气相色谱法测定药用辅料聚西托醇1000中的残留杂质

李浩宇; 唐宝强; 何东升; 涂家生

doi:10.11665/j.issn.1000-5048.20220306

气相色谱法测定药用辅料聚西托醇1000中的残留杂质

李浩宇^1,2,
唐宝强^1,2,
何东升^1,2,
涂家生^1,2

1.
中国药科大学药学院药用辅料及仿创药物研发评价中心，南京 210009
2.
国家药品监督管理局药物制剂及辅料研究与评价重点实验室，南京 210009

基金项目: 国家“重大新药创制”科技重大专项资助项目（No.2017ZX09101001-006-002）；国家药典委员会药品标准制修订研究课题2020Y047

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出版历程
- 收稿日期: 2022-01-05
- 修回日期: 2022-05-13
- 刊出日期: 2022-06-24

Determination of residual impurities in pharmaceutical excipient cetomacrogol 1000 by gas chromatography

1.
Center for Research Development and Evaluation of Pharmaceutical Excipients and Generic Drugs, School of Pharmacy, China Pharmaceutical University, Nanjing 210009
2.
National Medical Products Administration (NMPA) Key Laboratory for Research and Evaluation of Pharmaceutical Preparations and Excipients, Nanjing 210009, China

Funds: This study was supported by China National Key Hi-Tech Innovation Project for the R&D of Novel Drugs (No.2017ZX09101001-006-002) and the Drug Standard Establishment and Revision Project of Chinese Pharmacopoeia Commission (No.2020Y047)

摘要

摘要: 建立气相色谱法测定聚西托醇1000中残留的环氧乙烷、1，4-二氧六环、乙二醇、二甘醇和三甘醇等杂质，为聚西托醇1000生产质量控制提供参考。采用DB-1色谱柱检测环氧乙烷和1，4-二氧六环，顶空进样，进样口温度150 ℃，检测器温度250 ℃，顶空平衡温度70 ℃，平衡时间45 min。采用VF-17MS色谱柱检测乙二醇、二甘醇和三甘醇，液体进样，进样口温度270 ℃，检测器温度290 ℃。实验结果显示，环氧乙烷和1，4-二氧六环在各加样量范围内线性良好（r > 0.999），精密度RSD小于8.0%，平均回收率分别为90.6%和101.2%；乙二醇、二甘醇和三甘醇在3 ~ 60 μg/mL内线性关系良好（r > 0.999），精密度RSD小于3.0%，回收率均在96% ~ 103%。本研究所建立的方法具有良好的专属性、线性、精密度和回收率，能够有效检测聚西托醇1000中多组分极微量杂质。
- 聚西托醇1000 /
- 杂质 /
- 气相色谱法 /
- 环氧乙烷 /
- 1,4-二氧六环 /
- 乙二醇 /
- 二甘醇 /
- 三甘醇
Abstract: For the quality control of cetomacrogol 1000, a gas chromatographic method for the determination of residual impurities in cetomacrogol 1000, such as ethylene oxide, 1, 4-dioxane, ethylene glycol, diethylene glycol and triethylene glycol, was established and validated.The DB-1 column with headspace injection was used to detect ethylene oxide and 1, 4-dioxane with the inlet temperature of 150 °C, the FID temperature of 250 °C, the headspace equilibration temperature of 70 °C and the equilibration time of 45 min.The VF-17MS column with liquid injection was used to detect ethylene glycol, diethylene glycol and triethylene glycol with the inlet temperature of 270 °C, and the FID temperature of 290 °C.The results showed that ethylene oxide and 1,4-dioxane have a good linearity within their specified addition amount ranges (r > 0.999), with the RSD of precision of below 8.0% and the average recovery rates of 90.6% and 101.2%; and that ethylene glycol, diethylene glycol and triethylene glycol also have a good linearity between 3 ? 60 μg/mL (r > 0.999), with the RSD of precision of below 3.0%, and the recovery rates of 96% ~ 103%.The method established in this study has good specificity, linearity, precision and recovery rate, which can effectively detect the multi-component and trace impurities.
- cetomacrogol 1000 /
- impurity /
- gas chromatography /
- ethylene oxide /
- 1,4-dioxane /
- ethylene glycol /
- diethylene glycol /
- triethylene glycol

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参考文献(13)

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