摘要
目的:建立气相色谱法检测多潘立酮原料药物中的有机残留溶剂二氯甲烷、氯仿、甲苯、二甲基甲酰胺。方法:色谱柱为 QC2/BP1(25 m×0.22 mm,0.25 μm),载气为氢气,采用氢离子火焰检测器,进样器温度为160℃,检测器温度为260℃,柱温采用二阶程序升温(50℃,保持5 min,以2℃·min^(-1)升至120℃,再以30℃·min^(-1)升至260℃,保持10 min),以二甲基亚砜为溶剂,进样量1 μL。结果:二氯甲烷、氯仿、甲苯、二甲基甲酰胺的线性关系 r 分别为0.9999,0.9998,0.9998,0.9994。平均回收率(n=5)分别为99.3%,97.6%,101.5%,96.9%;RSD 分别为2.0%,2.8%,2.5%,3.2%。结论:方法柱效高、灵敏、准确,适用于同时检测多潘立酮原料药物中二氯甲烷、氯仿、甲苯和二甲基甲酰胺的含量。
Objective：To establish a GC method for determination of methylene chloride, chloroform, toluene and dimethyl- formylamine in domperidone by eapillary gas ehromatographie. Method：A eolumn QC2/BP1,25 m × 0. 22 mm was adopted. The injeetor temperature was 160 ℃ ,the detector temperature was 260 ℃ ,the eolumn temperature is gradiently raised with initial temperature at 50℃, sustained for 5 min ,then raised to 120 ℃ at the rate of 2℃· min^-1, then raised to 260 ℃ at the rate of 30℃· min^-1, sustained for 10 rain. The solvent was dimethyl sulfoxide. Results：The eorrelation factors r in methylene chloride, chloroform, toluene and dimethyl -formylamine was 0. 9999,0. 9998,0. 9998 and 0. 9994 respectively. The recovery（ n =5 ） was 99.3% ,97.6%, 101.5% and 96. 9% with RSD 2. 0% ,2. 8% ,2. 5% and 3.2% ,respeetively. Conclusion：The method appeared to be sensitive and aeeurate, and can be used for the determination of the residual organic solvent in domperidone.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2006年第4期541-542,共2页
Chinese Journal of Pharmaceutical Analysis
关键词
气相色谱法
多潘立酮
残留溶剂
gas chromatographic
domperidone
residual solvents
