顶空气相色谱法测定依匹必利原料药中有机溶剂残留量

目的:建立以顶空气相色谱法测定依匹必利原料药中3种有机溶剂甲醇、乙醚、三乙胺残留量的方法。方法:采用顶空进样法,以二甲基甲酰胺为溶剂,甲苯为内标,平衡温度70℃,平衡时间30min。气相色谱条件中采用OV1701色谱柱;程序升温:40℃维持2min,以5℃·min-1的速率升至180℃,维持10min;气化室温度为200℃,检测器温度为260℃;载气为氮气,流速为5mL·min-1。结果:甲醇、乙醚、三乙胺检测浓度线性范围分别为53.8～376.6、62.0～434.0、20.2～141.4μg·mL-1(r均>0.9949);回收率均>98.1%,RSD均<1.9%。样品中3种有机溶剂残留量甲醇<0.092%、乙醚<0.0021%、三乙胺<0.00015%。结论:所建立方法灵敏、准确、可靠,适用于依匹必利原料药中有机溶剂残留量的测定。

Determination of Residue Level of Organic Solvents in Epidepride by Head Space Gas Chromatography

OBJECTIVE： To establish a head space gas chromatography method for quantification of residue level of methanol, ether and triethylamine in epidepride crude drug. METHODS： Head space GC was employed for the determination with dimethylformamide as solvent and methylbenzol as internal standard. The equilibrium temperature was 70℃ and the equilibrium time was 30 min. In GC, OV1701 chromatographic column was used with temperature programming with the initial column temperature kept at 40℃ for 2 min, and then the column temperature increased to 180℃ （maintained for 10 min） at an increasing rate of 5℃·min^-1. The gasification temperature was 200℃ and the FID detector was kept at 260℃. Nitrogen gas was used as carrier gas at a flow rate of 5mL·min^-1. RESULTS： The linear ranges of methanol, ether and triethylamine were 53.8-376.6, 62.0-434.0 and 20.2-141.4μg·mL^-1, respectively （R 〉0.994 9 for all） ; the average recovery rates of all were above 98.1% with RSDs all less than 1.9%. The residue levels of methanol, ether and triethylamine in sample were less than 0.092%, 0.002 1% and 0.000 15%, respectively. CONCLUSION： The established method is sensitive, accurate and reliable and it is applicable for the determination of the residue level of the organic solvents in epidepride crude drug.