污泥中有机磷酸酯检测的预处理优化

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Abstract

In this his study, based on the steps of "enrichment (accelerated solvent extraction) + purification + detection", the operation parameters of sludge sampling volume, extraction conditions, purification column type, wash polarity and eluent polarity were optimized. The optimal parameters include:a sludge sampling volume of 0.2g, an extraction temperature of 130℃, a 1:1 (v/v) solution mixing ratio of acetone/dichloromethane extractant, and an amino column purification operation. A 2:5 (v/v) mixing ratio was used for the dichloromethane/n-hexane wash solution, and dichloromethane was used as the eluent. The qualitative and quantitative detection of organophosphate esters (OPEs) using an ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS) demonstrated:the matrix spike recoveries for all identified OPEs were between 60% and 120% with a matrix effect no more than ±15%. The pretreatment method could also be appropriate for the determination of OPEs in wastewater samples. This pretreatment method was successfully applied to measure the concentrations of OPEs in the water phase and solid phase samples from the main units in a sewage treatment plant in Beijing, and a good result was achieved.

Key words： organophosphate esters (OPEs) sludge purify sewage

Received: 12 June 2018

PACS:

X705

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