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目的建立枸橼酸坦度螺酮原料药中甲醇、乙醇、异丙醇、乙酸乙酯、甲苯、N,N-二甲基甲酰胺残留量的测定方法。方法采用顶空气相色谱法,DB-624毛细管柱(30 m×0.32 mm,1.80μm),柱温为40℃,保持5 min,以20℃·min-1升至220℃,保持2 min;进样口温度为200℃;FID检测器温度为250℃;样品溶剂为二甲基亚砜。结果 6种溶剂均达到完全分离;在考察的浓度范围内线性关系良好,精密度和回收率良好。结论本方法能够准确测定枸橼酸坦度螺酮原料药中的残留溶剂。
Objective To establish a method for the determination of residues of methanol, ethanol, isopropanol, ethyl acetate, toluene and N, N-dimethylformamide in tandospirone citrate. Methods The method was characterized by headspace gas chromatography (DB-624) capillary column (30 m × 0.32 mm, 1.80 μm) with a column temperature of 40 ℃ for 5 min and a temperature of 220 ℃ for 2 min at 20 ℃ · min- Inlet temperature was 200 ° C; FID detector temperature was 250 ° C; sample solvent was dimethyl sulfoxide. Results The results showed that all six solvents were completely separated. The linearity was good within the investigated concentration range and the precision and recovery were good. Conclusion This method can accurately determine residual solvent in tandospirone citrate.