顶空气相色谱法测定硫酸羟氯喹原料药中的7种残留溶剂

Determination of 7 Residual Organic Solvents in Hydroxychloroquine Sulfate by Headspace Gas Chromatography

目的建立顶空气相色谱法测定硫酸羟氯喹原料药中的残留溶剂。方法采用顶空毛细管气相色谱法,色谱柱为Agilent DB-624毛细管色谱柱（30 m×0.25 mm,1.4μm）,柱温采用程序升温（初始温度45℃,保持8 min,以35℃·min^-1的速度升温至220℃,保持1 min）,检测器为氢火焰离子化检测器。进样口温度为250℃,检测器温度为280℃,载气为氮气,流速为1.0 mL·min^-1,分流比为5∶1,顶空温度为90℃,平衡时间为30 min,进样体积为1 mL。结果 7种溶剂均有良好的分离度,在考察的浓度范围内与峰面积均具有良好的线性关系,r=0.999 6-1.000,平均加样回收率为93.5%-107.7%（RSD为2.8%-5.2%,n=6）。结论该法简便快捷,灵敏度好,能准确有效地控制硫酸羟氯喹的质量。

OBJECTIVE To establish a method for the determination of residual organic solvents in hydroxychloroquine sulfate by headspace gas chromatography. METHODS Headspace capillary GC method was adopted. The determination was performed on DB- 624 capillary column at the rate of 1.0 mL · min^-1 using nitrogen gas as carrier gas and FID as the detector by temperature programming （ initial column temperature at 45℃ ,maintained for 8 rain,then raised to 220 ℃ at a rate of 35 ℃ · min^-1 and maintained for 1 min）. The split ratio was 5 ： 1, the temperature of the injector was maintained at 250℃ and that of detector at 250 %. The equilibrium temperature was 90 ℃ and equilibrium time was 30 min. The volume of sample was 1 mL. RESULTS The 7 solvents were separated completely. There was a good linearity relationship between the peak area and the concentration of each solvent （r=0.999 6-1.000 0）. The average recovery of the 7 solvents was 93.5% - 107.7% （ RSD was 2.8% - 5.2%, n = 6 ）. CONCLUSION This method is convenient and fast for the quantitative determination of residual organtc solvents in hydroxychloroquine sulfate, and can be used for its quality control.