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 ×0.25 μm)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 simuhaneously 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 ℃C,the static extraction time:10 min,and the number of extraction cycles:2.The extract was evaporated and separated on a DB-5 MS chromatographic column (30 m × 0.25 mm × 0.25 μm),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.
展开▼
