| 陈名清.顶空气相色谱法测定15-羟基硬脂酸聚乙二醇酯中环氧乙烷和二氧六环含量[J].中国药品标准,2023,24(2): |
| 顶空气相色谱法测定15-羟基硬脂酸聚乙二醇酯中环氧乙烷和二氧六环含量 |
| Determination of free ethylene oxide and dioxane in Polyoxyl 15 Hydroxystearate by headspace gas chromatography |
| 投稿时间：2022-07-11 修订日期：2023-03-30 |
| DOI： |
| 中文关键词: 15-羟基硬脂酸聚乙二醇酯 顶空气相色谱法 环氧乙烷 二氧六环 |
| 英文关键词: polyoxyl 15 hydroxystearate pharmaceutical excipients headspace gas chromatography ethylene oxide dioxane |
| 基金项目:无 |
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| 摘要点击次数: 245 |
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| 中文摘要: |
| 目的：采用顶空气相色谱法，建立药用辅料15-羟基硬脂酸聚乙二醇酯中的残留杂质环氧乙烷和二氧六环的含量测定方法。方法：选用色谱柱DB-5（15 m×0.32 mm, 1 μm），以5%苯基-95%甲基聚硅氧烷为固定液，采用程序升温模式：起始温度为35℃，维持5分钟，以每分钟5℃的速率升温至180℃，然后以每分钟30℃的速率升温至250℃，维持5分钟。进样口温度为150℃，检测器温度为250℃，顶空平衡温度70℃，平衡时间45 min，分流比为10：1。按标准加入法计算供试品中环氧乙烷和二氧六环的含量。结果：在该色谱条件下，环氧乙烷和二氧六环分别在0.5～4 μg/mL和5～40 μg/mL范围内线性关系良好（r≥0.99）；平均回收率均为75%（RSD=5%, n=9）。结论：该方法系统适用性好，精密度、稳定性试验结果符合要求，适用于15-羟基硬脂酸聚乙二醇酯中环氧乙烷和二氧六环含量测定，为15-羟基硬脂酸聚乙二醇酯的质量控制提供参考与指导。 |
| 英文摘要: |
| Objective：The headspace gas chromatography method was developed for the determination of free ethylene oxide and dioxane in Polyoxyl 15 Hydroxystearate to provide scientific basis for its quality control. The samples were separated on column DB-5(15 m×0.32 mm, 1 μm), using 5% phenyl-95% methylpolysiloxane as stationary liquid with temperature programming. Methods：The column temperature was kept at 35℃ for 5 min initially, and raised to 180℃ at the rate of 5℃/min, and then raised to 250℃ at the rate of 30℃/min and subsequently sustained for 5 min. Back inlet temperature was 150℃, FID detector temperature was 200℃, the equilibration time was 45 min and the split ratio was 10:1. Results：Samples were quantitively determined by a standard addition method. Ethylene oxide and dioxide were separated completely with a good linearity at the range of 0.5～4 μg/mL and 5～40 μg/mL（r≥0.99）, and the average recoveries were both 75%（RSD=5%, n=9）under the given chromatographic conditions. Conclusion：With high precision and good stability, the analytical method is specific and suitable for the determination of ethylene oxide and dioxane, providing reference and guidance for the quality control of Polyoxyl 15 Hydroxystearate. |
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