Simultaneous Determination of 12 Kinds of Organophosphates inWater and Sediment by High Performance LiquidChromatography-Tandem Mass Spectrometry / 分析化学

ABSTRACT

A method was developed for determination of 12 kinds of phosphate compounds in water and sediment by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) coupled with solid phase extraction (SPE) and ultrasonic extraction.The water samples were concentrated by HLB solid-phase extraction (SPE) column and eluted twice with ethyl acetate, ultrasonic solvent extraction for sediment samples and then repeated the operation of water samples after diluted with deionized water.The sample were separated on a ZORBAX Eclipse Plus C18 (150 mm × 2.1 mm, 3.5 μm) column by a gradient elution with 0.2% formic acid aqueous solution and methanol as the mobile phase.Ion mode analysis was monitored by high performance liquid chromatography mass spectrometer (MRM).The target compounds were quantified by external standard method.At the spiked levels (0.05, 0.1 and 0.5 μg/L), the average recoveries of 12 kinds of OPEs in water samples ranged from 66.4% to 115%, except for TMP (28.5%-47.8%) and TEHP (22.4%-73.8%).The relative standard deviation RSD (n=3) was 0.5%-9.09%, and the method quantification (MOQ) was 0.001-0.05 μg/L, However at the spiked levels of 5, 10 and 50 μg/kg, the average recoveries of 12 kinds of OPEs in sediment samples ranged from 65.4% to 120.0%, except for TMP (35.7%-44.9%) and TCEP (31.2%-48.9%).The relative standard deviation RSD (n=3) was 0.01%-9.54%, and the MOQ for sediment was 0.02-2.0 μg/kg dw.Based on the above methods, the detection and analysis of the targets in the water and sediments samples of Taihu Lake were carried out.The results showed that the concentrations of ΣOPEs were 0.1-1.7 μg/L and 8.1-420 μg/(kg dw), respectively.