毛细管气相色谱法测定联苯双酯有机溶剂的残留量

目的建立气相色谱法测定联苯双酯中3种有机溶剂的残留量的方法。方法采用DB-624毛细管色谱柱（30.0m×0.53mm×3μm）;进样口温度为200℃;FID检测器温度为260℃;柱温：程序升温,60℃保持5min,然后以20℃/min的速率升温220℃,保持5min;以氮气为载气,恒压模式,载气压力为2.4psi;直接进样,进样量为1μL;以二甲基亚砜为溶解介质,测定了联苯双酯中乙醇、二氯甲烷和N,N-二甲基甲酰胺的残留量。结果乙醇、二氯甲烷和N,N-二甲基甲酰胺及溶剂峰彼此均能良好分离,线性范围分别为0.90～401.72μg·mL-1（r=0.9999）,2.51～50.20μg·mL-1（r=0.9999）,1.43～75.36μg·mL-1（r=0.9998）;方法重复性良好,回收率也符合规定。结论该法适用于联苯双酯中这3种有机溶剂残留量的测定。

Determination of Residual Organic Solvents in Bifendate by Capillary GC

OBJECTIVE To establish a method for determination of residual organic solvents in Bifendate. METHODS The determination was carried out with DB-624 capillary column（ 30. 0m × 0. 53mm × 3μm）and FID detector. The inlet temperature was 200℃ and the detector temperature was 260℃. The column temperature rose by program： the initial temperature was 60℃,maintained for 5min,raise to 220℃ with a rate of 20℃ /min,maintained for 5min,The carries gas was nitrogen and the pressure of carries gas was 2. 4psi,the direct injection was used and the injection volume was 1μL. The dissolved medium used was Dimethylsulfoxide. RESULTS Ethanol,dichloromethane and N,N-dimethylformamide could be separated from solvent peak in chromatogram obtained from system suitability test. Their calibration curves were linear in the range of 0. 90 ～ 401. 72μg·mL- 1（ r =0.9999）,2.51 ～50. 20μg·mL- 1（ r =0. 9999）,1. 43 ～75. 36μg·mL- 1（ r =0.9998）,respectively. The repeatability and recovery met requirements. CONCLUSION The method can be applied in determination of three residual organic solvents in Bifendate.