毛细管气相色谱法测定甘氨双唑钠中有机溶剂残留量  

Determination of Organic Solvent Residue in Glycididazole Sodium by Capillary GC

作　　者：罗淑青 卓开华 周征 曹琳 

机构地区：[1]宁波市食品药品检验所,浙江宁波315048

出　　处：《药学进展》2012年第11期508-510,共3页Progress in Pharmaceutical Sciences

基　　金：国家药品标准提高研究课题(No.附件3-946)

摘　　要：目的:建立测定甘氨双唑钠中N,N-二甲基甲酰胺及乙醇残留量的毛细管气相色谱法。方法:采用HP-FFAP毛细管色谱柱(30 m×0.32 mm×0.25μm),氢火焰离子化检测器,二甲基亚砜为溶剂,氮气为载气;程序升温:初始温度为40℃,保持5 min,以每分钟8℃的升温速率升至110℃,保持2 min,再以每分钟30℃的升温速率升至230℃,保持2 min。结果:样品中未检出N,N-二甲基甲酰胺,但有乙醇残留,按内标法计算得3批样品中乙醇残留量分别为0.44%、0.46%和0.46%。结论:该方法灵敏、准确、重复性好,可用于甘氨双唑钠中有机溶剂残留量的测定。Objective： To establish a capillary gas chromatography method for the determination of resi- due of N, N-dimethylformamide（DMF） and alcohol in glycididazole sodium. Methods： HP-FFAP capillary column was used, with FID as detector, DMSO as the solvent and nitrogen as the carrier gas. Temperature programming was used as follows： the initial column temperature was 40 ℃ which was maintained for 5 min, and then raised to 110 ℃ at a rate of 8 ℃ -min-1 for 2 min, and then raised to 230 ℃ at a rate of 30 ℃ .min-1 for 2 min. Results： The DMF content was under the limit of detection, and the residue of alcohol calculated by interal standard method was 0. 44%, 0. 46% and 0. 46% in 3 batches of samples, respectively. Conclusion： The method is sensitive, accurate and highly reproducible. It can be used to determine the organic solvent residue in glycididazole sodium.

关 键 词：甘氨双唑钠 有机溶剂残留量 气相色谱法 

分 类 号：TQ460.72[医药卫生—药物分析学] O657.71[化学工程—制药化工]