Citation: GU Jun-Jie, HU Man, ZHANG Yi-Ning, QU Wei-Dong, ZHOU Ying. Ultra-High Performance Liquid Chromatography Coupled with Triple Quadrupole Mass Spectrometry for Simultaneous Determination of Organophosphate Triesters and Diesters in Serum for Human Biomonitoring Study[J]. Chinese Journal of Analytical Chemistry, ;2021, 49(8): 1384-1392. doi: 10.19756/j.issn.0253-3820.201541 shu

Ultra-High Performance Liquid Chromatography Coupled with Triple Quadrupole Mass Spectrometry for Simultaneous Determination of Organophosphate Triesters and Diesters in Serum for Human Biomonitoring Study

GU Jun-Jie ^1,2,4 ,
HU Man ^1,2,4 ,
ZHANG Yi-Ning ^1,2,4 ,
QU Wei-Dong ^1,3 ,
ZHOU Ying ^1,2,4,,

1.
Centers for Water and Health, Key Laboratory of Public Health Safety, Ministry of Education, Fudan University, Shanghai 200032, China;
2.
Department of Chemistry in Public Health Science, School of Public Health, Fudan University, Shanghai 200032, China;
3.
Department of Environmental Health, School of Public Health, Fudan University, Shanghai 200032, China;
4.
Pudong New Area for Disease Control and Prevention, Fudan University Pudong Institute of Preventive Medicine, Shanghai 200136, China

Corresponding author: ZHOU Ying, yingchou@fudan.edu.cn
Received Date: 7 September 2020
Revised Date: 19 May 2021

Fund Project: Supported by the National Key Research and Development Program of China (No.2017YFC1600500) and the National Natural Science Foundation of China (No.81373089).

A method for rapid and simultaneous determination of organophosphate triesters (triphenyl phosphate (TPHP), triethyl phosphate (TEP), tri-n-butylphosphate (TnBP), tri(2-chloroethyl) phosphate (TCEP)) and diesters (diethyl phosphate (DEP) and diphenyl phosphate (DPHP)) in human serum by ultra-high performance liquid chromatography coupled with triple quadrupole mass spectrometry (UPLC-MS/MS) was developed. Serum sample (400 μL) was extracted using 1.2 mL of ethyl acetate with 60 μL of formic acid, followed by concentrating the extracts with freeze vacuum centrifugation technology. The sample was separated on a Phenomenex Kinetex 2.6 μm F5 LC column with formic acid aqueous solution and methanol as the mobile phase, and then detected in turn under electrospray ionization (ESI) positive and negative ion multiple reactive monitoring (MRM) mode. Stable isotope-labeled internal standards were used to improve the assay performance of UPLC-MS/MS. The analytical parameters involving sample pretreatment, chromatographic separation and mass determination were optimized. Under the optimal conditions, low limits of detection (0.002-0.01 ng/mL), wide linearity (0.05-50 ng/mL) and good recovery (56.1%-112.2%) were achieved. The intra-day and inter-day precisions were expressed as variation coefficients within 15%. The proposed method was successfully applied to the determination of six target compounds in 30 serum specimens collected from residents living in Shanghai city. This method provided a reliable alternative for large-scale monitoring trace level of organophosphate triesters and diesters in human exposure measurement and risk assessment.
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