顶空气相色谱法测定头孢地嗪钠中残留溶剂

Determination of residual solvent in cefodizime sodium by headspace gas chromatography

目的 建立头孢地嗪钠中有机残留溶剂的测定方法。方法 顶空气相色谱法。色谱条件:采用Halomapics 624 0.3 mmI.D×30 m×3.0μm氰丙苯基甲基聚硅氧烷毛细管色谱柱;柱温40℃;气化室温度:200℃;检测室温度:250℃;N2为载 气;柱前压力为1.25 Kpa;H2流速:50 ml／min;空气流速:500 ml／min。结果 丙酮在124.4-995.4μg/ml,乙腈在10.2-82.1 μg／ml,二氯甲烷在15.2-121.8μg／ml浓度范围均呈良好的线性关系。平均回收率(n=9)分别为96.9％,RSD=4.8％; 96.4％,RSD=4.1％;97.2％,RSD=4.9％。结论 本方法操作简便、结果准确、是控制头孢地嗪钠中残留溶剂的可靠方法。

Objective To establish a method for determination of residue solvent in Cefodizime sodium. Methods Headspace Gas Chromatography. The test uses Halomapics 624 capillary column (30 m×0.3 mm×0.3μm) Carrier gas:nitrogen; The column inlet pressure: 1.2 5kPa; Temperature of column:40℃; FID detector at 250℃;Injector at 200℃. Result The calibration curves for acetone, acetonitril and dichloromethane were linear in the range of 124.4-995.4μg/ml(r-0.9999 n=5) ,10.2-82.1μg/ml(r= 0.9967 n=5) and 15.2-121.8 μg/ml (r=0.9979 n=5) respectively. The average recovery rates of acetone, acetonitril and dichloromethane were 96.9% (RSD=4.8% n=9),96.4% (RSD =4.1% n=9) and 97.2% (RSD =4.9% n=9) respectively. Conclusion This method is easy to operate with precise results,which establishes a reliable method for control residue solvent of Cefodizime sodium.