顶空毛细管气相色谱法测定盐酸头孢卡品酯中的残留有机溶剂

摘要

Objective To eastablish a method for determination of seven residual solvents in cefcapene pivoxil hydrochloride. Methods Using DB-1 capillary column (30.0m×0.53mm, 1.5μm), FID detector and programably tempreture .The initial tempreture was kept at 40 ℃ for 10 min, and the tempreture was raised to 80 ℃ at rate of 20 ℃/ min and lasted 5 min. Results Seven residual solvents were completely separated and there were good linearies (R2=0.9988~0.9999). The average recovery rate was in the range of 96.7%~103.3%. Conclusion The methods proved to be accurate and sensitive, thereby available for quality control.%目的 建立盐酸头孢卡品酯中7种有机溶剂的分离测定方法.方法 采用顶空进样毛细管气相色谱法,FID检测器,运用DB-1毛细管柱(30.0m×0.53mm,1.5μm)为色谱柱,氮气为载气,采取程序升温,初始柱温40℃,保持10min,再以20℃/min的速率升至80℃,保持5min.测定了盐酸头孢卡品酯中丙酮、乙醇、乙酸乙酯、二氯甲烷、甲基异丁基酮、四氢呋喃和N、N-二甲基甲酰胺的残留量.结果 各有机溶剂均能得到有效的分离,在所考察的溶度范围内线性关系良好,R2为0.9988～0.9999,平均同收率为96.7％～103.3％.结论 本方法灵敏、准确、可靠,可用于盐酸头孢卡品酯的质量控制.