Citation: HE Jing, YE Xiwen, TANG Zhixu, NIU Zengyuan, LUO Xin, ZOU Li. Determination of organophosphorus flame retardants in textile wastewater by dispersive liquid-liquid microextraction based on solidification of floating organic drop followed by ultra-high performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography, ;2020, 38(6): 679-686. doi: 10.3724/SP.J.1123.2019.10027 shu

Determination of organophosphorus flame retardants in textile wastewater by dispersive liquid-liquid microextraction based on solidification of floating organic drop followed by ultra-high performance liquid chromatography-tandem mass spectrometry

HE Jing ¹ ,
YE Xiwen ^2,, ,
TANG Zhixu ² ,
NIU Zengyuan ^2,, ,
LUO Xin ² ,
ZOU Li ¹

1.
College of Environmental Science and Engineering, Ocean University of China, Qingdao 266100, China;
2.
Qingdao Customs Technology Center, Qingdao 266003, China

Corresponding author: YE Xiwen, NIU Zengyuan,
Received Date: 27 October 2019

Fund Project: National Key Research and Development Project (No. NQI 2016YFF0203702).

A rapid method for the determination of five organophosphorus flame retardants (OPFRs) in textile wastewater was established by dispersive liquid-liquid microextraction (DLLME) based on solidification of floating organic drop (SFO) coupled with ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The analytes were extracted from the water samples by SFO-DLLME, which was performed using a mixture of an extraction solvent that was less dense than water, 1-undecanol, and a dispersive solvent, methanol. The influences of the SFO-DLLME parameters on the extraction efficiencies were studied. 1-Undecanol (extraction solvent, 400 μL) and methanol (dispersive solvent, 300 μL) were added to textile wastewater (containing 2 g NaCl) with pH between 6 and 9, and the solution was shaken for 2 min. Under optimum conditions, the linear ranges of the proposed method were from 2 μg/L to 100 μg/L with correlation coefficients (R²) above 0.99 for all the analytes. The limits of detection (S/N=3) ranged from 2 μg/L to 5 μg/L. The precision of the method was evaluated in terms of repeatability; the relative standard deviations varied from 2.7% to 11.2% (n=6). The relative recoveries ranged from 71.6% to 117.6% for all analytes. Only 3 of the 11 selected samples were tested positive for OPFRs, and the total concentrations of OPFRs in them were in the range of 2.6-3.4 μg/L. Hence, this method is accurate, environmentally friendly, fast, and convenient for the routine analysis of OPFRs in textile wastewater.
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