| 李继 李霞 王发 赵婷 王嫦鹤△.顶空气相色谱法测定熊去氧胆酸中3 种有机溶剂残留量[J].,2015,15(31):6156-6159 |
| 顶空气相色谱法测定熊去氧胆酸中3 种有机溶剂残留量 |
| Determination of Three Residual Solvents in Ursodeoxycholic Acid byHeadspace Gas Chromatography |
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| DOI： |
| 中文关键词: 熊去氧胆酸 顶空气相色谱 溶剂残留 |
| 英文关键词: Ursodeoxycholic acid Headspace gas chromatography Residual organic solvent |
| 基金项目:陕西省自然科学基金青年基金项目（2011JQ4017） |
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| 中文摘要: |
| 目的：建立顶空气相色谱法同时测定熊去氧胆酸原料药中3 种有机溶剂残留量的方法。方法：用0.25 mol·L-1的氢氧化钠溶
液溶解样品，采用顶空进样- 气相色谱法，应用FID 检测器，在DB-WAX毛细管色谱柱（30.0 m × 320 um × 1.0 um）上程序升温
（起始温度70 ℃，保持5 分钟，再以15 ℃·min-1的升温速率升至180 ℃，保持5 分钟），载气为氮气，进样口温度200 ℃，检测器温
度230 ℃。结果：待测组分均能得到有效分离，各组分在所考察的浓度范围内线性关系良好，r = 0.9976～0.9996，平均回收率为
91.00%～99.09%。结论：本方法可准确测定熊去氧胆酸原料药中丙酮、乙醇及N, N-二甲基甲酰胺的残留量，操作简便、准确度和
灵敏度高，可达到有效控制其质量的目的。 |
| 英文摘要: |
| Objective:To establish a headspace gas chromatography method for the determination of three residual solvents in ursodeoxycholic
acid.Methods:Samples were resolved by 0.25 mol·L-1 NaOH, and then the concentration of residual solvents were measured
by headspace gas chromatography using FID detector and DB-Wax capillary column (30.0 m× 320 um× 0.5 um) with temperature
program (the initial temperature was kept at 70 ℃ for 5 min, then the temperature was raised to 180 ℃ at the rate of 15 ℃·min-1 and
kept for 5 min). The inlet temperature was controlled at 200 ℃, and the detector temperature was 230 ℃, with nitrogen as the carrier gas.Results:The linear range (r=0.9976～0.9996) were satisfactory and three residual solvents were completely separated. The average recovery
rates were 91.00%～99.09%.Conclusion:This method is simple, accurate and sensitive for detection of three residual solvents
(acetone, ethyl alcohol and N, N-dimethylformamide) in ursodeoxycholic acid, and can be used for quality control. |
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