Determination of aflatoxins in food samples by automated on-line in-tube solid-phase microextraction coupled with liquid chromatography-mass spectrometry

Y. Nonaka, K. Saito, N. Hanioka, S. Narimatsu, H. Kataoka

Research output: Contribution to journalArticle

93 Citations (Scopus)

Abstract

A simple and sensitive automated method for determination of aflatoxins (B1, B2, G1, and G2) in nuts, cereals, dried fruits, and spices was developed consisting of in-tube solid-phase microextraction (SPME) coupled with liquid chromatography-mass spectrometry (LC-MS). Aflatoxins were separated within 8 min by high-performance liquid chromatography using a Zorbax Eclipse XDB-C8 column with methanol/acetonitrile (60/40, v/v): 5 mM ammonium formate (45:55) as the mobile phase. Electrospray ionization conditions in the positive ion mode were optimized for MS detection of aflatoxins. The pseudo-molecular ions [M+H]+ were used to detect aflatoxins in selected ion monitoring (SIM) mode. The optimum in-tube SPME conditions were 25 draw/eject cycles of 40 μL of sample using a Supel-Q PLOT capillary column as an extraction device. The extracted aflatoxins were readily desorbed from the capillary by passage of the mobile phase, and no carryover was observed. Using the in-tube SPME LC-MS with SIM method, good linearity of the calibration curve (r > 0.9994) was obtained in the concentration range of 0.05-2.0 ng/mL using aflatoxin M1 as an internal standard, and the detection limits (S/N = 3) of aflatoxins were 2.1-2.8 pg/mL. The in-tube SPME method showed >23-fold higher sensitivity than the direct injection method (10 μL injection volume). The within-day and between-day precision (relative standard deviations) at the concentration of 1 ng/mL aflatoxin mixture were below 3.3% and 7.7% (n = 5), respectively. This method was applied successfully to analysis of food samples without interference peaks. The recoveries of aflatoxins spiked into nuts and cereals were >80%, and the relative standard deviations were

Original languageEnglish
Pages (from-to)4416-4422
Number of pages7
JournalJournal of Chromatography A
Volume1216
Issue number20
DOIs
Publication statusPublished - May 15 2009

Fingerprint

Solid Phase Microextraction
Aflatoxins
Liquid chromatography
Liquid Chromatography
Mass spectrometry
Mass Spectrometry
Food
Ions
formic acid
Nuts
Aflatoxin M1
Food Analysis
Electrospray ionization
Spices
Injections
Aflatoxin B1
Monitoring
Direct injection
High performance liquid chromatography
Fruits

Keywords

  • Aflatoxin
  • Automated sample preparation
  • Food samples
  • In-tube solid-phase microextraction
  • Liquid chromatography-mass spectrometry
  • Mycotoxin

ASJC Scopus subject areas

  • Analytical Chemistry
  • Organic Chemistry
  • Biochemistry

Cite this

Determination of aflatoxins in food samples by automated on-line in-tube solid-phase microextraction coupled with liquid chromatography-mass spectrometry. / Nonaka, Y.; Saito, K.; Hanioka, N.; Narimatsu, S.; Kataoka, H.

In: Journal of Chromatography A, Vol. 1216, No. 20, 15.05.2009, p. 4416-4422.

Research output: Contribution to journalArticle

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