气相色谱法与高效液相色谱法测定琥珀酸索利那新原料药中的残留溶剂

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

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AQC18色谱柱为分离柱,以50mmol·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254nm。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0.01mg·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 8residual 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-5capillary 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 and50mmol· 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 9solvent was found in certain ranges.The detection limit of pyridine was 0.01 mg·L-1 and those of the other 8solvents were in the range of 1.17-5.00mg·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%.