顶空气相色谱法测定盐酸克林霉素中的残留溶剂

目的：建立顶空毛细管气相色谱法测定盐酸克林霉素中有机溶剂残留量。方法：采用顶空气相色谱法,色谱柱为DB-624毛细管柱,载气为氮气,流速为2 ml·min^-1,分流比为1∶1。 FID检测器,检测器温度为300℃；进样口温度为200℃；柱温采取程序升温,起始温度40℃,保持5 min,以20℃·min^-1升温至200℃,持续10 min。顶空进样,平衡温度为80℃,平衡时间为30 min。以水为溶剂,外标法测定盐酸克林霉素中甲醇,乙醇,丙酮,三氯甲烷和N,N-二甲基甲酰胺的残留量。结果：在此色谱条件下,各有机溶剂均能得到有效分离,在所考察的浓度范围内线性关系良好,r=0.9991~0.9999；平均回收率为97.2%~101.2%,RSD为0.68%~1.98%（n=9）。结论：本试验建立的顶空气相色谱方法适合盐酸克林霉素原料中有机溶剂残留量的检测。

Determination of Residual solvents in Clindamycin Hydrochloride by Headspace Gas Chromatography

Objective：To establish a headspace capillary gas chromatography method for the determination of residual solvents in clindamycin hydrochloride. Methods：A headspace gas chromatography was used to separate the residual solvents on a DB-624 capillary column with an FID detector. The carried gas was nitrogen at a flow rate of 2ml·min^-1 . The split ratio was 1∶1. The temperature of the injector was 200℃ and that of the FID was 300℃. The programmed column temperature was set as follows：maintained at 40℃ for 5 min and then raised to 200℃ at the rate of 20℃·min^-1 and maintained for 10 min. The containers of headspace injector were in e-quilibrium at 80℃ for 30 min. Water was used as the solvent. The amounts of the residual solvents such as methanol,ethanol,acetone, chloroform and N,N-dimethyformamide were calculated by an external standard method. Results：The detected solvents were separated completely. The calibration curve of each solvent showed a good linear relationship （r=0. 999 1 ~0. 999 9）. The average recovery was within the range of 97. 2% ~101. 2% and RSD was within the range of 0. 68% ~1. 98%（n=9）. Conclusion：The method is suit-able for the determination of residual solvents in clindamycin hydrochloride.