建立了测定琥珀酸索利那新原料药中残留溶剂甲醇、乙醇、丙酮、叔丁醇、乙酸乙酯、正庚烷、石油醚、甲苯的气相色谱法和测定吡啶的高效液相色谱法。气相色谱法中以N,N-二甲基甲酰胺为溶剂,以TR-5毛细管柱为分离柱,采用氢火焰离子化检测器。高效液相色谱法中以AQ-C18色谱柱为分离柱,以50 mmol·L-1磷酸氢二钠水溶液(含0.1%三乙胺,pH为7.6)-乙腈(1+1)为流动相,检测波长为254 nm。9种溶剂的质量浓度在一定范围内呈线性,吡啶的检出限为0.01 mg·L-1,其余8种溶剂的检出限在1.17~5.00 mg·L-1之间,加标回收率在86.3%~101%之间,相对标准偏差(n=6)在2.4%~6.3%之间。

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%.