditure of American health institutions
2009, 27(1): 51-53,60.
Abstract:
Objective : To analyze the trends and effect factors of the drug expenditure in American health institutions and describe some rules. Methods :literatures about drug expenditure of pharmacies in American health system were collected and the relationship between drug expenditure and the factors was described. Results and Conclusion :The growth of the prescription drug expenditure in American health institutions has a significant decrease in the growth rate,but total drug expenditure remain a high growth.The primary factors that affect the drug expenditure are new drug's marketing and generic drugs.
Objective : To analyze the trends and effect factors of the drug expenditure in American health institutions and describe some rules. Methods :literatures about drug expenditure of pharmacies in American health system were collected and the relationship between drug expenditure and the factors was described. Results and Conclusion :The growth of the prescription drug expenditure in American health institutions has a significant decrease in the growth rate,but total drug expenditure remain a high growth.The primary factors that affect the drug expenditure are new drug's marketing and generic drugs.
2009, 27(1): 58-60.
Abstract:
Objective : To select the optimal condition of polyamide column adsorption chromatogtaphy for separating the total flavonoids in Rhodobryum giganteum(Schwaegr.) Par. Methods :The amount of polyamide,the eluting reagent and the eluting rate were studied. Results :It was suitable when the herb amount:polyamide amount was 11,and 50% ethnoal was the sutiable eluting reagent.The flow rate of eluent was 2 times volume of column/h. Conclusion :polyamide is suitable for the separation and collection of the total flavonoids from Rhodobryum giganteum(Schwaegr.) Par.
Objective : To select the optimal condition of polyamide column adsorption chromatogtaphy for separating the total flavonoids in Rhodobryum giganteum(Schwaegr.) Par. Methods :The amount of polyamide,the eluting reagent and the eluting rate were studied. Results :It was suitable when the herb amount:polyamide amount was 11,and 50% ethnoal was the sutiable eluting reagent.The flow rate of eluent was 2 times volume of column/h. Conclusion :polyamide is suitable for the separation and collection of the total flavonoids from Rhodobryum giganteum(Schwaegr.) Par.
2009, 27(1): 61-62.
Abstract:
Objective : To establish a clustering analysis of microsphere by near-infrared diffuse reflectance spectrometry. Methods : Near-infrared diffuse reflectance spectroscopy combined with clustering analysis was used in the identification of microsphere. Results :The results of clustering analysis are obviously different,and the three samples of microspheres can be distinguished. Conclusions :This method is rapid,simple,low cost and can be used in the identification and quality control of microsphere.
Objective : To establish a clustering analysis of microsphere by near-infrared diffuse reflectance spectrometry. Methods : Near-infrared diffuse reflectance spectroscopy combined with clustering analysis was used in the identification of microsphere. Results :The results of clustering analysis are obviously different,and the three samples of microspheres can be distinguished. Conclusions :This method is rapid,simple,low cost and can be used in the identification and quality control of microsphere.
2009, 27(1): 63-65.
Abstract:
Objective : To develop a HPLC method to determine the content of 3 flavonoids in Potentilla chinensis ser. Methods : ZORBAX SB-C18 column(4.6mm×150mm,5μm) was used,and the mobile phase was methanol-0.3% Phosphoric acid(51:49) with the flow rate of 0.9 mL/min and the detection wanelength at 360 nm. Results :The linear ranges of quercetin,potengriffioside A and apigenin were 0.72～10.08 μg/mL,0.86～12.04μg/mL and 0.54～7.56μg/mL,respectively(r= 0.999 9);the average recovery was 95.37%,96.87% and 97.66%,the RSD was 1.79%,1.63% and 2.08%,respectively;the content of these three flavonoids in the herb was 100μg/g、323μg/g and 55μg/g,respectively. Conclusion :This method is fast,and reliable convenient,which refers to the assay of flavanoids in Potentilla chinensis.
Objective : To develop a HPLC method to determine the content of 3 flavonoids in Potentilla chinensis ser. Methods : ZORBAX SB-C18 column(4.6mm×150mm,5μm) was used,and the mobile phase was methanol-0.3% Phosphoric acid(51:49) with the flow rate of 0.9 mL/min and the detection wanelength at 360 nm. Results :The linear ranges of quercetin,potengriffioside A and apigenin were 0.72～10.08 μg/mL,0.86～12.04μg/mL and 0.54～7.56μg/mL,respectively(r= 0.999 9);the average recovery was 95.37%,96.87% and 97.66%,the RSD was 1.79%,1.63% and 2.08%,respectively;the content of these three flavonoids in the herb was 100μg/g、323μg/g and 55μg/g,respectively. Conclusion :This method is fast,and reliable convenient,which refers to the assay of flavanoids in Potentilla chinensis.
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