目的 建立测定头孢替坦二钠原料药中9种残留溶剂的方法。方法 使用DB-624毛细管柱(30 m×0.32 mm, 1.8 μm)为色谱柱, 以水为溶剂, 测定头孢替坦二钠原料药中甲醇、丙酮、乙腈、二氯甲烷、丁酮、乙酸乙酯、四氢呋喃的含量;使用HP-FFAP毛细管柱(25 m×0.32 mm, 0.5 μm)为色谱柱, 以20%的二甲亚砜为溶剂, 测定头孢替坦二钠原料药中苯甲醚、异辛酸的含量。结果 甲醇、丙酮、乙腈、二氯甲烷、丁酮、乙酸乙酯、四氢呋喃、苯甲醚、异辛酸分离度良好;在所考察的浓度范围内线性关系良好, r分别在0.998 8～0.999 7之间;3个水平的回收率分别在95.71%～103.55%之间, RSD分别在0.39%～2.28%之间。结论 两种方法均准确、灵敏, 可用于头孢替坦二钠原料药中残留溶剂的测定。

OBJECTIVE To establish a METHOD for determining nine residual solvents in cefotetan disodium by headspace gas chromatography.METHODS The residual solvents including methanol, acetone, acetonitrile, dichloromethane, butanone, ethyl acetate, tetrahydrofuran in cefotetan disodium were quantitatively determined on a DB-624 column(30 m×0.32 mm, 1.8 μm). Water was solvent media. The residual solvents of anisole and isocaprylic acid in cefotetan disodium were quantitatively determined on a HP-FFAP column(25 m×0.32 mm, 0.5 μm). The 20%dimethylsulfoxide(DMSO) was used as the solvent. RESULTS Nine residual solvents were completely separated. Good linearity of the solvents were obtained within the determination ranges. There between 0.998 8 and 0.999 7. The average recoveries of three levels were in the range of 95.71%-103.55%. The RSDs were 0.39%-2.28%. CONCLUSION The established two methods are accurate and sensitive, and can be used for the determination of residual solvents in cefotetan disodium.