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

关键词:  盐酸克林霉素棕榈酸酯  气相毛细管色谱法  残留溶剂  顶空进样  直接进样

Key words:  clindamycin palmitate hydrochloride  GC  residual organic solvents  head-space sampling  direct sampling

摘要:

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。

Abstract:

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.