QuEChERS-超高效液相色谱-串联质谱法测定食物中有机磷酸酯阻燃剂
Determination of organophosphate ester flame retardants in foodstuffs by QuEChERS and ultra-high performance liquid chromatography coupled with tandem mass spectrometry
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摘要: 本文建立了适用于多种食物中有机磷酸酯（OPEs）阻燃剂的快速分析方法.方法基于QuEChERS方法对样品进行萃取和净化，并对萃取溶剂和净化吸附剂进行优化，最终建立的方法采用含0.1%甲酸的乙腈作为萃取溶剂，萃取液用N-丙基乙二胺（PSA）和十八烷基硅烷（C18）去除基质干扰；待测物采用超高效液相色谱-串联质谱法（UPLC-MS/MS）检测.对10种测试的OPEs采用同位素内标法定量，方法定量限（MQLs）为0.05 ng·g-1（TMP）-0.42 ng·g-1（TEHP）鲜重之间，加标相对回收率在72.5%-105.5%.该方法灵敏度、准确度和精密度均符合食物中OPEs残留测定要求，并成功应用于实际样品检测.Abstract: A method was developed for the rapid determination of 10 organophosphate esters (OPEs) in foodstuffs based on QuEChERS and UPLC-LC-MS/MS. The extraction solvent and clean-up sorbents were optimized during the method development. In the optimized method, acetonitrile containing 0.1% formic acid was used for extraction. Primary-secondary-amine (PSA) together with octadecylsilane (C18) were applied as clean-up sorbents. Determination of analytes was performed on ultrahigh performance liquid chromatography coupled with tandem mass spectrometry. Matrix-matched internal standard curve was employed to quantify the OPEs. The method quantification limits of 10 OPEs ranged from 0.05 ng·g-1 of TMP to 0.42 ng·g-1 of TEHP. The relative recoveries were 72.5%-105.5% for the analytes. Finally, the method was successfully applied to the analysis of OPEs in real food samples.
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