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Hydrophilicity nano-titania coating modified magnetic graphene oxide for pass-through cleanup of fipronil and its metabolites in human blood.

Authors
  • He, Shi-Wei1
  • Zhao, Yong-Gang2
  • Zhang, Yun1
  • Jin, Mi-Cong3
  • Zhu, Yan4
  • 1 Department of Chemistry, Zhejiang University, Hangzhou, Zhejiang, 310027, China. , (China)
  • 2 Department of Chemistry, Zhejiang University, Hangzhou, Zhejiang, 310027, China; Key Laboratory of Health Risk Appraisal for Trace Toxic Chemicals of Zhejiang Province, Ningbo Municipal Center for Disease Control and Prevention, Ningbo, Zhejiang, 315010, China. , (China)
  • 3 Key Laboratory of Health Risk Appraisal for Trace Toxic Chemicals of Zhejiang Province, Ningbo Municipal Center for Disease Control and Prevention, Ningbo, Zhejiang, 315010, China. , (China)
  • 4 Department of Chemistry, Zhejiang University, Hangzhou, Zhejiang, 310027, China. Electronic address: [email protected] , (China)
Type
Published Article
Journal
Journal of chromatography. A
Publication Date
Jun 08, 2018
Volume
1553
Pages
16–24
Identifiers
DOI: 10.1016/j.chroma.2018.04.019
PMID: 29691057
Source
Medline
Keywords
License
Unknown

Abstract

A novel hydrophilicity nano-titania coating modified magnetic graphene oxide (HTC-Mag-GO) has been synthesized. It has been evaluated in PRiME (process, robustness, improvements, matrix effects, ease of use) pass-through cleanup procedure for human blood prior to analysis of fipronil and its metabolites, i.e., fipronil sulphone, fipronil sulphide and fipronil desulfinyl by liquid chromatography-tandem quadrupole mass spectrometry (LC-MS/MS). Compared with the Oasis PRiME HLB cartridge, HTC-Mag-GO is much more effective for the removal of matrix effect. Furthermore, it is beneficial to protect the chromatographic column and ESI source by the HTC-Mag-GO PRiME pass-through cleanup procedure, resulting from the much cleaner blood samples. Under the optimum conditions, the results show higher cleanup efficiency of HTC-Mag-GO with recoveries in the range of 92.4%-108%. Especially, the HTC-Mag-GO is also evaluated for reuse (20 times) without much sacrifice of the cleanup efficiency. The limits of quantification (LOQs) for fipronil, fipronil sulphone, fipronil sulphide and fipronil desulfinyl are 8.9 ng/L, 7.2 ng/L, 8.0 ng/L and 42 ng/L, respectively. The developed method has also been successfully applied to monitoring fipronil and its metabolites in 120 blood samples, and fipronil sulphone is detected in six samples with concentrations in the range of 12.1 ng/L-106 ng/L. Further, the well validation results and the application to analysis of fipronil and its metabolites in real samples demonstrate the applicability to toxico kinetic studies and clinical studies.

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