Method for the determination of thyreostats in milk samples using LC-MS/MS

Církva, A.; Šťastný, Kamil

doi:10.1080/19440049.2013.787651

Cited by 17 publications

(8 citation statements)

References 3 publications

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“…For extraction of thyreostats from matrix, polar solvents such as acetonitrile (9), methanol (12), and ethyl acetate (8) are usually used. The extracts are then cleaned-up by liquid-liquid extraction (LLE) with diethyl (23) ether or dichloromethane (20) or combination of LLE with solid phase extraction (SPE), mainly with silica cartridges, but also with C18 columns (1,11,25).…”

Section: Introductionmentioning

confidence: 99%

Determination of the Thyreostats in Animal Feeding Stuffs Using Liquid Chromatography-Tandem Mass Spectrometry

Woźniak

Witek

Matraszek-Żuchowska

et al. 2014

Bulletin of the Veterinary Institute in Pulawy

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A rapid liquid chromatography tandem mass spectrometry method was developed and validated to detect and confirm five thyreostatic drugs: tapazole, thiouracil, methylthiouracil, propylthiouracil, and phenylthiouracil in animal feeding stuff samples. Thyreostats were extracted from feed with methanol, and then degreasing of the extract with petroleum ether was performed, followed by the derivatisation of the compounds with 3-iodobenzylbromide in basic medium (pH 8.0). The derivatives were extracted with diethyl ether and analysed by gradient elution on a Poroshell 120-EC C18 column with triple quadrupole MS detection with turbo spray source in positive ionisation mode. The method was validated in accordance with the Commission Decision 2002/657/EC. For validation level of 10 μg kg -1 , the recovery ranged from 82% to 97.5% for all examined compounds. The repeatability and reproducibility did not exceed the limit of 20% for all analytes. The linearity was good for all thyreostats in the whole range of tested concentrations, as proved by the correlation coefficients greater than 0.99. The decision limits (CC) ranged from 1.63 μg kg -1 to 3.95 μg kg -1 , whereas the detection capabilities (CC) ranged from 2.74 μg kg -1 to 6.73 μg kg -1 . The developed analysis is sensitive and robust, and therefore useful for quantification and confirmation of thyreostats in residue control programme.

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Section: Introductionmentioning

confidence: 99%

Determination of the Thyreostats in Animal Feeding Stuffs Using Liquid Chromatography-Tandem Mass Spectrometry

Woźniak

Witek

Matraszek-Żuchowska

et al. 2014

Bulletin of the Veterinary Institute in Pulawy

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“…We tested different pH values (from 2.5 to 8) and we found that a good stability for both goitrin and thiouracil was obtained when the pH value was not modified (pH = 8), as reported by Církva and Šťastný (2013). However, it is preferable to perform the instrumental determination on the same day of the derivatisation step, since a low decrease (about 10 %) of the peak area of goitrin occurs after 5-6 h.…”

Section: Derivatisation Stepmentioning

confidence: 48%

“…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%

“…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: 97%

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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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“…By referring to the milk, it must be stated that it is the important component of the human diet. However, accumulation of some drug residues in milk reducing its quality may pose a risk to the human population of different groups especially for infants and children (Cirkva and Št'astnỳ 2013;Courant et al 2008;Gamba et al 2009). Contaminated milk from the epidemiological point of view can be the cause of allergic reactions, hormone-dependent diseases and potential risk factor for cancer in humans (Azzouz et al 2011;Ganmaa and Sato 2005;Khaniki 2007).…”

Section: Introductionmentioning

confidence: 99%

Determination of Hormones Residues in Milk by Gas Chromatography-Mass Spectrometry

2016

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T h e a rti c le p re s en t s th e u se of ga s chromatography-mass spectrometry (GC-MS) technique in a method for the determination of 18 anabolic hormones from synthetic stilbenes, steroids and resorcylic acid lactones (RALs) groups in raw milk and milk powder. Sample preparation consisted of liquid-liquid extraction with diethyl ether and purification by solid phase extraction (SPE). Prior to instrumental analysis, the reaction of derivatisation with the heptafluorobutyric anhydride or N-methyl-N-trimethylsilyltrifluoroacetamide was performed. Method validation was carried out according to the required performance criteria of the Commission Decision 2002/657/EC. The apparent recovery of all analytes at 1 μg L −1 (kg −1 ) level was ranged between 70.4 and 119.4 % with the coefficients of variation values less than 30 %. The decision limits (CCα) and the detection capabilities (CCβ) were in the range of from 0.11 to 0.44 μg L −1 (kg −1 ) and from 0.19 to 0.75 μg L −1 (kg −1 ), respectively. The procedure has been accredited and successfully applied as a screening method for the presence of hormone residues in the study of commercial samples of milk.

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Method for the determination of thyreostats in milk samples using LC-MS/MS

Cited by 17 publications

References 3 publications

Determination of the Thyreostats in Animal Feeding Stuffs Using Liquid Chromatography-Tandem Mass Spectrometry

Determination of the Thyreostats in Animal Feeding Stuffs Using Liquid Chromatography-Tandem Mass Spectrometry

Trace Monitoring of Goitrin and Thiouracil in Milk and Cheese

Determination of Hormones Residues in Milk by Gas Chromatography-Mass Spectrometry

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