顶空毛细管气相色谱法测定交联羧甲基纤维素钠中的5种残留溶剂

目的:建立测定交联羧甲基纤维素钠(CS)中5种残留溶剂即二氯甲烷、三氯甲烷、苯、三氯乙烯和1,4-二氧六环量的方法。方法:采用顶空毛细管气相色谱法。色谱柱为AgilentDB-624弹性石英毛细管柱;程序升温;进样口温度为200℃,检测器温度为250℃;载气为氮气,不分流进样;顶空加热温度为85℃,平衡时间为30min。结果:5种残留溶剂在各自的检测浓度范围内线性关系良好(r为0.9980～0.9997),最低定量限为0.04～1.2μg·mL-1,最低检测浓度为0.02～0.5μg·mL-1;平均回收率为83.8%～89.4%,RSD为2.56%～4.40%。结论:该法灵敏度高,重复性和准确度好,可用于CS中5种残留溶剂的检测,并为其质量标准方法的修订提供了依据。

Determination of 5 Kinds of Residual Solvents in Croscarmellose Sodium by Headspace Capillary GC

OBJECTIVE： To establish a method for the determination of 5 kinds of residual solvents such as dichloromethane, chloroform, benzene, trichloroethylene and 1,4-dioxane in croscarmellose sodium （CS）. METHODS： Headspace capillary GC was adopted. The Agilent DB-624 fused-silica capillary column was used with temperature programming; the injection temperature was 200 ℃ and the temperature of detector was 250 ℃ ; the carder gas was nitrogen without split sampling; the containers of head- space injector were in equilibrium at 85 ℃ for 30 min. RESULTS： There was a good linear relationship of 5 residual solvents （r of 0.998 0-0.999 7）. The minimum quantitative concentration were 0.04-1.2 μg.mL-1, and the limits of detection were 0.0240.5 μg.mL-1. Average recovery rates were 83.8%-89.4% （RSD of 2.56%-4.40%）. CONCLUSION： The established method is sensi- tive, reproducible and accurate, and it can be used for the determination of 5 residual solvents in CS and provides reference for re- vising the quality standard of CS.