毛细管气相色谱法测定硫酸异帕米星中的残留溶剂

目的 建立顶空进样和直接进样毛细管气相色谱法测定硫酸异帕米星中的残留溶剂.方法 样品溶于水-二甲基甲酰胺（7：3）溶液;色谱柱为DB-624（6%氰丙基苯基-94%二甲基聚硅氧烷固定液）毛细管柱;甲醇、丙酮测定采用顶空进样法,柱温50℃维持6min,以每分钟30℃升至180℃,维持5min;二甲基亚砜测定采用直接进样法,柱温为110℃.结果 3种残留溶剂均得到了很好的分离,峰面积与浓度的线性关系、精密度和回收率均良好.结论 该方法准确、可靠,可用于药品检验中硫酸异帕米星中残留溶剂的测定.

Determination of residual solvents in Isepamicin sulfate by capillary gas chromatography method

OBJECTIVE To establish a method of head-space/direct injection capillary gas chromatography for the determination of residual solvents in isepamicin sulfate. METHODS The samples were dissolved in the mixed solvent of water/dimethyl formamide （ 7 ： 3, v ： v）. The methanol and dichloromethane in isepamicin sulfate were sepa- rated on DB-624 capillary column by head-space injection. The column temperature was maintained at 50℃ for 6 min, then was raised to 180℃ at the rate of 30℃/min and maintained for 5 min, The dimethyl sulfoxide were separa- ted on DB-624 column by direct injection. The column temperature was 110℃. RESULTS Three measured solvents were separated completely. The calibration curve of each solvent showed a good linear relationship with good precision and accuracy. CONCLUSION The established method was accurate and reliable. It can be used for the determina- tion of residual solvents in isepamicin sulfate.