固相萃取-超高效液相色谱-串联质谱法测定EVA地垫中3种有机磷酸酯阻燃剂  

Determination of Three Organophosphate Esters Flame Retardants in EVA Mats by UPLC-MS/MS Combined with SPE

作　　者：李长于 胡丹 廖上富 鹿燕 杨铭 孙宵欢 Li Changyu;Hu Dan;Liao Shangfu;Lu Yan;Yang Ming;Sun Xiaohuan(Zhejiang Fangyuan Test Group Co.,Ltd.,Hangzhou 310018,China)

机构地区：[1]浙江方圆检测集团股份有限公司

出　　处：《塑料科技》2019年第9期110-114,共5页Plastics Science and Technology

基　　金：浙江省质量技术监督系统科研计划项目(20180346)资助

摘　　要：建立了固相萃取-超高效液相色谱-串联质谱法测定乙烯-醋酸乙烯共聚物(EVA)地垫中磷酸三(2-氯乙基)酯(TCEP)、磷酸三(2-氯丙基)酯(TCPP)和磷酸三(1,3-二氯-2丙基)酯(TDCP)3种有机磷酸酯阻燃剂含量的分析方法。样品经乙腈超声提取、离心氮吹浓缩后,再经Florisil固相萃取柱净化,采用乙腈-0.1%甲酸水溶液为流动相,在HSS T3色谱柱(100 mm×2.1 mm×1.8μm)上梯度洗脱分离。在电喷雾正离子源(ESI+)模式下,采用多反应监测(MRM)模式对目标物进行检测,外标法定量。结果表明:3种有机磷酸酯阻燃剂在1~100μg/L浓度范围内均与对应的峰面积呈良好线性关系(r2>0.99);TCEP、TCPP、TDCP的方法检出限(S/N=3)分别为0.75、1.0、3.0 mg/kg,加标回收率为81.9%~104.0%,相对标准偏差为0.27%~8.3%。该方法操作简单、快速、灵敏度高,适用于EVA地垫中有机磷酸酯阻燃剂的测定。A method for the determination of three organophosphate esters(OPEs,including TCEP,TCPP,TDCP)flame retardants in ethylene-vinyl acetate(EVA)mats was established by using ultra high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)combined with solid phase extraction(SPE).The samples were ultrasonically extracted with acetonitrile.Then the analytes were centrifuged,concentrated and purified with Florisil solid phase extraction column,separated in a HSS T3 column(100 mm×2.1 mm,1.8μm)by gradient elution using acetonitrile-0.1%formic acid in water as the mobile phase.The target analytes were ionized by the electrospray ionization positive(ESI+)mode and detected using the multiple reaction monitoring(MRM)mode.The results were quantitated by external standard method.Results indicated that the standard curves were linear over the selected concentration range of 1~100μg/L for three OPEs flame retardants(r2>0.99).The limits of method detection for TCEP,TCPP and TDCP(S/N=3)were 0.75,1.0 and 3.0 mg/kg,respectively.The mean recoveries(n=5)at three spiked levels were in the range of 81.9%~104.0%,and the relative standard deviations(RSDs)were in the range of 0.27%~8.3%.The method is simple,rapid,high sensitivity,and suitable for the determination of OPEs flame retardants in EVA mats.

关 键 词：固相萃取 超高效液相色谱-串联质谱 乙烯-醋酸乙烯共聚物 地垫 有机磷酸酯 阻燃剂 

分 类 号：O657.63[理学—分析化学]