Novel Multiresidue Method for the Determination of Eight Trichothecene Mycotoxins in Pollen Samples Using QuEChERS-Based GC-MS/MS

2017 ◽  
Vol 68 (2) ◽  
pp. 304-306
Author(s):  
Ionela Daniela Morariu ◽  
Liliana Avasilcai ◽  
Madalina Vieriu ◽  
Alina Diana Panainte ◽  
Nela Bibire

A simple multi-residue method based on QuEChERS-sample preparation was developed for the determination of eight trichothecene mycotoxins (nivalenol, fusarenon-x, diacetoxyscirpenol, 3-acetyl-deoxynivalenol, neosolaniol, deoxynivalenol, T-2 and HT-2 toxins) in pollen, using gas chromatography coupled with mass spectrometry. The developed method was validated by evaluating the following parameters: linearity, limit of quantification, matrix effect and precision of measurements. All mycotoxins showed good linearity. The method gave good recoveries (91-104%) with RSDs ] 11% for most of the analites (6 out of 8). The limits of quantification varied from 1 to 4�g�kg--1.

2011 ◽  
Vol 29 (2) ◽  
pp. 159-162 ◽  
Author(s):  
Nobuyuki Adachi ◽  
Hiroshi Kinoshita ◽  
Minori Nishiguchi ◽  
Motonori Takahashi ◽  
Harumi Ouchi ◽  
...  

Processes ◽  
2021 ◽  
Vol 9 (9) ◽  
pp. 1571
Author(s):  
Patricia Jové ◽  
Marina Vives-Mestres ◽  
Raquel De Nadal ◽  
Maria Verdum

Compounds 2,4,6-trichloroanisole (TCA), 2,3,4,6-tetrachloroanisole (TeCA), 2,4,6-tribromoanisole (TBA) and pentachloroanisole (PCA), 2-methylisoborneol (2MIB) and geosmin (GSM) have been reported as being responsible for cork and wine taint. A sustainable method based on thermal desorption-gas chromatography–mass spectrometry (TD-GC/MS) has been developed and optimized, taking into account desorption parameters and chromatographic and mass spectrometric conditions. The combination of parameters that jointly maximized the compound detection was as follows: desorption temperature at 300 °C, desorption time at 30 min, cryo-temperature at 20 °C and trap high temperature at 305 °C. The proposed methodology showed a good linearity (R ≤ 0.994) within the tested range (from 0.1 to 2 ng) for all target compounds. The precision expressed as repeatability and reproducibility was RSD < 10% in both. The limits of quantification ranged from 0.05 to 0.1 ng. The developed methodology and the sampling rates (R-values) of all targeted compounds (from 0.013 to 0.071 m3 h−1) were applied to the air analysis of two wineries. The results showed that the developed methodology is a sustainable and useful tool for the determination of these compounds in air.


2005 ◽  
Vol 88 (6) ◽  
pp. 1834-1839 ◽  
Author(s):  
Nicholas G Tsiropoulos ◽  
Konstantinos Liapis ◽  
Dimitrios T Likas ◽  
George E Miliadis

Abstract Analytical methodology was developed and validated for the determination of spiroxamine residues in grapes, must, and wine by gas chromatography/ion trap-mass spectrometry (GC/IT-MS). Two extraction procedures were used: the first involved grapes, must, and wine extraction with alkaline cyclohexane–dichloromethane (9 + 1, v/v) solution, and the second grape extraction with acetone, dichloromethane, and petroleum ether. In both procedures, the extract was centrifuged, evaporated to dryness, and reconstituted in cyclohexane or 2,2,4-trimethylpentane–toluene (9 + 1, v/v), respectively. Spiroxamine diastereomers A and B were determined by GC/IT-MS, and a matrix effect was observed in the case of grapes but not in must and wine. Recovery of spiroxamine from fortified samples at 0.02 to 5.0 mg/kg ranged from 78–102% for grapes and must, with relative standard deviation (RSD) &lt;13%; for red and white wines, recoveries ranged from 90 to 101% with RSD &lt;9%. The limit of quantification was 0.02 mg/kg for grapes, must, and wine or 0.10 mg/kg for grapes, depending on the extraction procedure used.


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