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Merck

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
要旨

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.

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製品内容

Sigma-Aldrich
ギ酸, reagent grade, ≥95%
Sigma-Aldrich
ギ酸, ACS reagent, ≥96%
Sigma-Aldrich
ギ酸, puriss. p.a., ACS reagent, reag. Ph. Eur., ≥98%
Sigma-Aldrich
アセトニトリル, ACS reagent, ≥99.5%
Sigma-Aldrich
アセトニトリル, anhydrous, 99.8%
Sigma-Aldrich
ギ酸, puriss., meets analytical specifications of DAC, FCC, 98.0-100%
Sigma-Aldrich
ギ酸, ACS reagent, ≥88%
Supelco
SPMEファイバーアセンブリー ジビニルベンゼン/カルボキセン/ポリジメチルシロキサン (DVB/CAR/PDMS), needle size 24 ga, StableFlex
Supelco
SPMEファイバーアセンブリー ジビニルベンゼン/カルボキセン/ポリジメチルシロキサン (DVB/CAR/PDMS), needle size 24 ga, for use with manual holder
Supelco
SPMEファイバーアセンブリー ジビニルベンゼン/カルボキセン/ポリジメチルシロキサン (DVB/CAR/PDMS), needle size 23 ga, StableFlex, for use with autosampler
Supelco
SPMEファイバーアセンブリー ジビニルベンゼン/カルボキセン/ポリジメチルシロキサン (DVB/CAR/PDMS), needle size 23 ga, StableFlex, for use with manual holder or autosampler, fiber L 2 cm
Sigma-Aldrich
四塩化ケイ素, 99%
Supelco
SPMEファイバーアセンブリー ジビニルベンゼン/カルボキセン/ポリジメチルシロキサン (DVB/CAR/PDMS), needle size 24 ga, StableFlex, for use with autosampler
Sigma-Aldrich
アセトニトリル, biotech. grade, ≥99.93%
Supelco
SPMEファイバーアセンブリー ポリジメチルシロキサン(PDMS), df 100 μm(PDMS, needle size 24 ga, for use with manual holder
Supelco
SPMEファイバーアセンブリー ポリジメチルシロキサン(PDMS), df 100 μm(PDMS, for use with autosampler, needle size 23 ga
Supelco
SPMEファイバーアセンブリー ポリジメチルシロキサン(PDMS), df 100 μm(PDMS, for use with autosampler, needle size 24 ga
Supelco
SPMEファイバー・アセンブリカルボキセン/ポリジメチルシロキサン(CAR/PDMS), df 75 μm(CAR/PDMS, for use with manual holder, needle size 24 ga
Sigma-Aldrich
ギ酸, ≥95%, FCC, FG
Supelco
SPMEファイバー・ポリジメチルシロキサン/ジビニルベンゼン(PDMS/DVB), df 65 μm(PDMS/DVB, needle size 24 ga, StableFlex, for use with autosampler
Sigma-Aldrich
アセトニトリル, ReagentPlus®, 99%
Supelco
SPMEファイバー・アセンブリカルボキセン/ポリジメチルシロキサン(CAR/PDMS), df 85 μm(CAR/PDMS, needle size 23 ga, StableFlex, for use with autosampler
Supelco
SPMEファイバー・ポリジメチルシロキサン/ジビニルベンゼン(PDMS/DVB), df 65 μm(PDMS/DVB, needle size 24 ga, for use with manual holder
Supelco
SPMEファイバー・アセンブリカルボキセン/ポリジメチルシロキサン(CAR/PDMS), df 75 μm(CAR/PDMS, needle size 24 ga, for use with autosampler
Supelco
SPMEファイバー・アセンブリカルボキセン/ポリジメチルシロキサン(CAR/PDMS), df 85 μm(CAR/PDMS, needle size 24 ga, StableFlex, for use with autosampler
Supelco
SPMEファイバーアセンブリー ポリアクリラート (PA), df 85 μm(PA, for use with autosampler, needle size 23 ga
Sigma-Aldrich
アセトニトリル, electronic grade, 99.999% trace metals basis
Sigma-Aldrich
アセトニトリル, suitable for DNA synthesis, ≥99.9% (GC)
Supelco
SPMEファイバー・ポリジメチルシロキサン/ジビニルベンゼン(PDMS/DVB), df 65 μm(PDMS/DVB, needle size 23 ga, PDMS/DVB StableFlex, for use with autosampler
Supelco
SPMEファイバーアセンブリー ポリアクリラート (PA), df 85 μm(PA, for use with autosampler, needle size 24 ga