微波萃取-GC/MS法测定乙烯-乙酸乙烯酯共聚物制品中的苯乙酮

Determination of Acetophenone in EVA Products by Microwave Extraction-GC/MS Method

建立了采用微波萃取-气相色谱/质谱（GC/MS）法检测乙烯-醋酸乙烯酯共聚物（EVA）制品中苯乙酮的方法。将破碎后的样品用甲苯进行微波萃取,萃取液经硅胶小柱净化、平行蒸发定量浓缩后采用GC/MS法测定含量,外标法定量。优化了样品前处理条件,包括前处理方式的选择、微波萃取溶剂和萃取时间的选择,以及净化小柱的选择。对于苯乙酮标准溶液,在0.1~10 mg/L范围内,线性关系良好,相关系数大于0.998;方法定量测定下限为0.5 mg/kg,相对标准偏差为2.2%~5.5%,加标回收率为87.5%~95.3%。该方法操作简便分、析迅速结、果准确可,以满足对EVA制品中苯乙酮的定性和定量分析。

A new method was established for the determination of acetophenone in EVA products by microwave extraction technique combining with GC/MS method.The sample was crushed and then extracted with toluene in microwave extraction equipment.The extract was purified with silica gel solid phase extraction cartridge,and then quantitatively concentrated with parallel evaporation instrument.The pretreatment condition,including the extraction method,extractant,microwave extraction time and SPE cartridge is optimized.Under the optimum separation and detection condition,acetophenone is confirmed and determined with external standard method.The standard curves of acetophenone solution are linear in the concentration range of 0.1~10 mg/L with correlation coefficient more than 0.998.The limit of quantitation is 0.5 mg/kg.The recoveries range from 87.5% to 95.3%,with the relative standard deviation（RSD） of 2.2%~5.5%.This method is rapid,simple,accurate,and is suitable for qualitatively confirm and quantitatively analysis of the content of acetophenone in EVA products.