摘要
目的:采用毛细管气相色谱法测定扎托洛芬原料药中四氯化碳、三氯甲烷、甲醇及乙醇4种有机溶剂的残留量。方法:使用HP-5毛细管色谱柱(0.32mm×30m×0.25μm),柱温分别为60和80℃,氢火焰检测器和电子捕获检测器,以N,N-二甲基甲酰胺为溶剂,载气为氮气,进样口温度200℃,检测器温度250℃,分流比为50:1,进样量1μL。结果:4种有机溶剂分离完全,且线性关系良好,线性范围分别为四氯化碳0.0399～0.3990mg/L、三氯甲烷0.5619～5.6190mg/L、甲醇29.67～296.70mg/L及乙醇49.33～493.30mg/L。在所考察的浓度范围内线性关系良好,r为0.9990～0.9995,平均回收率为97.9%～103.9%,精密度重复性RSD<5%。结论:该方法简便、快速、准确,可作为扎托洛芬有机溶剂残留量的检测方法。
Aim：To determine the contents of the residual solvents,carbon tetrachloride,chloroform,methanol,and ethanol in zaltoprofen raw material by capillary gas chromatography.Methods：Gas chromatography was used to analyze the residual solvents quantitatively.After being dissolved in DMF,samples were analyzed on HP-5 column with oven temperature at 60 and 80 ℃,respectively,with input temperature at 200 ℃,FID detector and ECD detector,nitrogen as the carrier gas,detector temperature 250 ℃,split ratio 50：1,injection volume 1 μL.Results：The liner ranges of carbon tetrachloride,chloroform,methanol,and ethanol were 0.039 9～0.399 0 mg/L,0.561 9～5.619 0 mg/L,29.67～296.70 mg/L,and 49.33～493.30 mg/L,respectively,r was 0.999 0~0.999 5.The linear range and recoveries were satisfied.RSD of precision and accuracy was less than 5% with average recoveries between 97.9% and 103.9%.Conclusion：The method could be used for the quality control of zaltoprofen raw material.
出处
《郑州大学学报（医学版）》
CAS
北大核心
2010年第1期134-137,共4页
Journal of Zhengzhou University(Medical Sciences)
关键词
毛细管气相色谱法
非甾体抗炎药
扎托洛芬
有机溶剂残留量
capillary gas chromatography
nonsteroidal anti-inflammatory drug
zaltoprofen
residual organic solvent
