顶空毛细管气相色谱法测定克林霉素磷酸酯中甲酸残留量

摘要

目的 建立测定克林霉素磷酸酯中甲酸残留的顶空毛细管气相色谱法.方法 使用Agilent DB-FFAP毛细管柱(30 m×0.32 mm,0.5μm)及氢火焰离子检测器(FID),进样口温度200℃,检测器温度250℃;程序升温,初始温度为40℃,保持6 min,然后以30℃/min的速率升温至180℃,保持3 min;顶空进样,平衡温度为65℃,平衡时间为30 min.结果 甲酸质量浓度在0.003743~0.9980 g/L范围内与峰面积线性关系良好,r=0.9992(n=8),平均回收率为99.30%,RSD为0.64%(n=12).结论 该方法简便,灵敏度高,重复性好,结果准确,适用于克林霉素磷酸酯中甲酸残留量的测定.%Objective To establish an headspace capillary GC method for the content determination of formic acid in clindamycin phos-phate. Methods Agilent DB-FFAP capillary column(30 m × 0. 32 mm,0. 5 μm)and FID were adopted. The inlet temperature was 200 ℃and the FID detector temperature was 250 ℃. The oven temperature was initially held at 40 ℃ for 7 min and was then programmed to 150 ℃ at 30 ℃ /min and held for 3 min. The head-space sampling was used at heated temperature 65 ℃ for 30 min. Results The concentration of formic acid was linear in the range of 0. 003743-0. 9980 g/L,r=0. 9992( n=8). The average recovery rate was 99. 30%,RSD=0. 64%( n=12). Conclusion The method is simple,sensitive,reproducible and accurate. It is suitable for the content determination of formic acid residue in clindamycin phosphate.