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Assessment of a New GC-MS/MS System for the Confirmatory Measurement of PCDD/Fs and (N)DL-PCBs in Food under EU Regulation.

ABSTRACT: Polychlorodibenzo-p-dioxins (PCDDs), polychloro-dibenzofurans (PCDFs), dioxin-like (DL), and non dioxin-like (NDL) polychlorinated biphenyls (PCBs) are currently regulated in food and feed within the European territory (EU 2017/644-771). The confirmatory methods of analysis for checking compliance with maximum levels (MLs) for these involve either the historically-established GC-magnetic sector high-resolution mass spectrometry (GC-HRMS) and, more recently, GC-triple quadrupole mass spectrometry operating in tandem mode (GC-QQQMS/MS). In this study, the performance of a novel triple quadrupole GC-QQQMS/MS system equipped with a programable temperature vaporization (PTV) injector was evaluated for the analysis of regulated PCDD/Fs and PCBs in food and feed. The MS analyzer was equipped with a titanium ionization chamber and a new short collision cell capable to accumulate and eject ions by means of very narrow pulses that allow to minimize the noise and to adapt accumulation times for sensitive multiple reaction monitoring (MRM). The analytical capability of the system was confronted by the strict requirements (selectivity, reproducibility, linearity, quant/qual MRM transitions, accuracy, robustness) set by the EU Regulation for a range of standards, quality control (QC) and food/feed samples. In this respect, the approach showed high precision (1.9-15% relative standard deviation (RSD) at low pg/µL) and accuracy (>80%, except for one hexa-CDD). The quantitative results were also compared to the most used GC-HRMS. In this case, comparable results in terms of single congener concentration basis and total toxic equivalent (TEQ) basis for PCDD/Fs and DL-PCBs were obtained for the QC samples analyzed.

SUBMITTER: Franchina FA

PROVIDER: S-EPMC6722952 | biostudies-literature |

REPOSITORIES: biostudies-literature

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Project description:Highlights • Malondialdehyde (MDA) is an important biomarker of oxidative stress (lipid peroxidation)• MDA and [1,3-dideutero]MDA (d2-MDA) for use as internal standard react with pentafluorobenzyl bromide (PFB-Br) in aqueous acetone to form di-PFB derivatives.• GC–MS/MS allows for highly accurate measurement of MDA in human plasma, serum and urine.• Many pre-analytical factors including hemolysis may compromise measurement of biological MDA.• Sample storage and study design of long-term clinical studies are important factors to be considered. Malondialdehyde (MDA; 1,3-propanedial, OHC-CH2-CHO) is one of the most frequently measured biomarkers of oxidative stress in plasma and serum. L-Arginine (Arg) is the substrate of nitric oxide synthases (NOS), which convert L-arginine to nitric oxide (NO) and L-citrulline. The Arg/NO pathway comprises several members, including the endogenous NOS-activity inhibitor asymmetric dimethylarginine (ADMA) and its major metabolite dimethyl amine (DMA), and nitrite and nitrate, the major NO metabolites. Reliable measurement of MDA and members of the Arg/NO pathway in plasma, serum, urine and in other biological samples, such as saliva and cerebrospinal fluid, is highly challenging both for analytical and pre-analytical reasons. In our group, we use validated gas chromatography-mass spectrometry (GC–MS) and gas chromatography-tandem mass spectrometry (GC–MS/MS) methods for the quantitative determination in clinical studies of MDA as a biomarker of oxidative stress, and various Arg/NO metabolites that describe the status of this pathway. Here, the importance of pre-analytical issues, which has emerged from the use of GC–MS and GC–MS/MS in clinico-pharmacological studies, is discussed. Paradigmatically, two studies on the long-term oral administration of L-arginine dihydrochloride to patients suffering from peripheral arterial occlusive disease (PAOD) or coronary artery disease (CAD) were considered. Pre-analytical issues that were addressed include blood sampling, plasma or serum storage, study design (notably in long-term studies), and the alternative of measuring MDA in human urine.

Dataset Information

Assessment of a New GC-MS/MS System for the Confirmatory Measurement of PCDD/Fs and (N)DL-PCBs in Food under EU Regulation.

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