气相色谱法测定头孢匹胺中的残留溶剂

Determination of the residual solvents in cefpiramide by GC

目的建立测定头孢匹胺中的残留溶剂含量的方法。方法采用气相色谱法,用涂渍PEG-20M的填充柱,N_2为载气,柱温100℃,以正丁醇为内标物,FID检测。结果丙酮、乙腈和二甲基甲酰胺分别在进样量0.500～2.000μg、0.041～0.164μg和0.088～0.352μg范围内,与相应溶剂峰/内标峰的面积比值线性关系良好(r分别为0.9997、0.9994和0.9999),丙酮、乙腈和二甲基甲酰胺的平均回收率分别为101.0%、97.7%和100.4%,重复进样峰面积RSD分别为0.31%、1.28%和0.73%(n= 5)。结论所建立的方法专属性好,简便准确,可用于检测头孢匹胺中的残留溶剂。

Objective To establish a method for content determination of the residual solvents in cefpiramide.Methods The analysis was performed on a column coated by PEG-20M under the column temperature of 100℃,with N2 as carrier gas.Results The standard curves of acetone,acetonitrile and N,N-dimethylformamide were linear within the ranges of 0.500～2.000μg,0.041～0.164μg and 0.088～0.352μg （r=0.9997,0.9994 and 0.9999）,respectively.The average recoveries of acetone,acetonitrile and N,N- dimethylformamide were 101.1%,97.7% and 100.4%,while the RSD for replications were 0.31%,1.28% and 0.73% （n=5）, respectively.Conclusion The method is specific,simple and accurate for the quality control cefpiramide raw materials.