气相色谱-质谱法快速测定罗氏海盘车中6种邻苯二甲酸酯类有机污染物

建立了气相色谱-质谱联用技术(GC-MS)测定罗氏海盘车中6种邻苯二甲酸酯类化合物(PAEs)的方法,采用丙酮-正己烷混合溶剂超声提取,通过中性氧化铝和弗罗里硅土填装层析柱净化样品,选用HP-5MS毛细色谱柱分离,选择离子监测模式(SIM)进行定性定量。该方法能同时分离测定罗氏海盘车中邻苯二甲酸二甲酯、邻苯二甲酸二乙酯、邻苯二甲酸二正丁酯、邻苯二甲酸丁基苄酯、邻苯二甲酸二(2-乙基己基)酯、邻苯二甲酸二正辛酯等6种邻苯二甲酸酯类化合物。在优化条件下,方法标准曲线的相关系数为0.9975～0.9996,回收率为80.30%～119.00%,精密度(RSD,n=7)为2.2%～5.7%,方法最低检出限为10.00 ng/g。运用建立的方法对罗氏海盘车样品进行分析,检测出罗氏海盘车中含有邻苯二甲酸二异丁酯、邻苯二甲酸二正丁酯、邻苯二甲酸二(2-乙基己基)酯3种污染物,3种污染物含量均低于欧盟的限量标准,同时远低于其他各类食品中的检出含量,样品中邻苯二甲酸二(2-乙基己基)酯平均含量偏高。本法具有高的选择性、灵敏度和准确度,适用于罗氏海盘车中痕量PAEs的测定,为保护海洋环境及海洋资源开发提供技术支持。

Determination of Six Phthalate Ester Contaminants in Asterias rollestoni Bell Samples by Gas Chromatography-Mass Spectrometry

Gas Chromatography-Mass Spectrometry(GC-MS) was used to determine six phthalate ester contaminants in Asterias rollestoni Bell samples.The samples were sonic extracted with n-hexane-acetone.Then,the extracting solution step was followed by a combined purification separation step on an alumina-silica column.The analytes were separated by GC with an HB-5 capillary column,and then simultaneously identified and quantified by Selected Ion Monitoring(SIM) mode.Under the optimized conditions,all six of the PAEs components were separated completely from each other.The correlation coefficients of the standard curves were 0.9975~0.9996.The recoveries were within 80.30%-119.00%,detection limits of the six PAEs were 10.00 ng/g with 2.2%-5.7% RSD(n=7).Isobutyl phthalate,dibutyl phthalate and di-2-ethylhexyl phthalate were found in all of the Asterias rollestoni Bell samples.However,the total contents of Isobutyl phthalate,dibutyl phthalate and di-2-ethylhexyl phthalate in the samples were lower than the daily toleration limit specified in European regulations and the content in other groceries.The average concentration of isobutyl phthalate in all the samples was higher than those of the other phthalate esters.The method was highly selective,rapid and sensitive,which is completely suitable for the determination of trace PAEs analysis in marine biology samples.It is a suitable technology to support marine environment protection and resource exploration.