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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,1.8μm)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HPFFAP毛细管柱(25 m×0.32 mm,0.5μm)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 the determination of 9 residual solvents in cefotetan disodium raw drug. Methods DB-624 capillary column (30 m × 0.32 mm, 1.8 μm) was used as the chromatographic column. The aqueous solution of cefotetan as raw material was used for the determination of methanol, acetone, acetonitrile, methylene chloride, butanone, Ester and tetrahydrofuran were determined. The column of HPFFAP (25 m × 0.32 mm, 0.5 μm) was used as the column and the dimethylsulfoxide as the solvent was used for the determination of anisole, isooctanoic acid Content. Results The separation of methanol, acetone, acetonitrile, methylene chloride, butanone, ethyl acetate, tetrahydrofuran, anisole and isooctanoic acid was good. The linearity was good in the investigated concentration range, with r ranging from 0.998 8 to 0.999 7 The recovery rates of three levels were between 95.71% and 103.55%, RSD were between 0.39% and 2.28% respectively. Conclusion Both methods are accurate and sensitive and can be used for the determination of residual solvents in cefotetan disodium.