Determination of Residual Organic Solvents in Raw Medicine of Solifenacin Succinate by GC and HPLC

A GC method was developed for the determination of 8 residual organic solvents, i.e., methanol, ethanol, acetone, tert-butyl alcohol, ethyl acetate, n-heptane, petroleum ether and toluene, and HPLC was applied to the determination of pyridine, in raw medicine of solifenacin succinate. In GC analysis N,N-dimethylformamide was used as solvent, a TR-5 capillary column was used as a separation column, and FID was adopted. In HPLC analysis an AQ-C18 column was used for separation of pyridine, with the mobile phase consisted of acetonitrile and 50 mmol·L-1 of disodium hydrogen phosphate (containing 0.1% triethylamine, pH 7.6). UV detection wavelength was 254 nm. The linear relationship between the peak areas and the mass concentrations of 9 solvent was found in certain ranges. The detection limit of pyridine was 0.01 mg·L-1 and those of the other 8 solvents were in the range of 1.17-5.00 mg·L-1. The recovery rates obtained by standard addition method were in the range of 86.3%-101%, and RSDs (n=6) were in the range of 2.4%-6.3%.