液相色谱串级质谱同时测定木制品中3种有机磷酸酯阻燃剂

Simultaneous determination of three kinds organophosphorous flame retardants in wood based panels by LC-MS/MS

为建立有效的阻燃剂的使用规范和为监管制度提供理论依据,本文建立了微波辅助萃取,液相色谱串级质谱法同时测定木制品中3种有机磷阻燃剂分析方法,并考察了萃取溶剂、萃取条件、流动相对试验结果的影响。结果表明,以丙酮为萃取溶剂,70℃微波辅助萃取30 min,利用多反应检测MRM模式,TCEP、TDCP在线性范围0.02-1.0 mg/kg,TCPP在线性范围0.002-0.2 mg/kg内质量浓度与响应值呈现良好的线性关系,定量下限分别为27、50、8μg/kg,加标回收率82.7%-98.3%,相对标准偏差1.8%-10.8%。该方法操作简单,提取效果较好,能够有效的检测木制品中三种有机磷酸酯阻燃剂。

In order to establish effectively using criterion and control system, we established three kinds of organophosphorous flame retardants test method in wood products in this article, based on microwave assisted extraction coupled with LC-MS/MS. We also discussed the influence of test such as extraction solvent, extraction condition and moving phase. The result indicates that the optimal conditions were as follows： extraction solvent： acetone, extraction temperature： 70 ℃, extraction time： 30 min. Under the optimal conditions, TCEP,TDCP calibration curves were linear in the range of 0.02- 1.0 mg/kg, TCPP calibration curve was linear in the range of 0.002-0.2 mg/kg, the LOQ were 27, 50, 8 μg/kg, respectively, the recovery distributed in the range of 82.7%-98.3%, the RSD distributed in the range of 1.8%-10.8%. The method is effective in extracting 3 kinds of organophosphorous flame retardants in wood products, easily to operate and has a preferable extracting effect.