Determination of T-2 and HT-2 toxins in food and feed: an update

2014 ◽  
Vol 7 (2) ◽  
pp. 131-142 ◽  
Author(s):  
R. Krska ◽  
A. Malachova ◽  
F. Berthiller ◽  
H.P. van Egmond

Based on the recent scientific opinion of the European Food Safety Authority (EFSA) Panel on Contaminants in the Food Chain on the risks to human and animal health related to the presence of T-2 and HT-2 toxins in food and feed that was published by EFSA in the EFSA Journal, this article provides an update on the determination of these Fusarium mycotoxins. After a brief introduction into the chemistry of these toxins, both chromatographic and immuno-analytical methods are discussed for the determination of these type A trichothecenes. During the last decade, liquid chromatography with (tandem) mass spectrometry has become the most frequently used method for the determination of T-2 and HT-2 toxins, often within a multi-analyte approach. However, complex matrices and the resulting signal suppression effects, as observed particularly in electrospray-mass spectrometry methods owing to matrix effects, may require careful optimisation of clean-up, usage of matrix matched standards, or e.g. the use of internal standards. For specific purposes where extremely low limits of quantification are needed, e.g. for the analysis of duplicate diets, a dedicated gas chromatography method with multistage mass spectrometry has become available. Other novel analytical approaches to determine T-2 and HT-2 toxins in food and feed include biosensor-based methods in surface plasmon resonance and electrochemical formats, as well as DNA microchip assays. For rapid screening, several immunochemical methods (mostly ELISAs) have become available and some are sold as commercial test kits. Whereas these methods work fast, cross-reactivities with other trichothecenes can have an undesired effect on their accuracy. While proficiency tests including T-2 and HT-2 toxins have been carried out, none of the chromatographic or immunochemical methods have been formally validated in interlaboratory validation studies. There are no certified reference materials available for T-2 and HT-2 toxins.

2021 ◽  
Vol 22 (12) ◽  
pp. 6283
Author(s):  
Jérémy Lamarche ◽  
Luisa Ronga ◽  
Joanna Szpunar ◽  
Ryszard Lobinski

Selenoprotein P (SELENOP) is an emerging marker of the nutritional status of selenium and of various diseases, however, its chemical characteristics still need to be investigated and methods for its accurate quantitation improved. SELENOP is unique among selenoproteins, as it contains multiple genetically encoded SeCys residues, whereas all the other characterized selenoproteins contain just one. SELENOP occurs in the form of multiple isoforms, truncated species and post-translationally modified variants which are relatively poorly characterized. The accurate quantification of SELENOP is contingent on the availability of specific primary standards and reference methods. Before recombinant SELENOP becomes available to be used as a primary standard, careful investigation of the characteristics of the SELENOP measured by electrospray MS and strict control of the recoveries at the various steps of the analytical procedures are strongly recommended. This review critically discusses the state-of-the-art of analytical approaches to the characterization and quantification of SELENOP. While immunoassays remain the standard for the determination of human and animal health status, because of their speed and simplicity, mass spectrometry techniques offer many attractive and complementary features that are highlighted and critically evaluated.


Metabolites ◽  
2021 ◽  
Vol 11 (1) ◽  
pp. 47
Author(s):  
Kourosh Hooshmand ◽  
Inge S. Fomsgaard

Glucosinolates are biologically active secondary metabolites in Brassicaceae plants that play a critical role in positive and negative interactions between plants and root-associated microbial communities. The aim of this study was to develop a reversed-phase liquid chromatography method to quantify and identify intact glucosinolates in the root of Arabidopsis thaliana (Arabidopsis) grown in non-sterile natural soil by using liquid chromatography-hybrid triple quadruple-linear ion trap (LC-QqQ(LIT)) mass spectrometry. The Synergi Fusion C18-based column was found to be effective for sufficient retention and separation of nine intact glucosinolates without the need for time-consuming desulfation or ion-pairing steps. Method validation results showed satisfactory inter-day and intra-day precision for all glucosinolates except for 4-hydroxyglucobrassicin. Good inter-day and intra-day accuracy and recovery results were observed for glucoiberin, gluconapin, glucobrassicin, 4-methoxyglucobrassicin and neoglucobrassicin. However, for 4-hydroxyglucobrassicin, glucoraphanin and glucoerucin corrections to quantification results might be necessary since the recovery and accuracy results were not optimal. Matrix effects were shown to have a negligible effect on the ionization of all target analytes. The established liquid chromatography–tandem mass spectrometry (LC-MS/MS) method was applied to quantify target intact glucosinolates in Arabidopsis root crude extract of four different wild-type accessions where differences in terms of concentration and composition of intact glucosinolates were observed. Employment of sensitive and selective precursor ion survey scan of m/z 97 in combination with the information-dependent acquisition (IDA) of the enhanced product ion (EPI) dependent scan (Prec97-IDA-EPI) using LC-QqQ(LIT) provided high confidence in structural characterization of diverse intact glucosinolate profiles in complex Arabidopsis root crude extract.


