摘要
目的 :建立顶空气相色谱法分析几丁糖酯中溶剂残留。方法 :采用水溶液顶空和固体顶空 2种气相色谱法 ,用AC -2 0石英毛细管色谱柱 ,以正丙醇为内标进行定量。结果 :水溶液顶空气相色谱法乙醇的线性范围为 8～ 192 μg·mL-1,丙酮的线性范围为 2～ 6 4μg·mL-1;方法的回收率为乙醇 10 3 3% ,丙酮 95 71% ,RSD均为 4 2 % ;最低检测限溶液中乙醇为 4μg·mL-1,丙酮为 1μg·mL-1。固体顶空气相色谱法乙醇的线性范围为 0 16～ 2 4μg·mL-1,丙酮的线性范围为 0 16～ 1 6 μg·mL-1;方法的回收率为乙醇 96 32 % ,丙酮 10 2 1% ,RSD分别为 3 5 %和 2 6 % ;最低检测限乙醇为 0 12 μg·g-1,丙酮为 0 0 6 μg·g-1。结论 :此 2种方法简单 ,准确 ,灵敏度高 ,经显著性检验二者无显著性差异。
Objective:To develop headspace gas chromatography for the determination of residual solvent in chitosan ester.Methods:Using two methods which were solution headspace analysis and solid headspace analysis with AC-20 capillary column and n -propanol as internal standard.Results:In solution headspace analysis,the linear concentration region of ethanol was 8～192 μg·mL\+\{-1\},acetone was 2～64 μg·mL\+\{-1\},the relative recovery of ethanol was 103 3%,acetone was 95 71%,with RSD 4 2% respectively,the lowest detective concentration was 4 μg·mL\+\{-1\} for ethanol and 1 μg·mL\+\{-1\} for acetone.In solid headspace analysis,the linear concentration region of ethanol was 0 16～2 4 μg·mL\+\{-1\},acetone was 0 16～1 6 μg·mL\+\{-1\},the relative recovery of ethanol was 96 32%,acetone was 102 1%,with RSD 3 5% and 2 6% respectively,the lowest detective concentration was 0 12 μg·g\+\{-1\} for ethanol and 0 06 μg·g\+\{-1\} for acetone.Conclusion:These two methods are simple,accurate and sensitive,there is no remarkable difference between these two methods.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2001年第4期276-278,共3页
Chinese Journal of Pharmaceutical Analysis
基金
国家"8 6 3"资助项目 (819-0 7-0 3)
关键词
顶空气相色谱法
溶剂残留
几丁糖酯
测定
headspace gas chromatography,residual solvent,chitosan ester
