气相色谱法测定药用辅料聚西托醇1000中的残留杂质
Determination of residual impurities in pharmaceutical excipient cetomacrogol 1000 by gas chromatography
-
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。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.
-
Keywords:
- cetomacrogol 1000 /
- impurity /
- gas chromatography /
- ethylene oxide /
- 1,4-dioxane /
- ethylene glycol /
- diethylene glycol /
- triethylene glycol
-
-
[1] . ACS Omega，2021，6（32）：20975-20983. [2] Eccleston GM. Structure and rheology of cetomacrogol creams：the influence of alcohol chain length and homologue composition［J］. J Pharm Pharmacol，1977，29（3）：157-162. [3] Secretin L，Anyakudo F，Gilissen L，et al. Qualitative analysis of cetomacrogol creams by thin-layer chromatography-flame ionization detection （TLC-FID）［J］. SN Appl Sci，2020，2（9）. doi：https：//doi.org/10.1007/s42452-020-03389-4 .[4] Chen L，Zhang Y，Zheng A，et al. Thoughts on the high quality development of pharmaceutical excipients industry in China［J］. Chin Pharm Aff （中国药事），2021，35（9）：972-977. [5] Liu J，Wu Y，Li HL. Determination of ethylene oxide and dioxane in PEG 10000 by headspace gas chromatography［J］. Drug Stand China（中国药品标准），2017，18（2）：117-119. [6] Yi CC，Sha RL，Chen QY，et al. Quality study of pharmaceutical excipient polysorbate 80［J］. J China Pharm Univ（中国药科大学学报），2020，51（2）：168-174. [7] Lei YJ，Xiong YR，Zhu YY，et al. Determination of ethylene glycol，diethylene glycol and triethylene glycol in poloxamer 188 by gas chromatography［J］. J China Pharm Univ（中国药科大学学报），2019，50（6）：694-698. [8] Gao S，Zhu S，Zhao X，et al. Comparative study on HPLC and GC methods for determination of ethylene glycol and diethylene glycol residues in polyethylene oxide［J］. Chin J Pharm Anal （药物分析杂志），2020，40（10）：1820-1827. [9] Duan MR，He DS，Sun HM，et al. Determination of epoxide impurity in Poloxamer188 by gas chromatography［J］. J Pharm Res（药学研究），2020，39（6）：331-335，340. [10] The British Pharmacopoeia Commission. British Pharmacopoeia：Monograph 1123 ［S］. London：The Stationery Office，2020：1123-1125.[11] The United States Pharmacopeial Convention. United States Pharmacopoeia：Vol 31（3） ［S］.43th ed . Rockville：The United States Pharmacopeial Convention，2020：5955-5957.[12] World Health Organization. The International Pharmacopoeia［EB/OL］. 10th ed .https：//digicollections.net/phint/2020/index.htmL#p/home .[13] Chinese Pharmacopoeia Commission. Chinese Pharmacopoeia：part 4（中华人民共和国药典：四部） ［S］. Beijing：China Medical Science Press，2020：819-820. -
期刊类型引用(8)
1. 刘健弘，张欣橦，李颖娴，杨展，符艺，周瑜芳. 药物缓释体系的研究进展. 广东化工. 2024(15): 90-92+45 . 
百度学术
2. 郑丽君，刘玲，张向荣. 脂质体在乳品中的应用. 中国药剂学杂志(网络版). 2023(01): 34-48 . 百度学术
3. 郭文娣，彭玉帅，许卉，陈华. 脂质体制剂制备工艺及质量控制研究进展. 药物分析杂志. 2023(01): 61-69 . 百度学术
4. 柳宇红，姜宇，郝贵周，刘善奎. 挤出法制备卡巴他赛脂质体的工艺优化. 药学研究. 2023(04): 243-246+284 . 百度学术
5. 吴灿，关延彬，贾永艳. 药剂学课程思政探索——以“脂质体”为例. 中国教育技术装备. 2023(18): 72-74 . 百度学术
6. 毛欣亮，邓惠林，张浩，李吉平，蔡德富，樊丽，孙珈，岳丽玲，潘思文，温宪春. 共载紫草素和盐酸阿霉素pH敏感脂质体的制备及理化性质评价. 齐齐哈尔医学院学报. 2023(23): 2201-2207 . 百度学术
7. 蔡成龙，闫雪生，于蓓蓓，孙丹丹. 透明质酸修饰茯苓皮总三萜脂质体制备与表征研究. 辽宁中医药大学学报. 2022(05): 50-55 . 百度学术
8. 张艺，杭太俊，宋敏. 载药脂质体包封率测定方法的研究进展. 中国药科大学学报. 2021(02): 245-252 . 本站查看
其他类型引用(12)
计量
- 文章访问数:
- HTML全文浏览量: 0
- PDF下载量:
- 被引次数: 20
下载:
