title: Determination of sterigmatocystin in feed by LC-MS/MS.
abstract: An LC-MS/MS method is proposed for the analysis of sterigmatocystin in cereals and feed. The method is based on a solid-liquid extraction and a dilute-and-shoot approach. Accuracy and precision were established at the LOQ (1 μg kg(-1)); the mean overall recovery (n = 6) was 98%, with a confidence interval of 3.8% and a CV% of 3.7%. Accuracy and precision were also assessed at three other concentration levels (2.03, 5.07 and 10.14 μg kg(-1); six replicates per level). The mean overall recovery (n = 24, LOQ included) was 99% with a confidence interval of 0.8% and a CV% of 1.9%. The method was then applied to 14 naturally incurred feed samples. Aflatoxin B1 was present in the range 28.7-240.1 µg kg(-1), while lower concentrations of sterigmatocystin were found (0.7-2.2 µg kg(-1)). This method may represent a valuable choice, ensuring a high level of accuracy and precision, as well as high-throughput performance. Therefore, it meets the recent EFSA opinion recommendation in terms of availability of fast and sensitive methods (recommended LOQ = 1.5 μg kg(-1)) in order to increase data collection to allow for the assessment of dietary exposure.
authors.affiliation: a Istituto Zooprofilattico Sperimentale della Lombardia e dell'Emilia-Romagna , Brescia , Italy.
authors.forename: Alberto
authors.initials: A
authors.lastname: Biancardi
authors.affiliation: b Dipartimento di Scienze degli Alimenti , Università degli Studi di Parma , Parma , Italy.
authors.forename: Chiara
authors.initials: C
authors.lastname: Dall'Asta
mesh_terms: D016604:Aflatoxin B1 / Q000096:biosynthesis / Q000302:isolation & purification*; D000821:Animal Feed / Q000032:analysis*; D000818:Animals; D001230:Aspergillus / Q000472:pathogenicity / Q000502:physiology; D002853:Chromatography, Liquid; D002523:Edible Grain / Q000737:chemistry* / Q000378:metabolism / Q000382:microbiology; D005506:Food Contamination / Q000032:analysis; D057230:Limit of Detection; D009183:Mycotoxins / Q000096:biosynthesis / Q000302:isolation & purification*; D010935:Plant Diseases / Q000382:microbiology; D015203:Reproducibility of Results; D052617:Solid Phase Microextraction; D013241:Sterigmatocystin / Q000096:biosynthesis / Q000302:isolation & purification*; D053719:Tandem Mass Spectrometry
chemical_list: D009183:Mycotoxins; D013241:Sterigmatocystin; D016604:Aflatoxin B1
keywords: feed; in-house validation; mass spectrometry; mycotoxins