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

    • 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.

       

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