Citation: CHEN Mei-Hong, XU Huai-Zhou, SONG Ning-Hui, WU Sheng-Min, CHENG Jie, LI Jiang, ZHANG Sheng-Hu, SHI Li-Li. Simultaneous Determination of 12 Kinds of Organophosphates in Water and Sediment by High Performance Liquid Chromatography-Tandem Mass Spectrometry[J]. Chinese Journal of Analytical Chemistry, ;2017, 45(7): 987-995. doi: 10.11895/j.issn.0253-3820.170180 shu

Simultaneous Determination of 12 Kinds of Organophosphates in Water and Sediment by High Performance Liquid Chromatography-Tandem Mass Spectrometry

1.
College of Resources and Environmental Engineering, Guizhou University, Guiyang 550025, China;
2.
Nanjing Institute of Environmental Sciences, Nanjing 210042, China;
3.
Second Institute of Oceanography, Hangzhou 310012, China

Received Date: 23 March 2017
Revised Date: 25 May 2017

Fund Project: This work was supported by the National Natural Science Foundation of China (Nos. 21407055, 41503115) and Research Fund on Talent Introduction of Guizhou University (No. (2013)13)

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.
- Organophosphate esters,
- High performance liquid chromatography-tandem mass spectrometry,
- Water samples,
- Sediments
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沈阳化工大学材料科学与工程学院沈阳 110142