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

秦威振; 毛丽莎; 陈裕华; 刘桂华; 罗贤如; 姜杰; 管玉峰

doi:10.13421/j.cnki.hjwsxzz.2020.01.013

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

摘要

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 mL乙酸乙酯丙酮溶液（3+2，V+V），涡旋1 min，超声5 min，3 500 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 mL正己烷复溶，CNWBOND NH₂固相萃取柱（6 mL乙酸乙酯，6 mL正己烷活化）富集净化，3 mL乙酸乙酯洗脱2次，氮气吹干，1 mL乙腈水溶液（1+1，V+V）定容，过0.22 μm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，1.8 μm）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。

Abstract:
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 mL 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 mL using n-hexane, enriched and purified through CNWBOND NH₂ solid phase extraction column (conditioned with 6 mL ethyl acetate, 6 mL n-hexane), eluted using 3 mL ethyl acetate twice, dried using nitrogen, adjusted to a constant volume using 1 mL 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.

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