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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
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.

MATERIALS
Product Number
Brand
Product Description

Sigma-Aldrich
Silicon tetrachloride solution, 1.0 M in methylene chloride
Sigma-Aldrich
Acetonitrile solution, contains 0.1 % (v/v) trifluoroacetic acid, suitable for HPLC
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Acetonitrile solution, contains 0.05 % (v/v) trifluoroacetic acid
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Acetonitrile solution, contains 0.05 % (w/v) ammonium formate, 5 % (v/v) water, 0.1 % (v/v) formic acid, suitable for HPLC
Sigma-Aldrich
Acetonitrile solution, contains 0.1 % (v/v) formic acid, suitable for HPLC
Sigma-Aldrich
Acetonitrile solution, contains 10.0% acetone, 0.05% formic acid, 40.0% 2-propanol
Supelco
SPME fiber assembly Polydimethylsiloxane (PDMS), df 100 μm(PDMS, for use with autosampler, needle size 23 ga
Supelco
SPME Fiber Assembly, matrix active group 50/30µm DVB/CAR/PDMS, StableFlex fiber, manual holder, needle size 24 ga
Supelco
SPME Fiber Assembly, 50/30µm DVB/CAR/PDMS, StableFlex (1 cm), needle size 23 ga, Autosampler, pk of 3, plain gray hub
Supelco
SPME fiber assembly Polydimethylsiloxane (PDMS), df 100 μm(PDMS, for use with autosampler, needle size 24 ga
Supelco
SPME Fiber Assembly Polydimethylsiloxane/Divinylbenzene (PDMS/DVB), df 65 μm(PDMS/DVB, for use with autosampler, needle size 23 ga
Supelco
SPME Fiber Assembly Polydimethylsiloxane/Divinylbenzene (PDMS/DVB), fused silica fiber, df 65 μm(PDMS/DVB, for use with manual holder, needle size 23 ga
Supelco
SPME fiber assembly polyacrylate (PA), df 85 μm(PA, for use with autosampler, needle size 23 ga
Supelco
SPME fiber assembly Carboxen/Polydimethylsiloxane (CAR/PDMS), df 75 μm(CAR/PDMS, needle size 23 ga, for use with autosampler
Supelco
SPME Fiber Assembly Polydimethylsiloxane/Divinylbenzene (PDMS/DVB), df 65 μm(PDMS/DVB, needle size 24 ga, for use with manual holder
Supelco
SPME fiber assembly Polydimethylsiloxane (PDMS), metal alloy fiber, df 100 μm(PDMS, needle size 23 ga, for use with autosampler
Supelco
SPME fiber assembly polyacrylate (PA), df 85 μm(PA, for use with manual holder, needle size 24 ga
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SPME Portable Field Sampler, coating PDMS
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SPME fiber assembly Polydimethylsiloxane (PDMS), df 7 μm(PDMS, needle size 24 ga, for use with manual holder
Supelco
SPME fiber assembly Carboxen/Polydimethylsiloxane (CAR/PDMS), df 85 μm(CAR/PDMS, needle size 23 ga, StableFlex, for use with autosampler
Supelco
SPME-OC Fiber Assembly, Polydimethylsiloxane/Divinylbenzene (PDMS/DVB), df 75 μm(Coating thickness includes 65 μm coating + 10 μm OC (overcoating), needle size 23 ga, pkg of 3 ea, fiber L 1 cm
Supelco
SPME fiber assembly Polydimethylsiloxane (PDMS), df 7 μm(PDMS, needle size 23 ga, for use with autosampler
Supelco
SPME Fiber Assembly, for use with autosampler, matrix active group 50/30µm DVB/CAR/PDMS, needle size 23 ga, metal alloy fiber, fiber L 2 cm
Supelco
SPME fiber assembly Carboxen/Polydimethylsiloxane (CAR/PDMS), df 75 μm(CAR/PDMS, needle size 24 ga, for use with autosampler
Supelco
SPME Fiber Assembly Polydimethylsiloxane/Divinylbenzene (PDMS/DVB), df 65 μm(PDMS/DVB, needle size 24 ga, StableFlex, for use with manual holder
Supelco
SPME Portable Field Sampler, coating PDMS/DVB
Supelco
SPME fiber assembly Carboxen/Polydimethylsiloxane (CAR/PDMS), df 85 μm(CAR/PDMS, for use with autosampler, needle size 23 ga, metal alloy fiber
Supelco
SPME fiber assembly polyacrylate (PA), df 85 μm(PA, for use with autosampler, needle size 24 ga
Supelco
SPME fiber assembly Polydimethylsiloxane (PDMS), df 100 μm(PDMS, for use with manual holder, needle size 23 ga
Supelco
SPME Fiber Assembly Polydimethylsiloxane/Divinylbenzene (PDMS/DVB), df 65 μm(PDMS/DVB, needle size 24 ga, StableFlex, for use with autosampler