| 引用本文: | 施俊伟,于晓敏,王晋星一,刘倩,周权.GC-MS测定地氯雷他定中基因毒性杂质氯甲酸乙酯的含量[J].中国现代应用药学,2021,38(6):726-729. |
| SHI Junwei,YU Xiaomin,WANG Jinxingyi,LIU Qian,ZHOU Quan.Content Determination of Genotoxic Impurity Ethyl Chloroformate in Desloratadine by GC-MS[J].Chin J Mod Appl Pharm(中国现代应用药学),2021,38(6):726-729. |
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| GC-MS测定地氯雷他定中基因毒性杂质氯甲酸乙酯的含量 |
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施俊伟1,2, 于晓敏3, 王晋星一4, 刘倩4,5, 周权6
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1.浙江大学药学院, 杭州 310058;2.杭州市中医院, 杭州 310007;3.温州医科大学药学院, 浙江 温州 325035;4.贵州医科大学第二附属医院, 贵州 凯里 556000;5.中山大学药学院, 广州 510006;6.浙江大学医学院附属第二医院, 杭州 310009
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| 摘要: |
| 目的 建立地氯雷他定中基因毒性杂质氯甲酸乙酯含量的GC-MS方法。方法 采用CNW CD-ACIDWAX色谱柱（30 m×0.25 mm，0.25 μm）进行分离，载气为氦气，气体流速为1.2 mL·min-1。通过20∶1分流顶空进样，顶空温度为70℃，程序升温：50℃柱温箱条件下保持5 min，再以10℃·min-1升温至80℃，保持3 min。在SIM扫描方式下，检测氯甲酸乙酯的含量，定量离子为m/z 63。结果 氯甲酸乙酯浓度在0.05~4.00μg·mL-1内线性良好，分析方法的重复性、中间精密度、回收率、溶液稳定性、耐用性等均在相关验证指导原则的规定范围内。结论 该定量方法准确、可靠、重复性好，可用于地氯雷他定原料药中氯甲酸乙酯的杂质检测。 |
| 关键词: 地氯雷他定 氯甲酸乙酯 基因毒性杂质 气相色谱-质谱联用法 |
| DOI：10.13748/j.cnki.issn1007-7693.2021.06.016 |
| 分类号:R917.101 |
| 基金项目: |
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| Content Determination of Genotoxic Impurity Ethyl Chloroformate in Desloratadine by GC-MS |
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SHI Junwei1,2, YU Xiaomin3, WANG Jinxingyi4, LIU Qian4,5, ZHOU Quan6
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1.College of Pharmaceutical Sciences, Zhejiang University, Hangzhou 310058, China;2.Hangzhou Hospital of Traditional Chinese Medicine, Hangzhou 310007, China;3.School of Pharmaceutical Sciences, Wenzhou Medical University, Wenzhou 325035, China;4.The Second Affiliated Hospital of Guizhou Medical University, Kaili 556000, China;5.School of Pharmaceutical Sciences, Sun Yat-sen University, Guangzhou 510006, China;6.The Second Affiliated Hospital, Zhejiang University School of Medicine, Hangzhou 310009, China
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| Abstract: |
| OBJECTIVE To develop the GC-MS quantitative method for genotoxic impurity ethyl chloroformate in desloratadine. METHODS CNW CD-ACIDWAX(30 m×0.25 mm, 0.25 μm) column was used with the helium as the carrier gas, the gas flow rate was set at 1.2 mL·min-1. Through 20:1 split head space injection, the headspace temperature was set at 70℃. The temperature was programmed by holding it for 5 min in a column temperature chamber at 50℃ and then heat up to 80℃ at a rate of 10℃·min-1, and kept at 80℃ for 3 min. Determined by SIM mode, the quantitative ion of ethyl chloroformate was m/z 63. RESULTS The calibration curve of ethyl chloroformate showed good linearity within the concentration range of 0.05-4.00 µg·mL-1. All the validation parameters about the method including repeatability, intermediate precision, accuracy, solution stability and durability met the required acceptance of relevant method validation guidance. CONCLUSION The method is accurate, reliable and reproducible, and it is suitable for the determination of ethyl chloroformate in desloratadine. |
| Key words: desloratadine ethyl chloroformate genotoxic impurity GC-MS |
