ABSTRACT
Objective:To develop a method for the quantitative determination of ambrisentan. Methods: 1 H NMR spectra were obtalned with a Bruker AscendTM 400 superconducting NMR spectrometer. For each sample, DMSO-D6 was used as the solvent, the pulse width was 10. 0 μs, the delay time was 5 s and the scanning time was 16. Results: The proton peaks of ambrisentan at δ6. 16 ppm and maleic acid atδ6. 28 ppm were used as the quantitative peaks. The linear regression equation of peak area and quality ratio was Y=0. 140 7X+0. 034 8 with the correlation coefficient of 0. 999 4. RSD was 0. 2%(n=6)in the repeated experiments. The absolute content of ambrisentan reference substance was 99. 9%. Conclusion: The results showed that 1 H NMR can be used in the quantitative determination of ambrisentan without reference substance. The method is reliable, rapid, accurate and simple.
ABSTRACT
This study was aimed to identify the main related substance in baicalein in order to provide basic study data for the safety, efficacy and quality control of the medicine. The analysis was carried out on activated carbon and silica gel column. The compound structure was identified by spectral analysis, which included UV, IR, NMR and MS. The results showed that the related substance was identified as oroxylin A. It was concluded that the determina-tion provided scientific data for studying the impurities of baicalein and improving its quality.
ABSTRACT
This study was aimed to establish a HPLC fingerprint of saponins in Sanjie-zhentong Capsule in order to make a quantitative analysis of the quality of Sanjie-zhentong Capsule. The Waters Symmetry ShieldTM RP18 (4.6 mmí 250 mm, 5 μm) column was used with a mobile phase of acetonitrile-water gradient elution. The flow rate was 1.2 mL/min. The column temperature was 30℃. The detection wavelength was 203 nm. The results showed that the fingerprint chromatography included 9 mutual peaks. The similarity among batches was more than 0.95. Compared with reference substance, five characteristic components were recognized. The five components are notoginsenoside R1, ginsenoside Rg1, ginsenoside Re, ginsenoside Rb1 and ginsenoside Rd. It was concluded that this method was rapid, simple and accurate and can be used as one of the effective methods for the quality control of Sanjie-zhen-tong Capsule.
ABSTRACT
<p><b>OBJECTIVE</b>To establish the chromatographic fingerprint for the quality control of gamboge.</p><p><b>METHOD</b>Analysis on a Luna C8 (4.6 mm x 250 mm, 5 microm) column eluted with mobile phases containing acetonitrile and 0.1% glacial acetic acid in water in gradient mode. The flow rate was 1.0 mL x min(-1) and the detection wavelength was at 362 nm. The temperature of column was 25 degrees C. And data of 11 batches of gamboge samples from different sources were analysed by "similarity evaluation for chromatographic Fingerprint of Traditional Chinese Medicine" software.</p><p><b>RESULT</b>Thirteen common peaks were selected in chromatograms, and all the common peeks were separated effectively.</p><p><b>CONCLUSION</b>The precision, repeatability, and stability of this method were satisfying. The method developed can be used to identify and evaluate the quality of gamboge.</p>