Rapid and sensitive determination of nine bisphenol analogues, three amphenicol antibiotics, and six phthalate metabolites in human urine samples using UHPLC-MS/MS
Bisphenol analogues, amphenicol antibiotics, and phthalate have widely aroused public concerns due to their adverse effects on human health. In this study, a rapid and sensitive method for determination of nine bisphenol analogues, three amphenicol antibiotics, and six phthalate metabolites in the urine based on ultra-high-performance liquid chromatography coupled with triple quadrupole tandem mass spectrometry was developed and validated. The sample pretreatment condition on the base of mixed-mode anion-exchange (Oasis MAX) SPE was optimized to separate bisphenol analogues and amphenicol antibiotics from phthalate metabolites: the former were detected with a mobile phase of 0.1% ammonium water solution/methanol containing 0.1% ammonium water solution in negative mode, whereas the latter were determined with a mobile phase of 0.1% acetic acid solution/acetonitrile containing 0.1% acetic acid in negative mode. The limits of detection were less than 0.26 ng/mL for bisphenol analogues, 0.12 ng/mL for amphenicol antibiotics, and 0.14 ng/mL for phathalate metabolites. The recoveries of all target analytes in three fortification levels ranged from 72.02 to 117.64% with the relative standard deviations of no larger than 14.51%. The matrix effect was adjusted by isotopically labeled internal standards. This proposed method was successfully applied to analyze 40 actual urines and 13 out of 18 studied compounds were detected.
KeywordsBisphenol analogues Amphenicol antibiotics Phthalate metabolites Mixed-mode solid-phase extraction Ultra performance liquid chromatography-tandem mass spectrometry Urine sample
This study was supported by the National Natural Science Foundation of China (No. 81373089), Scientific Research Foundation of Shanghai Municipal Commission of Health and Family Planning (No. 201540053), the National Science Fund for Distinguished Young Scholars of China (No. 81325017), and the Key Program of the National Natural Science Foundation of China (No. 81630088).
Compliance with ethical standards
The study was approved by the Institutional Review Board (IRB) of the School of Public Health, Fudan University (ref: IRB#2013-03-0437). Written informed consent was obtained from all participants and the parents/LAR of the participants.
Conflict of interest
The authors declare that they have no conflict of interest.
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