High performance liquid chromatography with a C18 reverse-phase column was used to separate the five components in cough syrup,including acetaminophen,p-aminophenol,caffeine,chlorphenamine maleate and guaifenesin.The ...High performance liquid chromatography with a C18 reverse-phase column was used to separate the five components in cough syrup,including acetaminophen,p-aminophenol,caffeine,chlorphenamine maleate and guaifenesin.The mobile phase consists of 15wt% acetonitrile,0.004mol/L sodium heptyl sulfonate, 0.03mole/L potassium di-hydrogen phosphate and triethylamine (volume ratio 13∶40∶44∶3),the pH of which is adjusted to 3.0 by phosphoric acid.The contents of the five components are analyzed on an ultraviolet spectrophotometer at 254nm,with a flow rate of 0.4mL/min.The results show that the calibration curves are linear in a certain range.The average recovery of five components is between 96.31% and 102.3%.展开更多
Si-Mo-Tang（SMT） oral liquid preparation, a traditional Chinese medicine, was prepared from four crude herbal drugs, Fructus Aurantii Submaturus, Radix Aucklandiae, Semen Arecae and Radix Linderae Aggregatae. A combi...Si-Mo-Tang（SMT） oral liquid preparation, a traditional Chinese medicine, was prepared from four crude herbal drugs, Fructus Aurantii Submaturus, Radix Aucklandiae, Semen Arecae and Radix Linderae Aggregatae. A combinative method using HPLC fingerprint and quantitative analysis was developed and validated for quality consistency evaluation of SMT. Individual HPLC chromatograms were evaluated against the mean chromatogram generated via a similarity evaluation computer program. Data from chromatographic fingerprints were also processed with principal component analysis（PCA） and hierarchical cluster analysis（HCA）. Additionally, six components （naringin, isonaringin, hesperidin, neohesperidin, norisoboldine and potassium sorbate） in SMT were simultaneously determined to interpret the quality consistency. For fingerprint analysis, 20 peaks were selected as the characteristic peaks to evaluate the similarities of 26 SMT collected from different manufacturers. Among the 20 characteristic peaks, 10 peaks were assigned to be naringin, hesperidin, neohesperidin, isonaringin, neoeriocitrin, tangeretin, nobiletin, norisoboldine, 5-（ethoxymethyl）furan-2-carbaldehyde and potassium sorbate, respectively. The results of similarity analysis, PCA and HCA, indicate that the samples from different manufacturers were consistent with each other in composition. The results from the quantitative data show that the contents of six compounds were significantly different in SMT oral liquid preparations from different manufacturers. The combinative method of chromatographic fingerprint with quantitative analysis developed here offered an efficient way for the quality consistency evaluation of the traditional Chinese medicine SMT.展开更多
Five different methods were tested and compared to prepare danofloxacin mesylate liposomes, the ammonium sulfate gradient method with freeze-thawing steps was validated as the best one; the optimal preparation conditi...Five different methods were tested and compared to prepare danofloxacin mesylate liposomes, the ammonium sulfate gradient method with freeze-thawing steps was validated as the best one; the optimal preparation condition confirmed by orthogonal experiment was as follows： EPC-CH ratio was 3 ： 2 and 2.6% SA was added to gain the positive electricity; drug-lipoid was 2 ： 5, the concentration of ammonium sulfate was 250 mmol·L-1, water-oil ratio was 1：5, and they were incubated at 35℃ for 15 min. The prepared liposome products were ivory white semitransparent suspension, the electron microscope appearance was intact and globular or globular-like vesicles with uniformed distribution; the particle size was centralized from 3 to 7 gm, zeta-electric potential valued＋ （15.92＋1.49） mV, pH valued 6.02~0.09; HPLC method was established in quantitative analyses of danofloxacin and reverse dialysis with RP-HPLC method was validated for determination of entrapment efficiency. The entrapment efficiency results were all above 90%. They were stored at 4℃ with satisfied stability. Six months later, the appearance, characters and entrapment efficiency were almost with no change展开更多
文摘High performance liquid chromatography with a C18 reverse-phase column was used to separate the five components in cough syrup,including acetaminophen,p-aminophenol,caffeine,chlorphenamine maleate and guaifenesin.The mobile phase consists of 15wt% acetonitrile,0.004mol/L sodium heptyl sulfonate, 0.03mole/L potassium di-hydrogen phosphate and triethylamine (volume ratio 13∶40∶44∶3),the pH of which is adjusted to 3.0 by phosphoric acid.The contents of the five components are analyzed on an ultraviolet spectrophotometer at 254nm,with a flow rate of 0.4mL/min.The results show that the calibration curves are linear in a certain range.The average recovery of five components is between 96.31% and 102.3%.
