GC测定枸橼酸坦度螺酮中的残留溶剂

Determination of Residual Organic Solvents in Tandospirone Citrate by GC

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 develop a headspace GC method for the determination of residual organic solvents such as methanol, ethanol, iso-propyl alcohol, ethyl acetate, methylbenzene, N,N-dimethylformamide in tandospirone citrate. METHODS Headspace GC was adopted using a DB-624 column（30m×0.32 mm, 1.80 μm）, the column temperature was maintained at 40 ℃ for 5 min, then was raised to 220 ℃ at the rate of 20 ℃·min-1 and maintained at 220 ℃ for 2 min. The injection port temperature was 200 ℃; the FID detector temperature was 250 ℃; the sample was dissolved in DMSO. RESULTS Six residual solvents were separated completely. It was appeared to present a good linearity within the experimental concentration, and the precision and recoveries were good. CONCLUSION The method can be used for the determination of the residual solvents in tandospirone citrate.