顶空毛细管气相色谱法测定硝酸异康唑中5种有机溶剂残留

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=0.9994),14.49~130.43μg·mL^-1 (γ=0.9994),62.86~565.74μg·mL^-1 (γ=0.9993),13.52~121.68μg·mL^-1 (γ=0.9995),2.76~24.84μg·mL^-1 (γ=0.9991)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。

Determination of residues of five organic solvents in isoconazole nitrate by headspace gas chromatography

OBJECTIVE To establish a gas chromatograph method for determination of methyl tert-butyl ether,methanol,dichloromethane,chloroform,tetra hydrofuran in isoconazole nitrate.METHODS The samples were detected by headspace gas chromatography.The detector was FID,detector temperature was 250℃ and injector temperature was 200℃,with nitrogen as carrier gas.RESULTS In the chromatographic conditions,concentrations of methyl tert-butyl ether,tetrahydrofuran,methanol,methylene chloride and chloroform,were 10.28-92.52μg·mL^-1 (γ=0.9994),14.49-130.43μg·mL^-1(γ=0.9994),62.86-565.74μg·mL^-1 (γ=0.9993),13.52-121.68μg·mL^-1(γ=0.9995) and 2.76-24.84μg·mL^-1 (γ=0.9991),respectively,with a good linear relationship.The average recoveries were 97.19% (RSD of 1.21%),99.90% (RSD of 0.28%),99.29% (RSD of 1.21%),99.15% (RSD of 0.65%) and 100.14% (RSD 2.58%),respectively.CONCLUSION The detection method is sensitive,accurate,reliable,and can be used for quality control of isoconazole nitrate.