毛细管气相色谱法检测替加环素中有机溶剂残留  

Determination of Residual Solvents in Tigecycline by Capillary Gas Chromatography

作　　者：杜丽媛[1] 乔俊花[2] 周冲[1] 葛秋景[1] 孙秀燕[1] 

机构地区：[1]烟台大学药学院,山东烟台264005 [2]烟台大学校医院,山东烟台264005

出　　处：《烟台大学学报（自然科学与工程版）》2012年第1期39-43,共5页Journal of Yantai University(Natural Science and Engineering Edition)

基　　金：山东省自然科学基金资助项目(Y2008C67)

摘　　要：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 of capillary gas chromatography for the determination of residual organic solvents in tigecycline is developed. ZB-624 capillary column （30 m × 0. 53 mm ×3μm） and FID detector are used with DMSO as dissol- vent. Six residual solvents （methanol, isopropanol, isopropyl ether, dichloromethane, tetrahydrofuran and toluene） are determined by headspaee sampling method. The initial column temperature is kept at 40℃ for 9 min, then raised to 200℃ at a rate of 20 ℃·min^-1 and maintained at 200℃ for 1 rain. The N, N-dimethylformamide is determined by direct injection method at a column temperature of 100℃ for 5 min and followed by an increase at a rate of 20℃·min^-1 to 200℃. Results show that the residual solvents can be effectively separated, and the standard curve of each solvent is essentially linear （ r = 0. 998 9 - 0. 999 9） within a certain range. The mean sample recovery rate is 92. 4% - 104. 8 % （RSD = 1.41% -5.6 % ） and the quantitation limit is 0. 15 - 10. 19μg/ mL. The residual levels for the seven solvents in 3 batches of the samples meet the relevant standards in Pharmacopeia of PRC. This method can be used for the determination and quality control of the residual solvents in raw drug substance of tigecycline.

关 键 词：替加环素 残留溶剂 毛细管气相色谱法 

分 类 号：R917[医药卫生—药物分析学]