scholarly journals Validation Including Uncertainty Estimation of a GC–MS/MS Method for Determination of Selected Halogenated Priority Substances in Fish Using Rapid and Efficient Lipid Removing Sample Preparation

Foods ◽  
2019 ◽  
Vol 8 (3) ◽  
pp. 101 ◽  
Author(s):  
Slávka Nagyová ◽  
Peter Tölgyessy

A rapid method is proposed for the determination of selected H2SO4 stable organic compounds—eight organochlorines (OCs; hexachloro-1,3-butadiene, pentachlorobenzene, hexachlorobenzene, hexachlorocyclohexane—HCH—isomers, heptachlor) and six polybrominated diphenyl ethers (PBDEs; BDE-28, 47, 99, 100, 153, 154)—in fish samples. In the method, a modified QuEChERS (quick, easy, cheap, effective, rugged and safe) sample preparation using pH-tuned dispersive liquid–liquid microextraction (DLLME) and H2SO4 digestion fish extract clean-up is followed by gas chromatography–triple quadrupole tandem mass spectrometry (GC–QqQ-MS/MS) analysis. The method was validated in terms of linearity, limits of the method, recovery, accuracy, analysis of standard reference material (NIST SRM 1946), and estimation of combined uncertainty of the measurement (top-down approach). For validation, chub composite samples were used, and subsequently, the method was successfully applied to analysis of real samples of eight fish species. Finally, the method passed the analytical Eco-Scale evaluation as “an acceptable green analysis method”, and showed its advantages (simplicity, rapidity, low cost, high extract clean-up efficiency, good sensitivity) when compared to other reported QuEChERS based methods.

Chemosphere ◽  
2007 ◽  
Vol 66 (10) ◽  
pp. 1990-1997 ◽  
Author(s):  
Jui-Hwa Peng ◽  
Chin-Wang Huang ◽  
Ying-Ming Weng ◽  
Hwa-Kwang Yak

2021 ◽  
Vol 16 (1) ◽  
pp. 32-40
Author(s):  
O.V. Bayer ◽  
O.V. Bondarets ◽  
V.М. Mykhalska ◽  
L.V. Shevchenko ◽  
О.М. Stupak ◽  
...  

A liquid chromatographic-tandem mass spectrometric (LC–MS/MS) multi-residue method has been used for the simultaneous quantification and identification of 9 residues and metabolites of benzimidazole derivatives that the most widely used as anthelmintic veterinary drugs of animals. The modified QuEChERS method was used for sample preparation, which was initially developed for pesticide residue analysis. This paper highlights how quick, easy, cheap, effective and rugged the QuEChERS extraction method is. The method was successfully validated according to the 2002/657/EC guidelines. Recovery of analytes was in the range 99 – 110 %. The decission limits (ССα ) were calculated at MRL level for analytes with an established permitted limit as next: 104.5 μg kg-1 (albendazole), 53.2 μg kg-1 (fenbendazole), 54.2 μg kg-1 (flubendazole), 12.1 μg kg-1 (levamisole), 53.9 μg kg-1 (cambendazole), 64.2 μg kg-1 (mebendazole), 52.5 μg kg-1 (parabendazole), 105.8 μg kg-1 (thiabendazole), 234.2 μg kg-1 (triclobendazole). The suitability of the assay has been assessed through InterVal Software by quo data GmbH (Germany). The method achieves high quality of the results, good recovery, repeatabilities, within-lab reproducibilities, and wide analytical scope and has practical benefits, low cost, high sample throughput, little labor used and few lab ware.


2016 ◽  
Vol 38 (3-4) ◽  
pp. 460-468 ◽  
Author(s):  
Paula Berton ◽  
Sabrina B. Mammana ◽  
Daniela A. Locatelli ◽  
Nerina B. Lana ◽  
María B. Hapon ◽  
...  

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