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Determination of sterigmatocystin in grain using gas chromatography-mass spectrometry with an on-column injector

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Abstract

Sterigmatocystin (STC) is a mycotoxin produced by several species of Aspergillus and other fungi. STC is a precursor of the carcinogen aflatoxin B1 and exerts carcinogenic, teratogenic, and mutagenic effects. A reliable GC-MS-based analytical method using on-column injection was developed and validated to determine STC content in grain. In this method, STC was extracted with acetonitrile (84 %), and the filtered extract was diluted with phosphate buffer before immunoaffinity column (IAC) cleanup. After elution and N2 evaporation, the sample containing STC was dissolved in acetone and injected into the GC-MS system without derivatization. Separation of STC was carried out by a capillary column (0.25 mm i.d. × 30 m, 0.25 μm) with a deactivated pre-column (0.53 mm i.d. × 0.6 m). The matrix effect was investigated in maize, wheat, and rice, and an insignificant matrix effect was observed after IAC cleanup. The calibration curve was linear in the range of 20–300 pg (equivalent to 8–120 μg/kg in grain) with a coefficient of determination (R 2) of 0.999, and the relative standard deviation of repeatability (RSDr) was less than 10 %. The limit of detection (LOD) of the method was 6 pg (equivalent to 2.4 μg/kg in grain), and the limit of quantification (LOQ) was 20 pg (equivalent to 8 μg/kg). The method described in this report is sensitive, reliable, and can be used to monitor STC contamination in grain.

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Abbreviations

GC-MS:

Gas chromatography mass spectrometry

IAC:

Immunoaffinity column

LC-MS:

Liquid chromatography mass spectrometry

LOD:

Limit of detection

LOQ:

Limit of quantification

RSD:

Relative standard deviation

S/N:

Signal-to-noise ratio

STC:

Sterigmatocystin

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I have full control of all primary data and there is no conflict of interest.

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Authors and Affiliations

  1. Faculty of Agriculture, Shinshu University, 8304 Minami-minowa-Mura, Kamiina, Nagano, 399-4598, Japan

    Md. Z. Hossain & T. Goto

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  1. Md. Z. Hossain
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  2. T. Goto
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Correspondence to T. Goto.

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Hossain, M.Z., Goto, T. Determination of sterigmatocystin in grain using gas chromatography-mass spectrometry with an on-column injector. Mycotoxin Res 31, 17–22 (2015). https://doi.org/10.1007/s12550-014-0214-2

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  • DOI: https://doi.org/10.1007/s12550-014-0214-2

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