超声辅助提取-固相萃取-同位素稀释高效液相色谱串联质谱测定室内灰尘中5种有机磷酸酯阻燃剂  

Determination of Five Organophosphate Flame Retardants in Indoor Dust using Ultrasound Assisted Extraction-Solid Phase Extraction-Isotopic Dilution High Performance Liquid Chromatography-tandem Mass Spectrometry

作　　者：秦威振 毛丽莎[2] 陈裕华[2] 刘桂华[2] 罗贤如[2] 姜杰[2] 管玉峰[3] QIN Weizhen;MAO Lisha;CHEN Yuhua;LIU Guihua;LUO Xianru;JIANG Jie;GUAN Yufeng

机构地区：[1]深圳市龙华区疾病预防控制中心,广东省深圳518000 [2]深圳市疾病预防控制中心理化检测所 [3]华南师范大学化学与环境学院

出　　处：《环境卫生学杂志》2020年第1期76-80,共5页JOURNAL OF ENVIRONMENTAL HYGIENE

基　　金：深圳市科技创新委员会知识创新计划基础研究项目(JCYJ20170306160527011,JCYJ20170306160932340);深圳市卫生计生系统科研项目(201602003);深圳市三名工程项目(SZSM201811070).

摘　　要：目的建立灰尘中磷酸三苯酯(TPHP)、磷酸三甲苯酯(TCP)、磷酸三(2-氯乙基)酯(TCEP)、磷酸三(2-氯丙基)酯(TCPP)和磷酸三(1,3-二氯异丙基)酯(TDCPP)5种有机磷酸酯阻燃剂的超声辅助提取-固相萃取(UAE-SPE)-同位素稀释高效液相色谱-串联质谱(HPLC-MS-MS)检测方法。方法取室内灰尘50 mg,加入3 m L乙酸乙酯丙酮溶液(3+2,V+V),涡旋1 min,超声5 min,3500 r/min离心5 min,取上层清液,循环3次,合并上清液,将合并上清液氮吹至近干,3 m L正己烷复溶,CNWBOND NH2固相萃取柱(6 m L乙酸乙酯,6 m L正己烷活化)富集净化,3 m L乙酸乙酯洗脱2次,氮气吹干,1 m L乙腈水溶液(1+1,V+V)定容,过0.22μm尼龙滤膜,以0.1%甲酸溶液和0.1%甲酸乙腈溶液为流动相,ACQUITY UPLC4HSS T3色谱柱(150 mm×2.1 mm,1.8μm)梯度洗脱分离,电喷雾离子源正离子模式(ESI+),多反应监测(MRM)模式检测。结果5种有机磷阻燃剂在(6.0~500)μg/L范围内线性关系良好,其相关系数均>0.999,检出限范围(1.8~36.0)ng/g,定量限范围(5.9~120.0)ng/g,回收率范围75.0%~116.7%,精密度(RSD)范围2.3%~9.7%。结论该方法操作快速可靠,适用于室内灰尘中5种有机磷酸酯阻燃剂的同时测定。Objectives To develop a method for the determination of five organophosphate flame retardants,triphenyl phosphate( TPHP),tritotyl phosphate( TCP),tris-( 2-chloroethyl) phosphate( TCEP),tris-( 2-chloropropyl) phosphate( TCPP) and tris-( 1,3-dichloropropyl) phosphate( TDCPP),in indoor dust using Ultrasound Assisted Extraction-Solid Phase Extraction( UAE-SPE)-High Performance Liquid Chromatography-tandem Mass Spectrometry( HPLC-MS-MS). Methods Add 3 m L ethyl acetate-acetone( 3 + 2,V + V) into the dust sample( 50 mg). After 1 min vortex,5 min ultrasound,and 5 min centrifugation at 3 500 r/min,and the operation was repeated three times. The supernatant of each time was combined and concentrated to near dryness using nitrogen,reconstituted to 3 m L using n-hexane,enriched and purified through CNWBOND NH2 solid phase extraction column( conditioned with 6 m L ethyl acetate,6 m L n-hexane),eluted using 3 m L ethyl acetate twice,dried using nitrogen,adjusted to a constant volume using 1 m L acetonitrile-water( 1+1,V+V) and filtered with 0. 22 μm nylon filter. The five organophosphate flame retardants were eluted and separated in gradient using ACQUITY UPLC  HSS T3 column( 150 mm × 2. 1 mm,1. 8 μm) with 0. 1% formic acid solution and acetonitrile solution of 0. 1% formic acid as mobile phase,then determined under positive ion mode of Electrospray Ionization( ESI+) and Multiple Reaction Monitoring( MRM) mode. Results The five organophosphate flame retardants showed a good linearity in the range of( 0. 5-500) μg/L,and the correlation coefficients were more than 0. 999. The limit of detection was in the range of( 1. 8-36. 0) ng/g,and the limit of quantification was in the range of( 5. 9-120. 0) ng/g. The recovery was in the range of 75. 0%-116. 7% with the relative standard deviations( RSD) of 2. 3%-9. 7%. Conclusions The method is fast and reliable,which is suitable for simultaneous determination of five organophosphate flame retardants in indoor dust.

关 键 词：有机磷酸酯阻燃剂 室内灰尘 超声辅助提取 固相萃取 高效液相色谱-串联质谱 

分 类 号：O657.6[理学—分析化学]