2012 ◽  
Vol 10 (3) ◽  
pp. 876-899 ◽  
Author(s):  
Ednei Primel ◽  
Sergiane Caldas ◽  
Ana Escarrone

AbstractResidues of pesticides, pharmaceutical and personal care products (PPCPs) are contaminants of world-wide concern. Consequently, there is a growing need to develop reliable analytical methods, which enable rapid, sensitive and selective determination of these pollutants in environmental samples, at trace levels. In this paper, a review of the liquid chromatography-tandem mass spectrometry (LC-MS/MS) based methods for the determination of pesticides and PPCPs in the environment is presented. Advanced aspects of current LC-MS/MS methodology, including sample preparation and matrix effects, are discussed.


2019 ◽  
Vol 40 (3) ◽  
pp. 135-146 ◽  
Author(s):  
Darren Allen ◽  
Brett McWhinney

The screening of biological samples for the presence of illicit or legal substances is an important frontline tool in both clinical and forensic toxicology. In the clinical setting, drug screening is a useful tool for the clinician in improving patient care and guiding treatment. Analytical approaches for the screening of drugs in biological samples are extensive and well documented, though many rapid screening techniques often lack appropriate sensitivity and specificity, requiring careful clinical interpretation. The continuous emergence of new psychoactive substances presents a considerable analytical challenge in maintaining up-to-date methods for the detection of relevant drugs. Adapting and validating methods for the detection of new substances can be a complicated and costly undertaking. There is also a considerable lag time between the emergence of new drugs and the release of commercial assays for detection. Quadrupole time-of-flight mass spectrometry (Q-TOF-MS) has gained considerable attention over the last decade as an analytical technique that is capable of meeting the challenges of a rapidly changing drug landscape. Exhibiting both high sensitivity and specificity in drug detection, Q-TOF-MS also allows methods to be rapidly updated for newly emerging psychoactive agents. The coupling of Q-TOF-MS with techniques such as liquid or gas chromatography can provide both rapid and comprehensive screening solutions that are gaining popularity in the clinical laboratory setting.


1991 ◽  
Vol 37 (2) ◽  
pp. 210-215 ◽  
Author(s):  
Margaret-Anne Vaughan ◽  
Andrew D Baines ◽  
Douglas M Templeton

Abstract A rapid survey of the elements in biological materials, covering most of the elements in the periodic table, is possible by using available software for semi-quantitative analysis (SEMI-QUANT) by inductively coupled plasma-mass spectrometry. The procedure takes 5 min after sample preparation and gives results with a precision (CV) of approximately 20%. At a 10-fold dilution, 13 elements can be consistently and reliably detected in serum and 15 elements in whole-blood samples. At present the most important limitation of this method is mass overlap by polyatomic species for some elements of interest (e.g., Cr, Mn, and V). However, for the set of elements that can be reliably determined at endogenous concentrations, including Li, B, Mg, Fe, Cu, Zn, Rb, and Sr, the rapid scanning capability may be useful. Although matrix effects limit the direct interpretation of the semi-quantitative output, reasonable estimates of concentration are attainable by using matrix-matched standards or by adding a multielement standard to an aliquot from one sample in the set. We also present an example of determination of 25 elements in saliva from a patient with extensive dental work: Components of many of his dental alloys were readily identified. The method may also prove useful for screening multiple toxic exposures to heavier elements, such as Pb, Tl, Cd, and Hg.


2019 ◽  
Vol 58 (2) ◽  
pp. 109-116
Author(s):  
Lili Ma ◽  
Liuwei Zhao ◽  
Jiaqi Wang ◽  
Canping Pan ◽  
Cong Liu ◽  
...  

Abstract A multiresidue method for determining 12 carbamate pesticides in purple cabbage, orange, watermelon, cucumber, cowpea and Lactuca sativa L. employing multi-plug filtration cleanup (m-PFC) and ultra-performance liquid chromatography coupled with electrospray ionization tandem mass spectrometry (UPLC-ESI-MS/MS) was developed. M-PFC was carried out by cleanup at dispersive solid phase extraction (d-SPE), one m-PFC tip-filtration, two m-PFC tip-filtration and other methods (1–3 m-PFC cleanups). Results demonstrated that filtration simplified the cleanup method compared with d-SPE and other m-PFC methods (1–3 m-PFC cleanups). The method validation results showed that the method was linear, selective and accurate. The limits of quantification (LOQs) were 0.05–5.0 μg/kg, and the recoveries were in the range of 70.1–119.9% in different matrices. Although matrix effects were observed, they were successfully compensated using matrix-matched calibration. Finally, the developed method was successfully applied to detect pesticides in real samples.


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