摘要
目的:建立同时测定盐酸帕罗西汀原料药中4种有机溶剂异丙醇、二氯甲烷、甲醇及丙酮残留量的顶空-气相色谱方法。方法:色谱柱为Agilent CP-Volamine毛细管柱,程序升温,高纯氮气作为载气,分流比10∶1,流速为3.0 mL/min,进样口温度200℃,检测器为FID检测器,温度为230℃,顶空加热温度85℃,平衡时间30 min。结果:甲醇、丙酮、异丙醇和二氯甲烷检测限均低于15μg/ml;定量限均低于45μg/mL;质量浓度线性范围分别为100~2500μg/mL(r2=0.9998)、200~5000μg/mL(r2=0.9996)、20~500μg/mL(r2=0.9996)、30~750μg/mL(r2=0.9997);各杂质的加样回收率均在93.09%~100.80%(n=9)。精密度RSD均小于3.2%,重复性RSD均小于2.9%。结论:该方法灵敏度高、重复性好、结果准确可靠、适用于测定盐酸帕罗西汀原料药4种有机溶剂的残留。
A headspace gas chromatographic method was established for the simultaneous determination of four organic solvents which is isopropanol, dichloromethane, methanol and acetone residues in paroxetine hydrochloride API. METHODS:Under the headspace gas chromatography, an Agilent CP volamine capillary column was used for temperature programming. The carrier gas is high-purity nitrogen with a flow rate of 3.0 ml/min, and the split ratio is 10:1.With the temperature of injection port 200 ℃, detector 230 ℃, headspace heating 85 ℃, the equilibrium time is 30 min. RESULTS: The linear ranges of methanol, acetone, isopropanol and dichloromethane were 100~2500μg/mL(r2=0.9998)、200~5000μg/mL(r2=0.9996)、20~500μg/mL(r2=0.9996)、30~750μg/mL(r2=0.9997);The average recoveries were ranged from 93.09%~100.80%(n=9). RSD of the precision and repeatability were 3.2%and 2.9%(n=6)respectively. Conclusion: This method was simple, rapid, sensitive, with good specificity, and it can be used for the determination of the residual organic solvent in Paroxetine Hydrochloride API.
作者
段立广
付冉
Duan Liguang;Fu Ran(The Frist Hospital of Hebei Medical University,Dept.of Pharmacy,Shijiazhuang 050000,China)
出处
《科学技术创新》
2022年第11期73-76,共4页
Scientific and Technological Innovation
