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建立了毛细管气相色谱法测定替加环素原料药中7种有机残留溶剂的分析方法.采用ZB-624熔融石英毛细管柱(30 m×0.53 mm×3μm),FID检测器,以二甲基亚砜为溶剂.其中甲醇、异丙醇、异丙醚、二氯甲烷、四氢呋喃与甲苯的测定采用顶空进样法,柱温40℃保持9 min,以20℃/min升温至200℃,保持1 min;N,N-二甲基甲酰胺的测定采用直接进样法,柱温100℃保持5 min,以20℃/min升温至200℃.结果表明各残留溶剂均能得到有效分离,在所考察的浓度范围内呈良好的线性关系(r=0.998 9～0.999 9),平均加样回收率在92.4%～104.8%(RSD=1.41%～5.6%)之间,定量限为0.15～10.19μg/mL,3批样品中7种残留溶剂的量均符合我国药典要求.该方法可用于替加环素原料药中残留溶剂的检测和质量控制.
A method was developed for the determination of seven organic residual solvents in tigecycline by capillary gas chromatography.The ZB-624 fused silica capillary column (30 m × 0.53 mm × 3 μm) and FID detector Sulfone was used as solvent, and the headspace injection method was used for the determination of methanol, isopropanol, isopropyl ether, methylene chloride, tetrahydrofuran and toluene. The column temperature was kept at 40 ℃ for 9 min and the temperature was raised to 200 ℃ at 20 ℃ / min. 1 min.The determination of N, N-dimethylformamide was carried out by direct injection, the column temperature was maintained at 100 ℃ for 5 min and the temperature was increased to 200 ℃ at 20 ℃ / min.The results showed that all the residual solvents could be effectively separated, (R = 0.998 9 ~ 0.999 9). The average recoveries ranged from 92.4% to 104.8% (RSD = 1.41% -5.6%), and the limits of quantification ranged from 0.15 to 10.19 μg / mL, and the amount of 7 residual solvents in 3 batches of samples accorded with the requirements of Chinese Pharmacopoeia.This method can be used for the detection and quality control of residual solvents in tigecycline bulk drug.