摘要
采用气相色谱法检测盐酸氟西汀原料中CHCl3和正己烷残留量。色谱柱：DB-17（50％二苯基／50％甲基硅氧烷，0．25mm i．d．×30m，0．25μm）；载气：H2（30mL／min），AIR（350mL／min），Make up＋Const col（N2）：35mL／min；进样口温度：250℃；检测器温度：250℃；柱温：60℃；不分流模式；Split柱流速：2mL／min；进样量：1μL。正己烷在157．2～393．0ng范围内，CHCl3在5．88～117．6ng范围内，峰面积与浓度之间线性性关系良好。检出限：信噪比3：1时，正己烷LOD： 2．62ng；CHCl3 LOD：2．94ng。定量限：信噪比10：1时，正己烷LOQ：2．62ng；CHCl3 LOQ：5．88ng。正己烷、氯仿理论塔板数分别为171513、206764。本法可检测盐酸氟西汀原料中有机溶剂残留量，为其质量控制提供依据。
To detect organic solvent residues （hexane and chloroform） in fluoxetine hydrochloride. Methods detections of chloroform and hexane were performed by gas chromatography （GC） with DB-17 column （0.25 μm×0.25 mm×30 m） and hydrogen as carrier gas at a flow rate of 2 mL/min. AIR （350 mL/min）. Make up ＋ Const col（N2） ： 35 mL/ min. Inlet, detector and column temperatures were 250, 250 and 60 ℃ respectively. Split mode. Injection volume was 1 μL. The detection limits were 2.62 μg/mL×1 μL = 2.62 ng and 5.88 μg/mL×1 μL = 5.88 ng for hexane and chloroform respectively （S/N = 3）. There were good linear relationships found at the concentrations of 157.2-393.0 ng for hexane anti 5.88-117.6 ng for chloroform. Theoretical plate numbers were 171513 （hexane） and 206764 （chloroform）. There were no residual hexane and chloroform detected in fluoxetine hydrochloride by the GC methods mentioned above. Conclusion Gas chromatography （GC） was simple, convenient, sensitive and feasible for the detection of residual hexane and chloroform in fluoxetine hydrochloride and applicable for quality control of fluoxetine hydrochloride.
出处
《分析试验室》
CAS
CSCD
北大核心
2008年第8期45-47,共3页
Chinese Journal of Analysis Laboratory
关键词
气相色谱法
盐酸氟西汀
CHCl3
正己烷
溶剂残留
Gas chromatography （GC）
Fluoxetine hydrochloride
Hexane
Chloroform
Solvent residue
