GC测定马来酸伊索拉定原料中二氧六环和2-甲氧基乙醇残留量

目的建立GC测定马来酸伊索拉定原料中二氧六环和2-甲氧基乙醇的残留量。方法样品以二甲基甲酰胺溶解，色谱柱为HP-INNOWAX毛细管柱（30m×0．53mm，1μm），检测器为氢火焰离子化检测器，柱温为程序升温，初始柱温为40℃，进样口温度为200℃，检测器温度为250℃。结果二氧六环和2-甲氧基乙醇分别在7．6～76μg·mL^-1和1．0～10gg·mL^-1内线性关系良好p分别为0．9999和0．9984），平均回收率分别为94．7％（RSD=3．7％）和98．2％（RSD=3．9％），检测限分别为0．9μg·mL^-1和0.3μg·mL^-1。结论本方法灵敏度高、准确度好，可用于马来酸伊索拉定原料中二氧六环和2-甲氧基乙醇的残留量测定。

Determination of Residual of 1,4-Dioxane and 2-Methoxyethanol in Irsogladine Maleate Bulk Drug by GC

OBJECTIVE To establish a method for the determination of residual of 1,4-dioxane and 2-methoxyethanol in irsogladine maleate bulk drug by capillary gas chromatography（GC）. METHODS Samples were dissolved in dimethyl formamide and separated on an HP-INNOWAX capillary column （30 m×0.53 mm, 1 μm） and detected by FID. The column temperature was programmed and initial temperature was 40 ℃. The injector temperature was 200℃ and the detector temperature was 250 ℃. RESULTS The linear ranges for 1,4-dioxane and 2-methoxyethanol were 7.6-76 μg·mL^-1（r=0.999 9） and 1.0-10 μg·mL-l（r=0.998 4）, respectively. Their average recoveries were 94.7%（RSD=3.7%） and 98.2%（RSD=3.9%）. The limits of detection were 0.9 μg·mL^-1 and 0.3 μg·mL^-1, respectively. CONCLUSION The method is sensitive, accurate and can be used for the determination of residual organic solvents in irsogladine maleate bulk drug.