Simultaneous determination of parabens, alkylphenols, phenylphenols, bisphenol A and triclosan in human urine, blood and breast milk by continuous solid-phase extraction and gas chromatography-mass spectrometry

J Pharm Biomed Anal. 2016 Feb 5:119:16-26. doi: 10.1016/j.jpba.2015.11.024. Epub 2015 Nov 22.

Abstract

A highly sensitive gas chromatography-mass spectrometry (GC-MS) method for the determination of endocrine disrupting chemicals (EDCs) including parabens, alkylphenols, phenylphenols, bisphenol A and triclosan in human breast milk, blood and urine samples is proposed. Blood and milk require a pretreatment to remove proteins and other substances potentially interfering with the continuous solid-phase extraction (SPE) system used; on the other hand, urine samples can be directly introduced into the system after filtering. Analytes are retained on a LiChrolut EN column and derivatized by silylation following elution with acetonitrile. The resulting trimethylsilyl derivatives are determined by GC-MS. The proposed method exhibited good linearity (r(2)>0.995) for all target EDCs over the concentration range 0.7-10,000ng/l in urine, and 3.3-50,000ng/l in blood and milk. Also, it provided low limits of detection (0.2-1.8ng/l in urine, and 1.0-9.0ng/l in blood and milk), good precision (relative standard deviations less than 7%) and recoveries from 86 to 104%. A total of 24 human fluid samples were analyzed and most found to contain some target EDC at concentrations from 0.10 to 14μg/l.

Keywords: Blood and urine samples analysis; Continuous solid-phase extraction; Endocrine disrupting chemicals; Gas chromatography–mass spectrometry; Human breast milk.

MeSH terms

  • Benzhydryl Compounds* / blood
  • Benzhydryl Compounds* / urine
  • Endocrine Disruptors* / blood
  • Endocrine Disruptors* / urine
  • Gas Chromatography-Mass Spectrometry / instrumentation
  • Gas Chromatography-Mass Spectrometry / methods
  • Healthy Volunteers
  • Humans
  • In Vitro Techniques
  • Limit of Detection
  • Milk, Human / chemistry*
  • Parabens / analysis*
  • Parabens / pharmacokinetics
  • Phenols* / blood
  • Phenols* / urine
  • Reference Standards
  • Reproducibility of Results
  • Solid Phase Extraction / instrumentation
  • Solid Phase Extraction / methods
  • Triclosan* / blood
  • Triclosan* / urine

Substances

  • Benzhydryl Compounds
  • Endocrine Disruptors
  • Parabens
  • Phenols
  • Triclosan
  • bisphenol A