GC和GC/MS法测定洗涤及化妆用品中二噁烷残留量

建立了用毛细管气相色谱配氢火焰离子化检测器测定洗涤和化妆品中二噁烷的方法。样品用适量的水提取,将二噁烷完全溶解。加入1.0 g氯化钠固体,产生“盐析”效应,以增加二噁烷在顶空瓶中的浓度。70℃时于顶空瓶中混合40 min,达到气液平衡状态,取上清气体直接注入气相色谱进行分析。采用程序升温,用保留时间定性,外标法定量。并进一步采用气相色谱-质谱定性定量。该方法测定二噁烷含量具有较高的准确度。二噁烷回收率为98.8%~108.5%,相对标准偏差2.95%~7.61%,最低检出限为2.5mg/kg。

Residue Determination of Dioxane in Washing Things and Cosmetics by Gas Chromatography and Gas chromatography-Mass Spectrometry

Determination with gas chromatography/flame ionization detector(GC/FID) for dioxane in cosmetics was developed.The cosmetics were extracted with water and dioxane was dissolved completely.1.0 g sodium chloride was added,producing "salting-out" effect,to increase the concentration of dioxane in headspace bottles.The cosmetics were mixed with water for 40 min at 70 ℃,then made gas-liquid balance state.The upper clear gas was injected into gas chromatography(GC) for detection.Programmed temperature was adopted,retention time of the chromatogram could be applied for qualitative analysis,and external standard was used for quantitative analysis.The quality and the quantity of the sample were confirmed further by gas chromatography-mass spectrometry.The result indicated good accuracy.The recovery rates of the dioxane were 98.8%108.5%.The RSDs of the dioxane were 2.95%-7.61%.The low detection limits of the method were 2.5 mg/kg.