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氯甲酸异丁酯质量控制研究
引用本文:安巧,梁光义,黄正明,刘昌孝,夏文,曹佩雪.氯甲酸异丁酯质量控制研究[J].精细化工中间体,2013(5):77-80.
作者姓名:安巧  梁光义  黄正明  刘昌孝  夏文  曹佩雪
作者单位:[1]贵州省中国科学院天然产物化学重点实验室,贵州贵阳550002 [2]中国人民解放军第三0二医院,北京100039 [3]天津药物研究院,天津300193 [4]贵州百灵企业集团制药股份有限公司,贵州安顺561000
基金项目:“十二五”国家重大新药创制科技重大专项(2011ZX09102-009-002); 贵州省中药现代化科技产业研究开发专项(黔科合中药字[2012]5054); 贵州省创新人才基地(黔人领发[2011]1号)
摘    要:建立了氯甲酸异丁酯质量内控方法。实验采用毛细管气相内标法含量测定方法,用HP-5(30 m×0.32 mm×0.25μm)毛细管气相色谱柱,FID检测器,以正辛烷为内标进行氯甲酸异丁酯测定。氯甲酸异丁酯在0.300.49μg/μL(r=0.999 9)范围内呈良好线性关系;氯甲酸异丁酯回收率为96.55%。采用滴定方法测定其游离酸含量。

关 键 词:氯甲酸异丁酯  气相色谱法  含量测定

Quality Control of Isobutyl Chloroformate
AN Qiao;LIANG Guang-yi;HUANG Zheng-ming;LIU Chang-xiao;XIA Wen;CAO Pei-xue.Quality Control of Isobutyl Chloroformate[J].Fine Chemical Intermediates,2013(5):77-80.
Authors:AN Qiao;LIANG Guang-yi;HUANG Zheng-ming;LIU Chang-xiao;XIA Wen;CAO Pei-xue
Affiliation:AN Qiao, LIANG Guang-yi, HUANG Zheng-min, LIU Chang-xiao, XIA Wen, CA O Pei-xue (1. The Key Laboratory of Chemistry for Natural Products of Guizhou Province and Chinese Academy of Sciences, Guiyang 550002, China; 2. 302 Hospital of PLA, Beijing 100039, China; 3. Tianjin Institute of Pharmaceutical Research, Tianjin 300193, China; 4. Guizhou Bailing Enterprise Group Pharmaceutical CO., Ltd., Anshun 561000, China)
Abstract:A method for the content determination of isobutyl chloroformate was established by using capillary gas chromatography with a HP-5(30 m×0.32 mm×0.25 μm)capillary column and a flame ionization detector. Octane was used as the internal standard substance. The linear range of isobutyl chloroformate was 0.30 ~ 0.49 μg / μL(r=0.9999)and its recovery was 96.55%. Free acid was measured by titration.
Keywords:Isobutyl chloroformate  GC  capillary
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