| 引用本文: | 闻宏亮,彭茗,宋冬梅,杨永健.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[J].中国现代应用药学,2014,31(5):570-573. |
| WEN Hongliang,PENG Ming,SONG Dongmei,YANG Yongjian.Determination of Residual of 1,4-Dioxane and 2-Methoxyethanol in Irsogladine Maleate Bulk Drug by GC[J].Chin J Mod Appl Pharm(中国现代应用药学),2014,31(5):570-573. |
|
| 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。 |
| 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 |
| DOI： |
| 分类号: |
| 基金项目: |
|
| Determination of Residual of 1,4-Dioxane and 2-Methoxyethanol in Irsogladine Maleate Bulk Drug by GC |
|
WEN Hongliang, PENG Ming, SONG Dongmei, YANG Yongjian
|
|
Shanghai Institute for Food and Drug Control, Shanghai 201203, China
|
| 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. |
| Key words: irsogladine maleate solvent residue 1,4-dioxane 2-methoxyethanol GC |
