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

Determination of Organic Residual Solvents in Jiweiling Freeze-Dry Powder by Capillary Headspace Gas Chromatography

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

Key words:  Jiweiling freeze-dry powder  macroporous adsorption resin  organic residul solvent  capillary headspace gas chromatography

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。

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.