【摘要】 目的:建立测定硝酸芬替原料药中二氯甲烷、甲醇和乙醇3种有机溶剂残留量的分析方法。方法:采用毛细管气相色谱法,色谱柱:OV-1301毛细管色谱柱(30 m×0.53 mm,3.0μm),检测器:FID;检测器温度:250℃;进样器温度:200℃;载气:氮气;顶空进样。结果:在上述色谱条件下,二氯甲烷、甲醇和乙醇分别在2.436~21.924μg·ml-1(r=0.998 8),12.268~110.412μg·ml-1(r=0.999 5),20.052~180.468μg·ml-1(r=0.996 9)质量浓度范围内线性关系良好。平均回收率分别为99.30%(RSD=2.36%,n=9),100.21%(RSD=1.07%,n=9),100.15%(RSD=1.27%,n=9)。结论:该检测方法灵敏、准确、可靠,可用于硝酸芬替康唑原料药的质量控制。更多还原

【Abstract】 Objective: To establish a method for the determination of dichloromethane,methanol and ethanol in fenticonazole nitrate. Methods: The samples were detected by headspace GC. The column was OV-1301( 30 m × 0. 53 mm,3. 0 μm),the detector was FID with nitrogen as the carrier gas,the detector temperature was 250 ℃ and the injector temperature was 200 ℃. Results: The linear range of dichloromethane,methanol and ethanol was 2. 436-21. 924( r = 0. 998 8),12. 268-110. 412( r = 0. 999 5) and 20. 052-180. 468 μg·ml- 1( r = 0. 996 9) with the average recovery of 99. 30%( RSD = 2. 36%),100. 21%( RSD = 1. 07%) and 100. 15%( RSD = 1. 21%)( n = 9),respectively. Conclusion: The detection method is sensitive,accurate and reliable,and can be used in the quality control of fenticonazole nitrate.更多还原