顶空法测定头孢匹胺钠中的溶剂残留  

Determination of Residual Solvent in Cefpiramide Sodium by Headspace GC

作　　者：王喜梅[1] 李晓燕[1] 周海云[1] 黄仲立[1] 

机构地区：[1]中山大学测试中心,广东广州510275

出　　处：《中山大学学报（自然科学版）》2004年第4期122-123,127,共3页Acta Scientiarum Naturalium Universitatis Sunyatseni

摘　　要：采用顶空气相色谱法对头孢匹胺钠中的残留溶剂DMF进行测定。使用熔融石英毛细管柱HP＿INNOWax(30m×0 25mm×0 25μm);检测器FID;载气N2;程序升温:初始温度为60℃,以20℃ min的速度升温至100℃,停留2min,以10℃ min的速度升温至120℃,再以40℃ min的速度升温至200℃,结束。进样口温度:220℃;检测器温度:250℃;进样体积:1mL,分流比为20∶1;溶剂残留用外标法测定,分析结果表明,该方法对DMF的检测限量为0 004g L,回收率为102%,相对标准偏差为5 4%。该方法操作简单、快速、灵敏、重现性好。A method for the determination of residual solvent DMF in cefpiramide sodium by headspace gas chromatography was established. The analysis was performed on a HP-INNOWax capillary column (30 m×0.25 mm×0.25 μm) and a flame-ionization detector. Nitrogen was used as carrier gas. Oven temperature was programmed as following: initially at 60 ℃, raised up to 100 ℃ at 20 ℃/min and held for 2 min, and then to 120 ℃ at 10 ℃/min and raised up again to 200 ℃ at 40 ℃/min. The total run time was approximately 8 min. The temperatures set for injector and FID detector were 220 ℃ and 250 ℃ respectively. Injection volume was 1 mL in split mode (1∶20 ratio). The assay of residual solvent was calculated according to the external standard method. DMF was not found in the sample of cefpiramide sodium. There was a good linear relationship for DMF (r=0.997 2) within the range from 0.005 to 0.1 g/L. The detection limit of DMF was 0.004 g/L. The average recovery was 102%. The relative standard deviation of the residue was 5.4%.

关 键 词：气相色谱 顶空 溶剂残留 头孢匹胺钠 

分 类 号：O657.71[理学—分析化学]