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

Foods ◽  
2019 ◽  
Vol 8 (8) ◽  
pp. 302
Author(s):  
Flavio Antonio Franchina ◽  
Eliane Lazzari ◽  
George Scholl ◽  
Jean-François Focant
Keyword(s):  
Mass Spectrometry ◽  
High Resolution Mass Spectrometry ◽  
Multiple Reaction Monitoring ◽  
Triple Quadrupole ◽  
Eu Regulation ◽  
Relative Standard ◽  
Food And Feed ◽  
Quantitative Results ◽  
Feed Samples ◽  
The Eu

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.

Evaluation of ozonation as a method for mycotoxins degradation in malting wheat grains

2016 ◽  
Vol 9 (3) ◽  
pp. 409-417 ◽  
Author(s):  
I. Reinholds ◽  
G. Juodeikiene ◽  
E. Bartkiene ◽  
D. Zadeike ◽  
V. Bartkevics ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
High Performance ◽  
Degradation Rate ◽  
High Resolution Mass Spectrometry ◽  
Tandem Mass ◽  
Triple Quadrupole ◽  
Wheat Grain ◽  
Fusarium Mycotoxins ◽  
Wheat Grains ◽  
The Eu

The influence of ozone (O3) gas on reducing the contamination with Fusarium mycotoxins in malting wheat grains was investigated. Ultra-high performance liquid chromatography coupled to triple quadrupole tandem mass spectrometry (UHPLC-QqQ-MS/MS) and Orbitrap high resolution mass spectrometry (UHPLC-Orbitrap-HRMS) were used to determine mycotoxins in wheat grains before and 40 to 130 min after the exposure to 20 mg/l O3. Pearson’s analysis (R2=0.96-0.98) showed a good correlation between the performance efficiency of both mass spectrometry quantification techniques. The concentrations of determined mycotoxins (zearalenone (ZEA): 19.5-459 µg/kg, deoxynivalenol (DON): 3,370-4,620 µg/kg, T-2 toxin: 19.5-35.4 µg/kg, and HT-2 toxin: 258-819 µg/kg) decreased notably, depending on the duration of contact with ozone. A notable elimination of ZEA, HT-2, and T-2 in wheat grain was observed: the content of these compounds was reduced on average by 58.6, 64.6, and 62%, respectively, already after 40 min of ozonation. The effect was less pronounced in the case of DON, for which the average degradation rate reached the maximum of only 25% after 130 min exposure. We conclude that ozonation for up to 130 min was effective for reducing the content of most mycotoxins determined in this study, except for DON, in contaminated grains to concentrations below the acceptable maximum levels in wheat in accordance to the EU regulations.

scholarly journals Monitoring Lipophilic Toxins in Seawater Using Dispersive Liquid—Liquid Microextraction and Liquid Chromatography with Triple Quadrupole Mass Spectrometry

Toxins ◽  
2021 ◽  
Vol 13 (1) ◽  
pp. 57
Author(s):  
Ainhoa Oller-Ruiz ◽  
Natalia Campillo ◽  
Manuel Hernández-Córdoba ◽  
Javier Gilabert ◽  
Pilar Viñas
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Reversed Phase ◽  
Triple Quadrupole ◽  
Relative Standard ◽  
Mar Menor Lagoon ◽  
Lipophilic Toxins ◽  
Seawater Samples ◽  
Dispersive Liquid Liquid Microextraction ◽  
Liquid Microextraction

The use of dispersive liquid–liquid microextraction (DLLME) is proposed for the preconcentration of thirteen lipophilic marine toxins in seawater samples. For this purpose, 0.5 mL of methanol and 440 µL of chloroform were injected into 12 mL of sample. The enriched organic phase, once evaporated and reconstituted in methanol, was analyzed by reversed-phase liquid chromatography with triple-quadrupole tandem mass spectrometry. A central composite design multivariate method was used to optimize the interrelated parameters affecting DLLME efficiency. The absence of any matrix effect in the samples allowed them to be quantified against aqueous standards. The optimized procedure was validated by recovery studies, which provided values in the 82–123% range. The detection limits varied between 0.2 and 5.7 ng L−1, depending on the analyte, and the intraday precision values were in the 0.1–7.5% range in terms of relative standard deviation. Ten water samples taken from different points of the Mar Menor lagoon were analyzed and were found to be free of the studied toxins.

scholarly journals Pharmacokinetics of isocorynoxeine in rat plasma after intraperitoneal administration by UPLC–MS/MS

2020 ◽  
Vol 32 (4) ◽  
pp. 260-263
Author(s):  
Haichao Zhan ◽  
Zhen Wei ◽  
Ke Ren ◽  
Shuhua Tong ◽  
Xianqin Wang ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Tandem Mass Spectrometry ◽  
Multiple Reaction Monitoring ◽  
Intraperitoneal Administration ◽  
Gradient Elution ◽  
Ultra Performance Liquid Chromatography ◽  
Rat Plasma ◽  
Tandem Mass ◽  
Relative Standard ◽  
Liquid Chromatography Tandem Mass

