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目的:建立克林霉素磷酸酯原料药中残留溶剂N,N-二甲基甲酰胺(DMF)的测定方法。方法:采用气相色谱法,氮磷检测器,DB-624型毛细管柱,柱温80℃,以5℃/min升至140℃,再以40℃/min升至225℃,保持5min;进样口温度200℃,检测器温度300℃进行检测。结果:N,N-二甲基甲酰胺浓度在18~1056μg/mL范围内线性关系良好,平均回收率为100.63%(n=9);3批次克林霉素磷酸酯原料中均未检出DMF。结论:该方法操作简便、灵敏、准确,适用于克林霉素磷酸酯原料药中DMF残留量的测定。
Objective: To establish a method for the determination of residual solvent N, N-dimethylformamide (DMF) in clindamycin phosphate drug substance. Methods: Gas chromatography, nitrogen and phosphorus detector, DB-624 capillary column were used. The column temperature was increased to 140 ℃ at 5 ℃ / min and the temperature was raised to 225 ℃ at 40 ℃ / min for 5 min. The injection The mouth temperature 200 ℃, the detector temperature 300 ℃ for testing. Results: The linear range of N, N-dimethylformamide was in the range of 18 ~ 1056μg / mL, with an average recovery of 100.63% (n = 9). None of the three batches of clindamycin phosphate raw materials Out of DMF. Conclusion: The method is simple, sensitive and accurate and is suitable for the determination of DMF residues in clindamycin phosphate drug substance.