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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 capillary gas chromatographic method for the determination of residual solvents in clindamycin palmitate hydrochloride. Methods Headspace injection method was used for determination of ethanol, acetone, acetonitrile, methylene chloride, ethyl acetate and chloroform. The chromatographic column was DB-624 (6% cyanopropylphenyl-94% dimethylpolysiloxane Stationary phase), and the column temperature was 60 ° C for 10 min. The temperature was raised to 180 ° C at 20 ° C for 1 min and maintained for 2 min. The solvent was dimethylformamide-water (1: 4) And dimethylformamide were determined by direct injection, the column was DB-624 (6% cyanopropyl phenyl-94% dimethyl polysiloxane stationary phase) quartz capillary column, the column temperature was 90 ℃, Methylene chloride is a solvent. Results The analytes can be well separated, the peak area and concentration showed a good linear relationship, good precision and recovery. Conclusion This method can be used for the determination of residual solvents in clindamycin palmitate hydrochloride.