Development and Application of LC-MS/MS Method for the Detection of Naturally Occurring Thiouracil in Milk Samples

Woźniak, Barbara; Witek, Sebastian; Matraszek-Żuchowska, Iwona; Żmudzki, J.

doi:10.1007/s12161-014-9793-y

Cited by 7 publications

(7 citation statements)

References 21 publications

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“…The following method for the determination of goitrin and thiouracil in milk is based on the method described by Wozniak et al (2014) with some modifications. An aliquot of 80 mL of methanol was added to 20 mL of milk (previously defatted by centrifugation at 5000g for 10 min at 4°C) or 20 g of cheese (previously grated), and the mixture was placed in a thermostat at 60°C for 15 min.…”

Section: Analysis For Goitrin and Thiouracilmentioning

confidence: 99%

“…Successively, Církva and Šťastný (2013) and Wozniak et al (2014) applied, after adequate clean-up, 3IBBr derivatisation in milk samples. Derivatisation with 3IBBr is a nucleophilic substitution occurring on the sulfhydryl group; then, we wondered whether 3IBBr derivatisation was also suitable for goitrin.…”

Section: Derivatisation Stepmentioning

confidence: 99%

“…Derivatisation with 3IBBr is a nucleophilic substitution occurring on the sulfhydryl group; then, we wondered whether 3IBBr derivatisation was also suitable for goitrin. A standard solution of goitrin (4 mg L −1 ) was derivatised as reported by Wozniak et al (2014) and analysed by LC-MS/MS with infusion mode; positive ionisation was preferred and a good sensitivity of the derivatised-goitrin ion (246 m/z) was achieved. Satisfactory chromatographic resolution and separation between thiouracil, methyl-thiouracil and goitrin were obtained through gradient elution (retention time of 5.8, 6.8 and 9.3 min, respectively; Fig.…”

Section: Derivatisation Stepmentioning

confidence: 99%

“…However, a scarce stability of the derivatised-goitrin was observed, since the peak area decreased very fast, also when the injection was repeated after a few minutes; no decrease was observed for thiouracil. As reported by Wozniak et al (2014), a critical point for the preparation of the sample was the pH of the derivative mixture; before extracting with diethyl ether, the authors adjusted the pH to 4.5 in order to obtain a good recovery for all considered thyreostatic compounds, in particular for tapazole.…”

Section: Derivatisation Stepmentioning

confidence: 99%

“…In recent years, the development of adequate liquid chromatography-tandem mass spectrometry (LC-MS/MS) analytical methods for the determination of thyreostatic compounds has led to their determination at very low levels (about 1 μg L −1 ) (Pinel et al 2005;Lõhmus et al 2009;Vanden et al 2010;Církva and Šťastný 2013;Wozniak et al 2014); as a result, thiouracil was frequently detected in urine samples (Pinel et al 2006;Vanden et al 2011;Wozniak et al 2012;Wauters et al 2015) and also in cow milk (Wozniak et al 2014). To explain this widespread incidence, a natural origin due to ingestion of Brassicaceae-rich feed was suggested and definitely demonstrated (Kiebooms et al 2012).…”

Section: Introductionmentioning

confidence: 99%

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Trace Monitoring of Goitrin and Thiouracil in Milk and Cheese

et al. 2016

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Goitrin and thiouracil belong to the thyreostats, a group of compounds that inhibit the thyroid function; thyreostats can be divided into two main groups: naturally occurring compounds, mainly originated from glucosinolates, and xenobiotic (thyreostatic drugs) compounds, used as growth-promoting agents and performance enhancers in food-producing animals. Recently, thiouracil was detected at low levels in urine and cow milk samples and a natural origin due to ingestion of Brassicaceae-rich feed was demonstrated. Considering that the natural occurrence of both goitrin and thiouracil can be due to the same type of feeding for cattle, a liquid chromatography-tandem mass spectrometry (LC-MS/ MS) method for their simultaneous determination at trace levels in milk and cheese was developed. Then, a limited survey and a study to evaluate their carry-over from milk to curd and ripened cheese were carried out. For both compounds, the limit of detection (LOD) and the limit of quantification (LOQ) were 0.07 and 0.20 μg L −1 in milk, and 0.05 and 0.16 μg kg −1 in cheese; the average recovery values were above 80 %. In milk, their incidence was very high (≥95 %); the maximum value was 3.6 and 8.7 μg L −1 for goitrin and thiouracil, respectively. In cheese, only thiouracil was detected at levels close to those in milk. During cheese-making, both compounds remained mainly in the whey; during ageing, goitrin content decreased quickly and it was never detected after 2 months of ripening.

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Section: Analysis For Goitrin and Thiouracilmentioning

confidence: 99%

Section: Derivatisation Stepmentioning

confidence: 99%

Section: Derivatisation Stepmentioning

confidence: 99%

Section: Derivatisation Stepmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

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Trace Monitoring of Goitrin and Thiouracil in Milk and Cheese

et al. 2016

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Hormones and &;#x003B2;&;#x02010;Agonists

Ginkel

Bovee

Blokland

et al. 2016

Chemical Analysis of Non&;#x02010;antimicrobial Veterinary Drug Residues in Food

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Analysis of thyreostats in bovine feces using ultra high performance liquid chromatography with tandem mass spectrometry

Witek

Woźniak

Matraszek-Żuchowska

et al. 2018

J of Separation Science

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A method based on ultra-high performance liquid chromatography was developed and validated to detect six thyreostatic compounds: tapazole, thiouracil, methylthiouracil, dimethylthiouracil, propylthiouracil, and phenylthiouracil in faeces of bovine. Thyreostats were extracted from the matrix with a mixture of methanol and buffer (pH = 8). Next step was derivatization of analytes with 3-iodobenzylbromide. The liquid chromatographic separation of derivatives was obtained on a SB-C18 column (50 × 2.1 mm; 1.8 μm, Agilent) with gradient elution using a mobile phase consisting of acetonitrile/0.1% acetic acid within 7.5 min. The analysis was performed on a Shimadzu NEXERA X2 ultra-high performance liquid chromatograph with triple quadrupole MS 8050 instrument operating in positive electrospray ionization mode. Depending on the target compound, two or three diagnostic signals (selected reaction monitoring transitions) were monitored. The procedure was validated according to the Commission Decision 2002/657/EC. Recovery and repeatability met the performance criteria specified by this document for banned compounds. The recovery ranged from 97.5 to 110.5%, and repeatability did not exceed 14.1%. Decision limits and detection capabilities were below 10 μg/kg. The highest decision limits and detection capabilities concentrations were observed for phenylthiouracil of 3.48 and 6.96 μg/kg, respectively.

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Development and Application of LC-MS/MS Method for the Detection of Naturally Occurring Thiouracil in Milk Samples

Cited by 7 publications

References 21 publications

Trace Monitoring of Goitrin and Thiouracil in Milk and Cheese

Trace Monitoring of Goitrin and Thiouracil in Milk and Cheese

Hormones and &;#x003B2;&;#x02010;Agonists

Analysis of thyreostats in bovine feces using ultra high performance liquid chromatography with tandem mass spectrometry

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