GC测定盐酸克林霉素棕榈酸酯中的9种残留溶剂

Determination of Nine Residual Organic Solvent in Clindamycin Palmitate Hydrochloride by GC

目的建立毛细管气相色谱法测定盐酸克林霉素棕榈酸酯中的残留溶剂。方法乙醇、丙酮、乙腈、二氯甲烷、乙酸乙酯和三氯甲烷测定采用顶空进样法,色谱柱为DB-624(6%氰丙基苯基-94%二甲基聚硅氧烷固定液)石英毛细管柱,柱温为60℃,维持10 min,以20℃.min 1升至180℃,维持2 min,二甲基甲酰胺-水(1∶4)为溶剂;甲苯、吡啶和二甲基甲酰胺测定采用直接进样法,色谱柱为DB-624(6%氰丙基苯基-94%二甲基聚硅氧烷固定液)石英毛细管柱,柱温为90℃,二氯甲烷为溶剂。结果被测物均能得到很好的分离,峰面积与浓度呈良好的线性关系,精密度和回收率良好。结论该法可用于盐酸克林霉素棕榈酸酯原料药中残留溶剂的检测。

OBJECTIVE To establish a method of capillary gas chromatography for the determination of residual solvents in clindamycin palmitate hydrochloride.METHODS Ethanol,acetone,acetonitrile,dichloromethane,acetic ether and trichlormethane were separated on DB-624 capillary column through head-space sampling mode.The column temperature was maintained at 60 ℃ for 10 min,then was raised to 180 ℃ at the rate of 20 ℃.min 1 and maintained at 180 ℃ for 2 min.The sample was dissolved in dimethylformamide-water（1 ∶ 4）.Pyridine,toluene and dimethylformamide were separated on DB-624 capillary column through direct sampling mode.The column temperature was 90 ℃.The sample was dissolved in dichloromethane.RESULTS The measured solvents were separated completely.The calibration curve of each solvent showed a good linear relationship with precision and accuracy.CONCLUSION The established method is simple,reliable,which can be used for determination of residual solvents in clindamycin palmitate hydrochloride.