基金Supported by the National Basic Research Program of China(No.2009CB523002)the National Action of Technology Personnel Servicing Enterprise Program of China(No.2009FJ5049)+1 种基金the Foundation of Hunan Science and Technology Committee, China(No.2009XK6032, 2009-152)the Foundation of Hunan Educational Committee, China(No.09CY001)
文摘Si-Mo-Tang（SMT） oral liquid preparation, a traditional Chinese medicine, was prepared from four crude herbal drugs, Fructus Aurantii Submaturus, Radix Aucklandiae, Semen Arecae and Radix Linderae Aggregatae. A combinative method using HPLC fingerprint and quantitative analysis was developed and validated for quality consistency evaluation of SMT. Individual HPLC chromatograms were evaluated against the mean chromatogram generated via a similarity evaluation computer program. Data from chromatographic fingerprints were also processed with principal component analysis（PCA） and hierarchical cluster analysis（HCA）. Additionally, six components （naringin, isonaringin, hesperidin, neohesperidin, norisoboldine and potassium sorbate） in SMT were simultaneously determined to interpret the quality consistency. For fingerprint analysis, 20 peaks were selected as the characteristic peaks to evaluate the similarities of 26 SMT collected from different manufacturers. Among the 20 characteristic peaks, 10 peaks were assigned to be naringin, hesperidin, neohesperidin, isonaringin, neoeriocitrin, tangeretin, nobiletin, norisoboldine, 5-（ethoxymethyl）furan-2-carbaldehyde and potassium sorbate, respectively. The results of similarity analysis, PCA and HCA, indicate that the samples from different manufacturers were consistent with each other in composition. The results from the quantitative data show that the contents of six compounds were significantly different in SMT oral liquid preparations from different manufacturers. The combinative method of chromatographic fingerprint with quantitative analysis developed here offered an efficient way for the quality consistency evaluation of the traditional Chinese medicine SMT.
基金Supported by Harbin Scientific and Technical Innovation Foundation (RC2007QH002031)
文摘Five different methods were tested and compared to prepare danofloxacin mesylate liposomes, the ammonium sulfate gradient method with freeze-thawing steps was validated as the best one; the optimal preparation condition confirmed by orthogonal experiment was as follows： EPC-CH ratio was 3 ： 2 and 2.6% SA was added to gain the positive electricity; drug-lipoid was 2 ： 5, the concentration of ammonium sulfate was 250 mmol·L-1, water-oil ratio was 1：5, and they were incubated at 35℃ for 15 min. The prepared liposome products were ivory white semitransparent suspension, the electron microscope appearance was intact and globular or globular-like vesicles with uniformed distribution; the particle size was centralized from 3 to 7 gm, zeta-electric potential valued＋ （15.92＋1.49） mV, pH valued 6.02~0.09; HPLC method was established in quantitative analyses of danofloxacin and reverse dialysis with RP-HPLC method was validated for determination of entrapment efficiency. The entrapment efficiency results were all above 90%. They were stored at 4℃ with satisfied stability. Six months later, the appearance, characters and entrapment efficiency were almost with no change