Isocorynoxeine is one of the main alkaloids in Chinese medicinal herbs, and has pharmacological activities such as antihypertensive, sedative, anticonvulsant, and neuronal protection. It is an effective component of Uncaria for the treatment of hypertension. In this study, we used a fast and sensitive ultra-performance liquid chromatography–tandem mass spectrometry (UPLC–MS/MS) to detect isocorynoxeine in rat plasma and investigated its pharmacokinetics in rats. Six rats were given isocorynoxeine (15 mg/kg) by intraperitoneal (i.p.) administration. Blood (100 μL) was withdrawn from the caudal vein at 5 and 30 min and 1, 2, 4, 6, 8, 12, and 24 h after administration. Chromatographic separation was achieved using a UPLC BEH C18 column using a mobile phase of acetonitrile–0.1% formic acid with gradient elution. Electrospray ionization (ESI) tandem mass spectrometry in the multiple reaction monitoring (MRM) mode with positive ionization was applied. Intra-day and inter-day precisions (relative standard deviation, %RSD) of isocorynoxeine in rat plasma were lower than 12%. The method was successfully applied in the pharmacokinetics of isocorynoxeine in rats after intraperitoneal administration. The t1/2 of isocorynoxeine is 4.9 ± 2.1 h, which indicates quick elimination.

scholarly journals Quantitation of neonicotinoid insecticides, plus qualitative screening for other xenobiotics, in small-mass avian tissue samples using UHPLC high-resolution mass spectrometry

2019 ◽  
Vol 31 (3) ◽  
pp. 399-407 ◽  
Author(s):  
Michael S. Filigenzi ◽  
Emily E. Graves ◽  
Lisa A. Tell ◽  
Karen A. Jelks ◽  
Robert H. Poppenga
Keyword(s):  
Mass Spectrometry ◽  
High Resolution ◽  
Analytical Method ◽  
High Resolution Mass Spectrometry ◽  
Small Body ◽  
Screening Process ◽  
Tissue Samples ◽  
High Resolution Mass ◽  
Relative Standard ◽  
Resolution Mass

We developed and validated a liquid chromatography–high-resolution mass spectrometry (LC-HRMS) analytical method for quantitatively measuring pesticide concentrations in small-body avian tissue samples using homogenized 1–2-d-old chicken carcasses as the test matrix. We quantified the following key insecticides: sulfoxaflor (sulfoximine class) and the neonicotinoids dinotefuran, nitenpyram, thiamethoxam, acetamiprid, thiacloprid, clothianidin, and imidacloprid. We used fortified chick carcass samples to validate method accuracy (80–125% recoveries), precision (<20% relative standard deviation), and sensitivity (≤1.2 ppb) for these targeted analytes. This method also uses full-scan, high-resolution MS to screen for the presence of a wide variety of other xenobiotics in bird carcasses. The utility of our screening process was demonstrated by the detection of carbaryl in some samples. This sensitive LC-HRMS analytical method for insecticide detection in a matrix of homogenized carcass is ideal for evaluating small birds for insecticide exposure. This novel whole-carcass method may allow for research studies of small-bodied, free-ranging avian species, and could provide insight regarding their exposure to multiple classes of environmental contaminants.

scholarly journals Dissipation Kinetics and the Pre-Harvest Residue Limits of Acetamiprid and Chlorantraniliprole in Kimchi Cabbage Using Ultra-Performance Liquid Chromatography-Tandem Mass Spectrometry

Molecules ◽  
2019 ◽  
Vol 24 (14) ◽  
pp. 2616
Author(s):  
Jonghwa Lee ◽  
Byung Joon Kim ◽  
Eunhye Kim ◽  
Jeong-Han Kim
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
High Performance ◽  
Multiple Reaction Monitoring ◽  
Ultra Performance Liquid Chromatography ◽  
Tandem Mass ◽  
Dissipation Kinetics ◽  
Relative Standard ◽  
Harvest Residue

The dissipation behaviors of acetamiprid and chlorantraniliprole in kimchi cabbages were studied under open-field conditions. A simple and rapid analytical method was developed using ultra-high performance liquid chromatography coupled with tandem mass spectrometry (UHPLC-MS/MS). The multiple reaction monitoring (MRM) conditions of two pesticides were optimized to quantify and identify the pesticide residues. Sample preparation was performed by the QuEChERS (quick, easy, cheap, effective, rugged, and safe) method. Average recovery rates at the different spiked levels (0.05 and 0.25 mg/kg) were in the range of 103.6–113.9% (acetamiprid) and 80.8–91.2% (chlorantraniliprole), and the relative standard deviations were ≤4.3% for all. The dissipation kinetics were assessed using first-order equations after spraying acetamiprid and chlorantraniliprole individually on kimchi cabbages. The biological half-lives in field 1 and 2 were 5.2 and 6.3 days (acetamiprid) and 10.0 and 15.2 days (chlorantraniliprole), respectively. Based on the dissipation equations, the pre-harvest residue limits (PHRLs) corresponding to each day before harvest were suggested as the guidelines to meet the MRL on harvest day. It was also predicted that the terminal residues observed after multiple sprayings (three and seven days) would be below the MRL when harvested, in compliance with the established pre-harvest intervals.

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