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

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0.9991~0.9998;方法精密度良好,RSD均小于3%;样品在8h内稳定;正己烷检测限为0.08μg·mL- 1、苯为0.025μg·mL- 1、甲苯为0.04μg·mL- 1、(对、间、邻)二甲苯均为0.2μg·mL- 1、苯乙烯为0.4μg·mL- 1、二乙烯苯为0.1μg·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。

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.