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顶空气相色谱法测定法罗培南钠残留溶剂

闫 妍,朱晓琼,刘永明   

  1. 东北制药集团股份有限公司,东北制药集团股份有限公司,东北制药集团股份有限公司
  • 收稿日期:2014-01-23 修回日期:2014-02-21 出版日期:2014-02-25 发布日期:2014-01-25

GC headspace determination of residual solvents in Faropenem SodiumYAN yan*, ZHU xiao-qiong, LIU yong-ming (Northeast Pharmaceutical(Shenyang) Science Technology Development Co.Ltd.,Shenyang,Liaoning ,110027,China)

  1. Northeast Pharmaceutical(Shenyang) Science,,
  • Received:2014-01-23 Revised:2014-02-21 Online:2014-02-25 Published:2014-01-25

摘要: 目的 建立顶空气相色谱法测定法罗培南钠中有机溶剂残留量。方法 色谱柱为TG-624毛细管柱,FID检测器。检测器温度为250℃,进样口温度为200℃;载气为氮气,载气流速为每分钟5.0 mL。程序升温,初始柱温50℃,保持3分钟,以每分钟10℃升温至200℃,保持2分钟。顶空进样,顶空瓶平衡温度为110℃,平衡时间为30min。结果 在此色谱条件下,乙醇、丙酮、二氯甲烷、乙酸乙酯、N,N-二甲基甲酰胺、二甲苯6种溶剂均能得到良好的分离,峰面积与检测浓度在所考察的范围内具有良好的线性(乙醇r=0.9996,丙酮r=0.9995,二氯甲烷r=0.9997,乙酸乙酯r=0.9997,N,N-二甲基甲酰胺r=0.9997,二甲苯r=0.9998);平均回收率在88.0%~107%之间,重复性试验中精密度RSD分别为1.85%、1.33%、1.11%、0.76%、3.6%、1.55%。结论 所建立的方法专属性好、简便准确、重复性好,可用于检测法罗培南钠中的6种残留溶剂。

Abstract: Objective To establish a head-space GC method for determination of residual solvents in Faropenem Sodium. Methods The gas chromatograph is equipped with a flame-ionization detector and TG-624 capillary column. The carrier gas is nitrogen with about 5ml per minute. The column temperatures is maintained at 50℃ for 3 minutes ,then raised at a rate of 10℃ per minute to 200℃,and maintained at 200℃ for 2minutes.The injection port and detector temperatures are maintained at 200℃ and 250℃, respectively. Headspace equilibration temperature is 110℃ an equilibration time is 30 minutes. Results A good linearity was obtained with in the designed range of each solvent. The average recoveries were from 88%-107%. The RSD of precision and accuracy test were1.85%、1.33%、1.11%、0.76%、3.6%、1.55%, respectively, they all meet the correlative criterion of Ch.p Conclusion The method was proved to be simple and accurate. It has a good reproducibility and can be used to determinate the six residual solvents in Faropenem Sodium.