气相法测定头孢他啶原料药中甲酸残留的含量

Determination of Residual Formic Acid in Ceftazidime Pentahydrate Bulk Drug by Gas Chromatography

目的建立柱前衍生气相色谱法测定头孢他啶原料药中甲酸残留含量的方法。方法采用DB-WAX毛细色谱柱;进样口温度200℃;FID检测器温度250℃;流速0.6 m L/min;柱温40℃;载气：氮气。结果甲酸在0.033 9~0.101 7 mg/m L范围内线性良好（r=0.999 7）,平均回收率为98.8%（RSD=0.9%）,检测限和定量限分别为4.7、15.7μg/m L。结论本方法操作简单,准确度好,可用于头孢他啶原料药中甲酸残留量的测定。

OBJECTIVE To establish a pre-column derivation capillary gas chromatography method for the determination of solvent of formic acid in ceftazidime pentabydrate bulk drug. METHODS The determination was performed on a DB-WAX capillary column. The injection port and detector temperature were 200 ℃ and 250 ℃ , respectively. The flow rate was 0.6 mL/L when the column temperature was 40 ℃. The carrier gas was nitrogen. RESULTS The liner range for formic acid was 0.033 9-0.101 7 mg/mL （r= 0.999 7）. The average recoveries were 98.8% （RSD = 0.9%）. The limit of detection and limit of quantification were 4.7 μg/mL and 15.7 μg/mL, respectively. CONCLUSION The method is easy to operate and has a good accuracy. It can be used for determination of residual solvent of formic acid in ceftazidime pentahydrate bulk drug.