Determination of polycyclic aromatic hydrocarbons in food samples by automated on-line in-tube solid-phase microextraction coupled with high-performance liquid chromatography-fluorescence detection

A. Ishizaki, K. Saito, N. Hanioka, S. Narimatsu, H. Kataoka

Research output: Contribution to journalArticle

129 Citations (Scopus)

Abstract

A simple and sensitive automated method, consisting of in-tube solid-phase microextraction (SPME) coupled with high-performance liquid chromatography-fluorescence detection (HPLC-FLD), was developed for the determination of 15 polycyclic aromatic hydrocarbons (PAHs) in food samples. PAHs were separated within 15. min by HPLC using a Zorbax Eclipse PAH column with a water/acetonitrile gradient elution program as the mobile phase. The optimum in-tube SPME conditions were 20. draw/eject cycles of 40 μL of sample using a CP-Sil 19CB capillary column as an extraction device. Low- and high-molecular weight PAHs were extracted effectively onto the capillary coating from 5% and 30% methanol solutions, respectively. The extracted PAHs were readily desorbed from the capillary by passage of the mobile phase, and no carryover was observed. Using the in-tube SPME HPLC-FLD method, good linearity of the calibration curve (r> 0.9972) was obtained in the concentration range of 0.05-2.0. ng/mL, and the detection limits (S/. N= 3) of PAHs were 0.32-4.63. pg/mL. The in-tube SPME method showed 18-47 fold higher sensitivity than the direct injection method. The intra-day and inter-day precision (relative standard deviations) for a 1. ng/mL PAH mixture were below 5.1% and 7.6% (n= 5), respectively. This method was applied successfully to the analysis of tea products and dried food samples without interference peaks, and the recoveries of PAHs spiked into the tea samples were >70%. Low-molecular weight PAHs such as naphthalene and pyrene were detected in many foods, and carcinogenic benzo[. a]pyrene, at relatively high concentrations, was also detected in some black tea samples. This method was also utilized to assess the release of PAHs from tea leaves into the liquor.

Original languageEnglish
Pages (from-to)5555-5563
Number of pages9
JournalJournal of Chromatography A
Volume1217
Issue number35
DOIs
Publication statusPublished - Aug 1 2010

Keywords

  • Automated sample preparation
  • Food samples
  • High-performance liquid chromatography-fluorescence detection
  • In-tube solid-phase microextraction
  • Polycyclic aromatic hydrocarbons

ASJC Scopus subject areas

  • Analytical Chemistry
  • Biochemistry
  • Organic Chemistry

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