Citation: LI Xin-Hong, XIANG Lei, HUANG Yu-Hong, MO Ce-Hui, LI Yan-Wen, LI Hui, CAI Quan-Ying. Simultaneous Determination of 15 Kinds of Phthalate Esters in Black and Odorous Water by Solid Phase Extraction and Gas Chromatography-Mass Spectrometry[J]. Chinese Journal of Analytical Chemistry, ;2019, 47(11): 1842-1849. doi: 10.19756/j.issn.0253-3820.191276 shu

Simultaneous Determination of 15 Kinds of Phthalate Esters in Black and Odorous Water by Solid Phase Extraction and Gas Chromatography-Mass Spectrometry

Guangdong Provincial Research Center for Environment Pollution Control and Remediation Materials, College of Life Science and Technology, Jinan University, Guangzhou 510632, China

Received Date: 10 May 2019
Revised Date: 11 July 2019

Fund Project: This work was supported by the National Natural Science Foundation of China-Guangdong Joint Fund (No. U1501233), the Research Team Project of the Natural Science Foundation of Guangdong Province (No. 2016A030312009), the Program of the Guangdong Science and Technology Department (Nos. 2017B020238002, 2015B090903070), and the 2017 Science and Technology Project of Guangzhou Water Resources Bureau, China (No. GZCPJ/YB-2016-15).

A solid phase extraction and gas chromatography/mass spectrometry (GC-MS) method was developed for simultaneous extraction and determination of fifteen phthalate esters (PAEs) in black and odorous water. The quantification of 15 kinds of PAEs was performed using a HP-5MS column for chromatographic separation, followed by electren ionization (EI) mass spectra and selected ion monitoring (SIM). Under optimal extraction conditions, 100 mL of water sample at pH 3 was loaded into a WondaSep C₁₈ cartridge, and then eluted with 6 mL of methanol/dichloromethane (1:4, V/V). Satisfactory linearity (R²>0.991) for the target PAEs in matrix of black and odorous water was obtained in the range of 0.05-2 μg/mL, with detection limit of 0.04-0.38 μg/L. The recoveries at two spiked levels (2 and 10 μg/L) in the matrix of black and odorous water generally ranged from 70% to 115%, with relative standard deviation of lower than 10%. The developed method was successfully used to detect PAEs in the actual black and odorous water samples, with total concentration and recoveries (spiked at 2 μg/L) ranging from 2.57 μg/L to 13.69 μg/L and 62% to 115%, respectively.
- Solid-phase extraction,
- Gas chromatography-mass spectrometry,
- Phthalic acid esters,
- Black and odorous water,
- Matrix effect
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