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目的:建立测定硝酸异康唑原料药中甲基叔丁基醚、甲醇、二氯甲烷、三氯甲烷、四氢呋喃5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,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,甲基叔丁基醚、四氢呋喃、甲醇、二氯甲烷和三氯甲烷分别在10.28~92.52μg·mL~(-1)(γ=0.999 4),14.49~130.43μg·mL~(-1)(γ=0.999 4),62.86~565.74μg·mL~(-1)(γ=0.999 3),13.52~121.68μg·mL~(-1)(γ=0.999 5),2.76~24.84μg·mL~(-1)(γ=0.999 1)质量浓度范围内线性关系良好。平均回收率分别为97.19%(RSD为1.21%),99.90%(RSD为0.28%),99.29%(RSD为1.21%),99.15%(RSD为0.65%),100.14%(RSD为2.58%)。结论:该检测方法灵敏、准确、可靠,可用于硝酸异康唑原料药的质量控制。
Objective: To establish a method for the determination of 5 kinds of organic solvents, methyl tert-butyl ether, methanol, dichloromethane, trichloromethane and tetrahydrofuran in isoconazole nitrate medicine. Method: capillary gas chromatography, detector: FID; detector temperature: 250 ℃; injector temperature: 200 ℃; carrier gas: nitrogen; Results: Under the above chromatographic conditions, methyl tert-butyl ether, tetrahydrofuran, methanol, methylene chloride and chloroform were in the range of 10.28-92.52μg · mL -1 (γ = 0.999 4), 14.49-130.43μg · ML ~ (-1) (γ = 0.999 4), 62.86 ~ 565.74 μg · mL -1 (γ = 0.999 3), 13.52 ~ 121.68 μg · mL -1 The linear range of 2.76 ~ 24.84μg · mL -1 (γ = 0.999 1) was good. The average recoveries were 97.19% (RSD 1.21%), 99.90% (RSD 0.28%), 99.29% (RSD 1.21%), 99.15% (RSD 0.65%) and 100.14% (RSD 2.58%). Conclusion: The method is sensitive, accurate and reliable and can be used for quality control of isoconazole nitrate drug substance.