顶空气相色谱法测定加米霉素原料药中有机溶剂的残留量

Determination of six residual solvents in gamithromycin by headspace GC

建立顶空气相色谱法测定加米霉素中甲醇、丙酮、异丙醇、二氯甲烷、乙酸乙酯和正庚烷共6种有机溶剂的的残留量。采用顶空气相色谱法,毛细管色谱柱为Agilent DB-624UI（30.0 m×0.32 mm,1.8μm）;程序升温;FID检测器;载气为氮气;流速为3 mL·min^（-1）;顶空平衡温度为90℃;平衡时间为30 min;用外标法计算甲醇、丙酮、异丙醇、二氯甲烷、乙酸乙酯和正庚烷共6种溶剂的含量。甲醇、丙酮、异丙醇、二氯甲烷、乙酸乙酯和正庚烷在各自的质量浓度范围内均具有良好的线性关系（r=0.997 3~0.999 6）,平均回收率为88.1%~97.7%,检测限分别为0.60、0.10、0.20、0.28、0.10和0.000 1μg·mL^（-1）。试验结果表明本方法适用于加米霉素原料药中溶剂残留量的检查。

The aim of the study was to establish a method for determination of six residual solvents in gamithromycin by headspace gas chromatography. The GC analysis was performed on a capillary column Agilent DB-624 UI（30. 0 m×0. 32 mm,1. 8 μm） with programmed temperature. Nitrogen was used as the carrier with a flow rate of 3 mL·min^（-1）. An FID detector was used. The headspace equilibrium temperature was set at 90 ℃,and the equilibrium time duration was set at 30 min. The external standard method was used for determining the content of the six residual solvents. Under the established chromatography condition,good linear relationships were obtained for the six residual solvents within the experimental concentration ranges（r = 0. 997 3-0. 999 6）. The average recovery rates were in the range of 88. 1%-97. 7%. The limits of detection were 0. 60,0. 10,0. 20,0. 28,0. 10 and 0. 000 1 μg·mL^（-1）,respectively. The results indicated that the present method would suitable for detecting the residual solvents in gamithromycin.