GC和GC/MS法分析替加环素中的13种残留溶剂

Analysis of thirteen residual organic solvents in tigecycline by GC and GC/MS

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p≥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 method of GC for the determination of residual solvents in tigecycline and a method of GC/MS for the verification of residual solvents in tigecycline. Methods Mixed sample solution of methanol, ethanol, ether, acetone, isopropyl alcohol, acetonitrile, hexane, acetic ether, isopropyl ether, 1,2-dimethoxyethane; isopropyl acetate, toluene and n-heptane were separated on DB-624 capillary column through head-space sampling mode. The column temperature was maintained at 45 ℃ for 7min, then was raised to 180℃ at the rate of 10℃/min and maintained at 180℃ for 4min. The sample was dissolved in dimethylformamide. Results The measured solvents were separated completely. The calibration curve of each solvent showed a good linear relationship （r≥0.9979）. The average recoveries （n=6） of these residual solvents are within 90% to 110%. The retention time of gas chromatogram and the spectra of n-hexane in samples are the same as the the reference. The residual solvents in tigecycline were confirmed by GC/MS. Conclusion The established method is simple, reliable, which can be used for determination of residual solvents in tigecycline.