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目的:建立毛细管气相色谱法测定枸橼酸他莫昔芬原料药中有机溶剂残留量的方法。方法:色谱柱:DB-624(30 m×0.53mm×3μm)弹性石英毛细管柱;柱温采用程序升温:起始40℃,保持13 min,20℃/min升至230℃,保持15 min;氢火焰离子化检测器,载气:氮气,流速:3.0 ml·min~(-1),进样口温度:140℃;检测器温度:250℃;分流比为5:1。结果:甲醇、丙酮、乙酸乙酯、四氢呋喃及甲苯浓度的线性均在各自浓度范围内,线性关系良好。平均回收率为:95.1%～98.1%。结论:方法操作简便、结果准确可靠,可以用于枸橼酸他莫昔芬原料药中有机溶剂残留的测定。
Objective: To establish a method for the determination of residual organic solvents in tamoxifen citrate capsules by capillary gas chromatography. Methods: Column: DB-624 (30 m × 0.53 mm × 3 μm) elastic quartz capillary column. The temperature of column was raised by programmed temperature from 40 ℃ for 13 min and then to 230 ℃ for 20 min / Flame ionization detector, carrier gas: nitrogen, flow rate: 3.0 ml · min -1, inlet temperature: 140 ℃, detector temperature: 250 ℃, split ratio 5: 1. Results: The linearity of methanol, acetone, ethyl acetate, tetrahydrofuran and toluene concentrations were in the range of their respective concentrations with good linearity. The average recovery was: 95.1% ~ 98.1%. Conclusion: The method is simple, accurate and reliable, and can be used for the determination of organic solvent residues in tamoxifen citrate raw materials.