同时加速溶剂萃取/气相色谱-质谱法测定植物中13种有机磷酸酯

Determination of Thirteen Organophosphate Esters in Plants Using Gas Chromatography-Mass Spectrometry with Simultaneously Accelerated Solvent Extraction

建立了同时加速溶剂萃取和净化、气相色谱-离子阱二级质谱检测植物中13种有机磷酸酯阻燃剂/增塑剂的分析方法。样品放入以硅胶和活性炭作为在线净化填料的萃取池中,在萃取溶剂为正己烷-丙酮(1∶1,体积比)、萃取温度100℃、静态萃取时间10 min、循环2次的条件下进行加速溶剂萃取,萃取液浓缩后经DB-5MS(30 m×0.25 mm×0.25μm)气相色谱柱分离,选择反应监测模式(SRM)检测,以保留时间和特征离子对定性,内标法定量。结果表明,该方法具有较好的准确度和精密度,13种有机磷酸酯在3个加标水平下的回收率为76.9%~113.0%,相对标准偏差为2.0%~14.6%,方法检出限为0.79~2.27 ng/g,方法定量下限为2.65~7.59 ng/g。该方法简便、快速、准确,可用于植物中13种有机磷酸酯的测定。

A method was developed for the determination of thirteen organophosphate esters in plants by gas chromatography-ion trap tandem mass spectrometry with simultaneously accelerated solvent extraction and purification.Silica gel and active carbon were selected as the on-line purification materials,and successively put into the extracting cell.Then the plant samples were put into the cell for extraction.The accelerated solvent extraction conditions were as follows:extraction solvent:hexane-acetone(1∶1,by volume),the extraction temperature:100℃,the static extraction time:10 min,and the number of extraction cycles:2.The extract was evaporated and separated on a DB-5MS chromatographic column(30 m×0.25 mm×0.25μm),and subsequently detected by ion trap tandem mass spectrometry under selected reaction monitoring(SRM)mode.An internal standard method was adopted for the quantitation.The recoveries obtained were in the range of 76.9%-113.0%,with the relative standard deviations of 2.0%-14.6%.The detection limits and quantitation limits of the method were in the ranges of 0.79-2.27 ng/g and 2.65-7.59 ng/g,respectively.The method is simple,rapid and accurate,and could be used for the determination of 13 organophosphate esters in plants.