顶空毛细管气相色谱法测定注射用氨苄西林钠中的有机溶剂残留量

 目的 建立顶空毛细管气相色谱法测定注射用氨苄西林钠中的有机溶剂残留量。方法 用DM-624毛细管气相色谱柱,顶空进样法,FID检测器,以甲醇为内标进行测定。结果 二氯甲烷、丙酮、异丙醇的线性范围分别为2.633～1 316.8μg·mL^-1(r=0.999 8),1.569～784.4μg·mL^-1(r=0.999 9),1.562～781.2μg·mL^-1(r=0.999 9);二氯甲烷、丙酮、异丙醇的平均回收率分别为100.8％,98.3％,99.3％;RSD分别为2.0％,2.3％,1.6％(n=5)。结论 本方法简单、准确、灵敏度高、重现性好,适用于注射用氨苄西林钠中有机溶剂残留量的测定。

Determination of residual organic solvents in ampicillin sodium for injection by capillary gas chromatography with headspace sampling

OBJECTIVE To develop headspace gas chromatography method for the determination of residual organic solvents in ampicillin sodium for injection. METHODS The samples were injected into DM-624 capillary column by headspace sampler and analysed with FID detector using methanol as the internal standard. RESULTS The linear ranges of dichloromethane, acetone and iso-propanol were 2.633～1 316.8μg·mL^-1(r=0.999 8), 1.569～784.4μg·mL^-1 (r=0.999 9) and 1.562～781.2μg·mL^-1(r=0.999 9) respectively.The recoveries were 100.8%,98.3% and 99.3% with RSD 2.0%,2.3%and 1.6%(n=5) respectively. CONCLUSIONS The method is simple, accurate and sensitive with good reproducibility. It can be used for the determination of the residual organic solvents in ampicillin sodium for injection.