| 引用本文: | 郑亚杰,贾继明,刘兴国,王贵金,宋剑.毛细管顶空气相色谱法测定肌萎灵冻干粉中有机溶剂的残留量[J].中国现代应用药学,2010,27(13):1201-1203. |
| .Determination of Organic Residual Solvents in Jiweiling Freeze-Dry Powder by Capillary Headspace Gas Chromatography[J].Chin J Mod Appl Pharm(中国现代应用药学),2010,27(13):1201-1203. |
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| 摘要: |
| 目的 建立肌萎灵冻干粉中AB-8型大孔吸附树脂有机溶剂(正己烷、苯、甲苯、邻二甲苯、间二甲苯、对二甲苯、苯乙烯、二乙烯苯)残留量的检测方法。方法 采用顶空气相色谱程序升温方法，以AT-WAX毛细管色谱柱分离，氢火焰离子化检测器检测。结果 8种大孔吸附树脂残留溶剂分离良好；在各自线性范围内峰面积和浓度均有良好的线性关系，r为0.999 1~0.999 8；方法精密度良好，RSD均小于3%；样品在8 h内稳定；正己烷检测限为0.08 μg·mL-1、苯为0.025 μg·mL-1、甲苯为0.04 μg·mL-1、(对、间、邻)二甲苯均为0.2 μg·mL-1、苯乙烯为0.4 μg·mL-1、二乙烯苯为0.1 μg·mL-1。结论 本法操作简便、准确可靠，可用于控制肌萎灵冻干粉中AB-8型大孔吸附树脂有机溶剂残留量。 |
| 关键词: 肌萎灵冻干粉 大孔吸附树脂 残留溶剂 毛细管顶空气相色谱法 |
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| Determination of Organic Residual Solvents in Jiweiling Freeze-Dry Powder by Capillary Headspace Gas Chromatography |
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ZHENG Yajie JIA Jiming LIU Xingguo WANG Guijin SONG Jian
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| Abstract: |
| OBJECTIVE To establish a method for determination of residual organic solvents from the AB-8 macroporous adsorption resin in Jiweiling freeze-dry powder, including n-hexane, benzene, toluene, 1,2-xylene, 1,3-xylene, 1,4-xylene, stryene, divinylbenzene. METHODS The residual organic solvents were analyzed by headspace gas chromatography on AT-WAX capillary column, FID detector and by temperature programming. RESULTS The eight residual organic solvents were completely separated. There was good linearity in resparatively linear ranges and r was 0.999 1-0.999 8, the RSD of precision was less than 3%, the samples were stable in 8 h, the detection limits were n-hexane 0.08 μg·mL-1, benzene 0.025 μg·mL-1, toluene 0.04 μg·mL-1, (1,2-; 1,3-; 1,4-)xylene 0.2 μg·mL-1, stryene 0.4 μg·mL-1, divinylbenzene 0.1 μg·mL-1. CONCLUSION The method is simple and accurate and can be used to detect and control the organic residul solvents from the AB-8 macroporous adsorption resin in Jiweiling freeze-dry powder. |
| Key words: Jiweiling freeze-dry powder macroporous adsorption resin organic residul solvent capillary headspace gas chromatography |
