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

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

关键词:  马来酸伊索拉定  溶剂残留  二氧六环  2-甲氧基乙醇  气相色谱法

Key words:  irsogladine maleate  solvent residue  1,4-dioxane  2-methoxyethanol  GC

摘要:

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(30 m×0.53 mm，1 μm)，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7.6~76 μg·mL^-1和1.0~10 μg·mL^-1内线性关系良好(r分别为0.999 9和0.998 4)，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0.9 μg·mL^-1和0.3 μg·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。

Abstract:

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^-1(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.