论文部分内容阅读
目的建立GC法测定替加环素中的13种残留溶剂,用GC/MS法对样品中检出的残留溶剂进行确证。方法采用顶空进样,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45℃维持7min,以每min10℃速率升至180℃,维持4min,二甲基甲酰胺为溶剂分离混合样品溶液。结果被测物均能得到很好的分离,在各自线性范围内峰面积与浓度均呈良好的线性关系(r≥0.9979),平均加样回收率(n=6)均在90%~110%之内,样品中的正庚烷的气相色谱图保留时间及质谱图与正庚烷对照品一致,证实了样品中检出的残留溶剂。结论该法可用于替加环素原料药中残留溶剂的检测。
Objective To establish a GC method for the determination of tigecycline 13 kinds of residual solvents, GC / MS method for the confirmation of the residual solvent samples. Methods The headspace sampling was performed on a DB-624 (6% cyanopropyl phenyl-94% dimethyl polysiloxane) quartz capillary column. The column temperature was maintained at 45 ℃ for 7min, The temperature was raised to 180 ° C for 4 min and dimethylformamide was used as the solvent to separate the mixed sample solution. Results The analytes could be well separated. The peak area and concentration in each linear range showed a good linear relationship (r≥0.9979), and the average recoveries (n = 6) ranged from 90% to 110% , The gas chromatogram retention time and mass spectrum of n-heptane in the sample are in agreement with the n-heptane reference sample, confirming the residual solvent detected in the sample. Conclusion This method can be used for the determination of residual solvents in tigecycline.