气相色谱-质谱法测定卤化丁基橡胶塞中油酸酰胺

Determination of Oleamide in Halogenated Butyl Rubber Stopper by Gas Chromatography-mass Spectrometry

本文通过试验建立了一种对药用橡胶塞中风险物质油酸酰胺的迁移量的检测方法,采用气相色谱-质谱法电子轰击离子源和选择离子检测模式分析测定药用卤化丁基橡胶塞中油酸酰胺的含量。样品经有机溶剂正己烷超声提取,用气相色谱质谱联用仪进行定性定量分析,油酸酰胺的响应浓度在0.5~50 mg/L范围内与峰面积呈线性关系,同时用DB-5MS毛细管色谱柱能够进行有效的分离,仪器检出限(三倍信噪比)为0.05 mg/L,方法检出限为12.5 mg/kg。阴性样品的加标回收率在为87.1%~102.4%,测定值的相对标准偏差(6次)为0.9%~1.5%。

A method for determining the migration of oleic amide in medical rubber stopper was established.The content of oleic amide in medical halogenated butyl rubber stopper was determined by gas chromatography-mass spectrometry with electron bombardment ion source and selective ion detection mode.The samples were extracted by organic solvent n-hexane ultrasound and analyzed qualitatively and quantitatively by gas chromatography-mass spectrometry.The response concentration of oleamide was linear with the peak area in the range of 0.5~50 mg/L.At the same time,DB-5 MS capillary chromatographic column could be used for effective separation.The detection limit of the instrument(triple signal-to-noise ratio) was 0.05 mg/L and the detection limit of the method was 12.5 mg/kg.The recoveries of negative samples were 87.1%~102.4%,and the relative standard deviation(6 times) was 0.9%~1.5%.