Quantitative reversed-phase HPLC analysis of dicumarol in sweetclover hay and silage samples

Muir, Alister D.; Goplen, B. P.

doi:10.1021/jf00017a022

Cited by 7 publications

(2 citation statements)

References 12 publications

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“…Table 1 summarizes some studies using HPLC for the determination of investigated coumarins in different matrices. Techniques, such as ultrasonic liquid extraction for plant and cosmetics samples (Muir et al 1992;Ikeda et al 2009;Xi et al 2010) or accelerated solvent extraction for food sample (Vieriková et al 2009) were applied for sample pretreatment. The aim of the present work was to develop a rapid and sensitive HPLC method for simultaneous determination dicoumarol, coumarin, and 4-hydroxycoumarin in sweet clover herb and hay.…”

Section: Introductionmentioning

confidence: 99%

HPLC separation and determination of dicoumarol and other simple coumarins in sweet clover

Hroboňová¹,

Sádecká²,

Čiẑmárik³

2018

Nova Biotechnologica Et Chimica

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Dicoumarol is a mycotoxin, that acts as a blood anticoagulant, is formed during the microbial action of molds and fungi in spoiled hay or silage containing high-coumarin plant. A HPLC-DAD method for determination of coumarins, including dicoumarol, coumarin, and 4-hydroxycoumarin was developed. Methanol and acetic acid were used as mobile phase with gradient elution. The simultaneous separation was performed using C18 type of stationary phase. The recoveries were 88.6 – 92.6 %, 91.8 – 95.0 %, and 89.7 – 94.1 % (evaluated for three concentration levels) for dicoumarol, coumarin, and 4-hydroxycoumarin respectively. The parameters of system suitability (repeatability of retention times and peak areas) were determined for evaluation of the method. The method showed a good linearity in the concentration range 0.7 – 100 μg.mL−1for dicoumarol, 0.05 – 100 μg.mL−1for coumarin and 4-hydroxycoumarin with correlation coefficients higher than 0.9885. Extracts of sweet clover herb, hay, and spoiled hay were subjected to HPLC-DAD analysis. The most abundant compound in sweet clover herb and hay extracts was coumarin. In spoiled sweet clover hay extract the 4-hydroxycoumarin was detected in addition. The formation of 4-hydroxycoumarin was also observed in the synchronous fluorescence spectra recorded at the wavelength difference of 90 nm (difference between emission and excitation wavelength).

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Section: Introductionmentioning

confidence: 99%

HPLC separation and determination of dicoumarol and other simple coumarins in sweet clover

Hroboňová¹,

Sádecká²,

Čiẑmárik³

2018

Nova Biotechnologica Et Chimica

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“…properties of 3 are reported and compared to those of 2, as well as to two other synthetic anils 4 and 5• Dicoumarol [1] is an anticoagulant often present in moldy clover, It is a cause of sickness and death in cattle (1,2), which has resulted in development of a variety of techniques for its quantitative measurement in clover (3,4). Its structure was determined by Stahmanetal. in 1941 (5), partly by means of its reaction with aniline.…”

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confidence: 99%