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作 者:侯慧杰 张俊杰 王英新 史大勇 解春文 HOU Hui-jie;ZHANG Jun-jie;WANG Ying-xin;SHI Da-yong;XIE Chun-wen(Shandong Dyne Marine Biopharmaceutical Limited Corporation,Shandong Rongcheng 264300,China)
机构地区:[1]山东达因海洋生物制药股份有限公司,山东荣成264300
出 处:《广州化工》2024年第5期107-110,131,共5页GuangZhou Chemical Industry
基 金:山东省重点研发计划(No:2019TSCYCX-31)。
摘 要:采用气相色谱法测定3-氟-4-吗啉基苯胺中吗啉的含量。具体方法:色谱柱:以5%苯基,95%二甲基聚硅氧烷为固定相的毛细管柱;载气:氦气;流速:2 mL/min;柱温条件:起始柱温40℃,维持时间2 min,以11℃/min速率升温至120℃,以33℃/min速率升温至250℃,维持3 min;进样口温度:200℃;FID检测器温度:240℃;分流比:10∶1;进样量:1μL。经方法学验证,方法专属性强,准确度及灵敏度较高,可用于3-氟-4-吗啉基苯胺中吗啉的含量测定。The content of morpholine in 3-fluoro-4-morpholinylaniline was determined by gas chromatography,using column as a capillary column with 5%phenyl and 95%dimethylpolysiloxane as the stationary phase,with carrier gas as Helium gas,flow rate was 2 mL/min;column temperature conditions were as follows:initial column temperature at 40℃,maintaining time for 2 min,heating up to 120℃at a rate of 11℃/min,heating to 250℃at a rate of 33℃/min,maintaining for 3 min,the injection temperature was 200℃,FID detector temperature was 240℃,split ratio was 10∶1,the injection volume was 1μL.The validation results showed that the method had strong specificity,high accuracy and sensitivity,and can be used for the determination of morpholine in 3-fluoro-4-morpholinyl aniline.
关 键 词:气相色谱法 吗啉 3-氟-4-吗啉基苯胺
分 类 号:R917[医药卫生—药物分析学]
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