气固顶空色谱法测定植入用缓释氟尿嘧啶中环己烷

Head-space gas chromatographic determination of residual solvent in fluorouracil sustained-release subcutaneous implant

目的:测定植入用缓释氟尿嘧啶中环已烧残留量。方法:研碎供试品,置针管中于60℃保温作气固顶空平衡,顶空气以气相色谱法测定,氢焰检测器,SE-30固定相,柱温80℃。结果:方法的精密度RSD为2.8％,回收率为101.4％,10～110ng·mL^(-1)范围内线性良好,检出限为3.4ng·mL^(-1)。结论:为类似难溶性固体药物的有机溶剂残留量检测提供了可靠的方法。

Objective: To determine cyclohexane, a residual solvent, in fuorouracil sustained-release subcutaneous implant. Methods: Pulverized sample was put into a syringe and maintained at 60^ for balance. The cyclohexane was determined with GC using SE-30 as stationary phase, a column temperature of 80℃, and a hydrogen flame detector. Results: The liner range of cyclohexane was 10-110ng·mL-1( r = 0. 999 8,n =6) with a detection limit of 3. 4ng·mL-1. The average recovery was 101.4% with a RSD of 2. 8 % . Conclusion: A reliable method was provided by the authors for determination of residual solvent in sparingly soluble drugs similar to fluorouracil.