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Determination of sterigmatocystin in feed by LC-MS/MS.

Food additives & contaminants. Part A, Chemistry, analysis, control, exposure & risk assessment (2015-10-17)
Alberto Biancardi, Chiara Dall'Asta
ZUSAMMENFASSUNG

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.

MATERIALIEN
Produktnummer
Marke
Produktbeschreibung

Sigma-Aldrich
Ameisensäure, reagent grade, ≥95%
Sigma-Aldrich
Ameisensäure, ACS reagent, ≥96%
Sigma-Aldrich
Ameisensäure, puriss. p.a., ACS reagent, reag. Ph. Eur., ≥98%
Sigma-Aldrich
Acetonitril, ACS reagent, ≥99.5%
Sigma-Aldrich
Acetonitril, anhydrous, 99.8%
Sigma-Aldrich
Ameisensäure, puriss., meets analytical specifications of DAC, FCC, 98.0-100%
Sigma-Aldrich
Ameisensäure, ACS reagent, ≥88%
Supelco
SPME-Faseranordnung Divinylbenzol/Carboxen/Polydimethylsiloxan (DVB/CAR/PDMS), needle size 24 ga, StableFlex
Supelco
SPME-Faseranordnung Divinylbenzol/Carboxen/Polydimethylsiloxan (DVB/CAR/PDMS), needle size 24 ga, for use with manual holder
Supelco
SPME-Faseranordnung Divinylbenzol/Carboxen/Polydimethylsiloxan (DVB/CAR/PDMS), needle size 23 ga, StableFlex, for use with autosampler
Supelco
SPME-Faseranordnung Divinylbenzol/Carboxen/Polydimethylsiloxan (DVB/CAR/PDMS), needle size 23 ga, StableFlex, for use with manual holder or autosampler, fiber L 2 cm
Sigma-Aldrich
Siliziumtetrachlorid, 99%
Supelco
SPME-Faseranordnung Divinylbenzol/Carboxen/Polydimethylsiloxan (DVB/CAR/PDMS), needle size 24 ga, StableFlex, for use with autosampler
Sigma-Aldrich
Acetonitril, biotech. grade, ≥99.93%
Supelco
SPME-Faseranordnung Polydimethylsiloxan (PDMS), df 100 μm(PDMS, needle size 24 ga, for use with manual holder
Supelco
SPME-Faseranordnung Polydimethylsiloxan (PDMS), df 100 μm(PDMS, for use with autosampler, needle size 23 ga
Supelco
SPME-Faseranordnung Polydimethylsiloxan (PDMS), df 100 μm(PDMS, for use with autosampler, needle size 24 ga
Supelco
SPME-Faseranordnung Carboxen/Polydimethylsiloxan (CAR/PDMS), df 75 μm(CAR/PDMS, for use with manual holder, needle size 24 ga
Sigma-Aldrich
Ameisensäure, ≥95%, FCC, FG
Supelco
SPME-Faseranordnung Polydimethylsiloxan/Divinylbenzen (PDMS/DVB), df 65 μm(PDMS/DVB, needle size 24 ga, StableFlex, for use with autosampler
Sigma-Aldrich
Acetonitril, ReagentPlus®, 99%
Supelco
SPME-Faseranordnung Carboxen/Polydimethylsiloxan (CAR/PDMS), df 85 μm(CAR/PDMS, needle size 23 ga, StableFlex, for use with autosampler
Supelco
SPME-Faseranordnung Polydimethylsiloxan/Divinylbenzen (PDMS/DVB), df 65 μm(PDMS/DVB, needle size 24 ga, for use with manual holder
Supelco
SPME-Faseranordnung Carboxen/Polydimethylsiloxan (CAR/PDMS), df 75 μm(CAR/PDMS, needle size 24 ga, for use with autosampler
Supelco
SPME-Faseranordnung Carboxen/Polydimethylsiloxan (CAR/PDMS), df 85 μm(CAR/PDMS, needle size 24 ga, StableFlex, for use with autosampler
Supelco
SPME-Faseranordnung Polyacrylat (PA), df 85 μm(PA, for use with autosampler, needle size 23 ga
Sigma-Aldrich
Acetonitril, electronic grade, 99.999% trace metals basis
Sigma-Aldrich
Acetonitril, suitable for DNA synthesis, ≥99.9% (GC)
Supelco
SPME-Faseranordnung Polydimethylsiloxan/Divinylbenzen (PDMS/DVB), df 65 μm(PDMS/DVB, needle size 23 ga, PDMS/DVB StableFlex, for use with autosampler
Supelco
SPME-Faseranordnung Polyacrylat (PA), df 85 μm(PA, for use with autosampler, needle size 24 ga