Development and application of salting-out assisted liquid/liquid extraction for multi-mycotoxin biomarkers analysis in pig urine with high performance liquid chromatography/tandem mass spectrometry

Song, Suquan; Ediage, Emmanuel Njumbe; Wu, Aibo; Saeger, Sarah De

doi:10.1016/j.chroma.2012.10.071

Cited by 104 publications

(70 citation statements)

References 31 publications

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“…2 Effects of different a loading solvents and b flow rates on IAC efficiency 0.30-25, 0.30-25, and 1.2-40 μg kg −1 , respectively. These linear ranges were larger than those of previous studies on multiple mycotoxins in body fluids (urine and plasma) [22].…”

Section: Matrix-matched Calibration Curves and Linear Rangecontrasting

confidence: 61%

Development of a multiple immunoaffinity column for simultaneous determination of multiple mycotoxins in feeds using UPLC–MS/MS

Zhang

et al. 2016

Anal Bioanal Chem

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A sensitive and specific immunoaffinity column to clean up and isolate multiple mycotoxins was developed along with a rapid one-step sample preparation procedure for ultraperformance liquid chromatography-tandem mass spectrometry analysis. Monoclonal antibodies against aflatoxin B1, aflatoxin B2, aflatoxin G1, aflatoxin G2, zearalenone, ochratoxin A, sterigmatocystin, and T-2 toxin were coupled to microbeads for mycotoxin purification. We optimized a homogenization and extraction procedure as well as column loading and elution conditions to maximize recoveries from complex feed matrices. This method allowed rapid, simple, and simultaneous determination of mycotoxins in feeds with a single chromatographic run. Detection limits for these toxins ranged from 0.006 to 0.12 ng mL −1 , and quantitation limits ranged from 0.06 to 0.75 ng mL −1 . Concentration curves were linear from 0.12 to 40 μg kg −1 with correlation coefficients of R 2 > 0.99. Intra-assay and inter-assay comparisons indicated excellent repeatability and reproducibility of the multiple immunoaffinity columns. As a proof of principle, 80 feed samples were tested and several contained multiple mycotoxins. This method is sensitive, rapid, and durable enough for multiple mycotoxin determinations that fulfill European Union and Chinese testing criteria.

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Section: Matrix-matched Calibration Curves and Linear Rangecontrasting

confidence: 61%

Development of a multiple immunoaffinity column for simultaneous determination of multiple mycotoxins in feeds using UPLC–MS/MS

Zhang

et al. 2016

Anal Bioanal Chem

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“…Thanks to the high sensitivity of the recently developed analytical instruments, different liquid chromatography tandem mass spectrometry methods (LC-MS/MS) for the detection and quantification of biomarkers in urine were developed in order to assess mycotoxin exposure (Ediage et al, 2012;Gambacorta et al, 2013;Rodriguez-Carrasco et al, 2014b;Solfrizzo et al, 2011Solfrizzo et al, , 2013Song et al, 2013;Warth et al, 2011Warth et al, , 2013b. Only recently, results of epidemiological studies were increasingly reported whereby the exposure to mycotoxins in different populations was assessed through biomarkers.…”

mentioning

confidence: 98%

Human biomonitoring of multiple mycotoxins in the Belgian population: Results of the BIOMYCO study

