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顶空气相色谱法测定硝酸布康唑中有机溶剂残留量
Determination of Organic Solvents Residue in Butoconazole Nitrate by Headspace Gas Chromatography
【摘要】 目的建立测定硝酸布康唑原料药中乙酸乙酯、三氯甲烷、N,N-二甲基甲酰胺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,程序升温,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,乙酸乙酯,三氯甲烷,N,N-二甲基甲酰胺分别在0.066~0.588,0.062~0.556,0.896~8.061μg·m L-1质量浓度范围内呈良好线性关系。平均回收率分别为99.18%,102.84%,98.71%,RSD分别为3.87%,4.33%,3.71%。结论该检测方法灵敏、准确、可靠,可用于硝酸布康唑原料药的质量控制。
【Abstract】 Objective To establish a gas chromatograph method for determing Chloroform,ethyl acetate and N,Ndimethyl formamide in butoconazole nitrate. Methods The samples was detected by Headspace Gas Chromatography.Temperature programming method was adpoted and FID was used as detector. The injector temperature was 200 ℃,and the detector temperature was reach 250 ℃. Nitrogen was used as carrier gas in the experiment. Results In the mentioned chromatographic conditions,Chloroform,ethyl acetate and N,N-dimethyl formamide had good linear relationships in the ranges of 0.066-0. 588,0. 062- 0. 556 and 0. 896- 8. 061 μg · m L-1respectively. The average recoveries were 99. 18%,102. 84% and98.71%.RSD were 3.87%,4.33% and 3.71%. Conclusion The detection method is sensitive,accurate,reliable,and can be used as a quality control for butoconazole nitrate.
【Key words】 Butoconazole,nitrate; Chromatography,gas; Organic solvent residue;
- 【文献出处】 医药导报 ,Herald of Medicine , 编辑部邮箱 ,2015年08期
- 【分类号】O657.71;R927.1
- 【下载频次】58