顶空气相色谱法同时测定索拉非尼中8种残留溶剂的含量

Simultaneous Determination of Eight Residual Solvents in Sorafenib by Headspace Gas Chromatography

目的建立顶空毛细管气相色谱法同时测定索拉非尼中8种残留溶剂含量的方法。方法采用顶空气相色谱法,色谱柱为DB-624毛细管柱,程序升温:初始温度为40℃,保持5 min,以10℃/min升温至100℃,再以20℃/min升温至200℃,保持5 min,进样口温度为230℃,采用氢火焰离子化检测器,检测器温度为250℃,载气为氮气,流速为2.0 ml/min,顶空平衡温度为80℃,平衡时间为20 min。结果甲醇、丙酮、乙酸甲酯、叔丁醇、乙酸乙酯、四氢呋喃、甲基异丁基酮、甲苯能完全分离,分别在48.92~342.44,82.48~577.36,82.78~579.43,82.92~580.44,83.37~583.58,12.06~84.45,83.75~586.26,14.63~102.42μg/ml范围内线性关系良好(r≥0.9990);平均加样回收率分别为102.12%(RSD=2.11%),103.57%(RSD=1.58%),103.82%(RSD=1.38%),102.72%(RSD=1.14%)103.42%(RSD=2.61%),104.52%(RSD=1.22%),103.72%(RSD=0.79%)和103.67%(RSD=1.74%)。结论此法灵敏度高,操作简便,准确可靠,可用于索拉非尼中8种残留溶剂的测定。

Objective To establish a headspace capillary gas chromatography method for the simultaneous determination of eight residual solvents in sorafenib.Methods A headspace gas chromatography was used to separate the residual solvents on a DB-624 capillary column with an FID detector.The programmed column temperature was set as follows:initial temperature of 40℃for 5 minutes,raised to 100℃at the rate of 10℃/min,then raised to 200℃at the rate of 20℃/min,maintained for 5 minutes.The temperature of the injector was 230℃and that of the FID was 250℃.The carrier gas was nitrogen at a flow rate of 2.0 ml/min.The containers of headspace injector were in equilibrium at 80℃for 20 minutes.Results Methanol,acetone,methyl acetate,tert-butanol,ethyl acetate,tetrahydrofuran,methyl isobutyl ketone and toluene could be completely separated with good linear relationships.The eight solvents have good linear relationships within the ranges of 48.92-342.44,82.48-577.36,82.78-579.43,82.92-580.44,83.37-583.58,12.06-84.45,83.75-586.26 and 14.63-102.42μg/ml(r≥0.9990),respectively.The average recoveries of the eight solvents were 102.12%(RSD=2.11%),103.57%(RSD=1.58%),103.82%(RSD=1.38%),102.72%(RSD=1.14%),103.42%(RSD=2.61%),104.52%(RSD=1.22%),103.72%(RSD=0.79%)and 103.67%(RSD=1.74%),respectively.Conclusion The method is sensitive,simple and accurate for the simultaneous determination of eight residual solvents in sorafenib.