Heyndrickx

Sioen

Huybrechts

et al. 2015

Environment International

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187

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Mycotoxins are important food contaminants responsible for health effects such as cancer, nephrotoxicity, hepatotoxicity or immunosuppression. The assessment of mycotoxin exposure is often based on calculations combining mycotoxin occurrence data in food with population data on food consumption. Because of limitations inherent to that approach, the direct measurement of biomarkers of exposure in biological fluids has been proposed as a suitable alternative to perform an accurate mycotoxin exposure assessment at individual level. For this reason, the BIOMYCO study was designed to assess mycotoxin exposure in Belgian adults and children using urinary biomarkers of exposure. Morning urine was gathered in a representative part of the Belgian population according to a standardised study protocol, whereby 155 children (3-12 years old) and 239 adults (19-65 years old) were selected based on random cluster sampling. These urine samples were analysed for the presence of 33 potential biomarkers with focus on aflatoxins, citrinin (CIT), fumonisins, trichothecenes, ochratoxin A (OTA), zearalenone and their metabolites using two validated LC-MS/MS methods. Nine out of the 33 analysed mycotoxins were detected whereby deoxynivalenol (DON), OTA, CIT and their metabolites were the most frequently detected. Deoxynivalenol-15-glucuronide was the main urinary DON biomarker and was found in all urine samples in the ng/mL range. Furthermore deoxynivalenol-3-glucuronide was quantified in 91% of the urine samples collected from children and in 77% of the samples collected from adults. Deoxynivalenol was detected in 70% and 37% of the samples of children and adults respectively. For the first time deepoxy-deoxynivalenol-glucuronide was detected in children's urine (17%). In the samples collected by adults, the prevalence was 22%. Whereas all these mycotoxins contaminated the urine samples in the ng/mL range, CIT and OTA were present in much lower concentrations (pg/mL). OTA contaminated 51% and 35% of the samples collected by children and adults respectively. CIT and its metabolite were present in 72% and 6% of children's urine, whereas they contaminated 59% and 12% of adult's urine. Finally, α-zearalenol and β-zearalenol-14-glucuronide were found in respectively one and two samples from adults. The exposure to DON, OTA and CIT was compared between subgroups and urinary mycotoxin concentrations differed significantly among age and gender. Based on the urinary levels, the daily intake of DON and OTA was estimated and evaluated whereby, depending on the used method, 16-69% of the population possibly exceeded the tolerable daily intake for DON and 1% for OTA. The BIOMYCO study is the first study whereby a multi-toxin approach was applied for mycotoxin exposure assessment in adults and children on a large-scale. Moreover, it is the first study that described the exposure to an elaborated set of mycotoxins in the Belgian population. Biomarker analysis showed a clear exposure of a broad segment of the Belgian population to DON, OTA and CIT. Th...

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“…To facilitate the phase separation and to reduce the miscibility of the analytes in the aqueous phase, this protocol adopted the approach of salting-out-assisted liquid-liquid extraction (SALLE), adding salt (NaCl) prior to the liquidliquid extraction to favour the transfer of the analytes into the organic solvent [26][27][28].…”

Section: Sample Preparationmentioning

confidence: 99%

Determination of Thyreostats in Bovine Urine and Thyroid Glands by HPLC–MS/MS

et al. 2016

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Abstract:Abstract The use of thyreostats in livestock is strictly forbidden by European legislation since 1981. The investigation of thyreostats is commonly performed by their detection as derivatives with 3-iodobenzylbromide. Although it leads advantages, the derivatisation procedure can generally cause a decrease in analyte concentrations. With the aim of simplifying the analysis of five thyreostats in both bovine urine and in thyroid glands, two methods were developed without the derivatisation step. Salting-out assisted liquid-liquid extraction was carried out for both matrices, followed by high-performance liquid chromatography coupled with triple-quadrupole mass spectrometry analysis. The methods were validated in agreement with the guidelines of Commission Decision 2002/657/EC. For all the thyreostats evaluated, satisfactory results were achieved; the recovery was within 96% to 104% for both the matrices, while precision (coefficient of variation) was less than 20% for urine and 21% for thyroid glands. The limits of decision and capacities of detection for all the compounds were lower than the recommended values of 10 μg L-¹ and 10 μg kg-¹, respectively. In urine, the limits of decision ranged from 6.9 to 7.3 μg L-¹, and the capacities of detection ranged from 8.5 to 9.7 μg L-¹, while in thyroid glands these values varied from 6.6 μg kg-¹ to 7.4 μg kg-¹ and from 8.0 μg g-¹ to 9.7 μg kg-¹, respectively. The results obtained show that the methods described are suitable for the direct detection of thyreostats in bovine urine and thyroid glands.

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Development and application of salting-out assisted liquid/liquid extraction for multi-mycotoxin biomarkers analysis in pig urine with high performance liquid chromatography/tandem mass spectrometry

Cited by 104 publications

References 31 publications

Development of a multiple immunoaffinity column for simultaneous determination of multiple mycotoxins in feeds using UPLC–MS/MS

Development of a multiple immunoaffinity column for simultaneous determination of multiple mycotoxins in feeds using UPLC–MS/MS

Human biomonitoring of multiple mycotoxins in the Belgian population: Results of the BIOMYCO study

Determination of Thyreostats in Bovine Urine and Thyroid Glands by HPLC–MS/MS

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