毛细管柱气相色谱法测定环孢素中残留溶剂

摘要

建立环孢素中乙醇、丙酮、乙酸乙酯的测定方法。使用配置顶空进样的气相色谱仪，用 HP -1毛细管色谱柱（100％二甲基聚硅氧烷），0.53 mm ×30 m；柱温40℃，保持5 min，以10℃·min -1的速度升温至150℃，保持2 min；以氮气为载气，流速30 cm/ min；氢火焰离子化检测器。乙醇、丙酮、乙酸乙酯线性关系良好，相关系数均大于0.99；平均回收率分别为97.75％、97.91％、98.31％；检测限分别为8.1691×10-4、3.8152×10-4、1.0082×10-7 mg/ mL。该方法的简单方便，灵敏度高，重复性好，结果准确，适用于环孢素中多种有机溶剂残留量的测定与控制。%To establish a GC method for the determination of ethanol,acetone,ethyl acetate in cyclosporine . The GC was quipped with a headspace injector and a flame - ionization detector. A. 0. 53mm 30m,HP - 1 capillary chromatographic column(coated with 100% dimethyl polysiloxane stationary phase)was adopted and the carrier gas was nitrogen. The initial column temperature was kept at 40℃ for 5min,then raised to 150℃ at the rate of 10℃ / min - 1 ,and kept at 150℃ for 2min. The correlation coefficient in ethanol ,acetone ,ethyl acetate were all higher than 0. 99,The recovery were 97. 75% 、97. 91% 、98. 31% ;and limit of detection respectively were8. 1691 × 10 - 4、3. 8152 × 10 - 4 、1. 0082 × 10 - 7 mg/mL. This method is reliable in terms of precision,accuracy,specificity,detectability,linearity and durability. It is applicable to the detection of residual organic solvents in cyclosporine.