Citation: HAN Lin-Xue, QIU Tian, LIN Xiao, LIU Jia-Rong, HU Xiao-Jian, ZHANG Xu. Determination of Four Metabolites of Di(isononyl) Cyclohexane-1,2-dicarboxylate in Urine via Ultra High Performance Liquid Chromatography-Tandem Mass Spectrometry[J]. Chinese Journal of Analytical Chemistry, ;2023, 51(2): 229-238. doi: 10.19756/j.issn.0253-3820.221183 shu

Determination of Four Metabolites of Di(isononyl) Cyclohexane-1,2-dicarboxylate in Urine via Ultra High Performance Liquid Chromatography-Tandem Mass Spectrometry

HAN Lin-Xue ¹ ,
QIU Tian ¹ ,
LIN Xiao ¹ ,
LIU Jia-Rong ² ,
HU Xiao-Jian ¹ ,
ZHANG Xu ^1,,

1.
China CDC Key Laboratory of Environment and Population Health, National Institute of Environmental Health, Chinese Center for Disease Control and Prevention, Beijing 100021, China;
2.
Yanjing Medical College, Capital Medical University, Beijing 101300, China

Corresponding author: ZHANG Xu, zhangxu@nieh.chinacdc.cn
Received Date: 15 April 2022
Revised Date: 19 October 2022

Fund Project: Supported by the National Natural Science Foundation of China (No. 22106154), the State Key Laboratory of Environmental Chemistry and Ecotoxicology, Research Center for Eco-Environmental Sciences, Chinese Academy of Sciences (No. KF2020-17) and the Project of Hubei Key Laboratory of Environmental and Health Effects of Persistent Toxic Substances (No. PTS2019-08).

A method for quantification of four kinds of metabolites of di(isononyl) cyclohexane-1,2-dicarboxylate (DINCH) in urine using ultra high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was developed. Urine sample (2 mL) were deconjugated by β-glucuronidase/arylsulfatase, extracted and cleaned using anion-exchange solid phase extraction cartridge and concentrated to 0.5 mL under gentle stream of nitrogen. The target analytes were separated on Waters Acquity UPLC BEH C₁₈ Column (100 mm×2.1 mm,1.7 μm), and eluted with 0.05% (V/V) acetic acid in water and 0.05% (V/V) acetic acid in acetonitrile in gradient. The target analytes were ionized in negative electrospray ionization (ESI-) mode and scanned under a multiple reaction monitoring (MRM) mode. Quantitative analysis of target analytes in urine was achieved by isotope labelled standard assay. In the range of 0.01-50 ng/mL, all four target analytes exhibited good linearity with correlation coefficients (r) above 0.9996. The method detection limits (MDLs) and method quantification limits (MQLs) were 0.01-0.03 ng/mL and 0.03-0.10 ng/mL, respectively. The recoveies were from 74% to 124%, with the relative standard deviations (RSD) between 1.2% and 15.0%. The intra-day and inter-day precisions were 3.5%-6.2% and 6.9%-9.8%, respectively. The developed method was performed to determinate the DINCH metabolites in 55 human urine samples collected in Beijing. All four DINCH metabolites were detected in urine, and the detected rates of MINCH, oxo-MINCH, OH-MINCH and cx-MINCH were 18.2%, 47.3%, 98.2% and 100%, respectively. The four metabolites were detected in the concentration ranges of
- Emerging plasticizer,
- Bio-monitoring,
- Urine,
- Internal exposure,
- Solid phase extraction
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