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Nathanail A.V.,Finnish Food Safety Authority | Sarikaya E.,Thermo Fisher Scientific | Jestoi M.,Finnish Food Safety Authority | Godula M.,Thermo Fisher Scientific | Peltonen K.,Finnish Safety and Chemicals Agency
Journal of Chromatography A | Year: 2014

In this study, we compared the performance of conventional sample preparation techniques used in mycotoxin analyses against automated on-line sample clean-up for the determination of deoxynivalenol (DON) and its conjugated derivative, deoxynivalenol-3-β-d-glucoside (D3G), in cereal grains. Blank wheat and barley samples were spiked with DON and D3G, extracted with a mixture of acetonitrile:water (84:16, v/v) and processed by one of the following: extract and shoot, MycoSep® 227 clean-up columns, MycoSep 227 with an additional acetonitrile elution step and centrifugal filtration, followed by analysis with liquid chromatography tandem mass spectrometry. Based on method performance characteristics and poor recoveries (<30%) obtained for the polar D3G with some techniques, the extract and shoot approach was chosen for the inter-laboratory method comparison study. Thus, the same spiked samples were analysed in parallel by another laboratory with an in-house validated on-line sample clean-up method, utilising TurboFlow™ chromatography coupled to high resolution mass spectrometry. Method validation was performed by determination of specificity, linearity, recovery, intra-day precision and the limits of detection and quantification. Matrix-matched linearity (R2>0.985) was established in the range of 100-1600 and 20-320μg/kg for DON and D3G, respectively. Average recoveries (%RSD) were acceptable with both methods for wheat and barley, ranging between 73% and 102% (3-12%) for DON and 72% and 98% (1-10%) for D3G. The benefit of using automated sample clean-up in comparison to extract and shoot is the ability to inject directly pure extracts into the mass spectrometer, offering faster analyses and improved sensitivity with minimum system maintenance. © 2014 Elsevier B.V.All rights reserved. Source


Rajamaki J.,Laurea University of Applied Sciences | Rajamaki M.,Finnish Safety and Chemicals Agency
European Conference on Information Warfare and Security, ECCWS | Year: 2013

The National Security Auditing Criteria, KATAKRI, were published in 2009, revised in 2011, and version III is currently under revision. The root of KATAKRI is to preserve the confidentiality of any confidential and classified information held by the organisation concerned. One of KATAKRI's aims is to combine the actions of authorities when verifying the security level of a company or other corporation by carrying out security auditing. From the enterprise operators' point of view, the focus of security auditing is to eliminate unfair competition and maintain an equal opportunity field for operators. Another of KATAKRI's aims is to improve national security when Finnish Defence Forces or other security authorities apply subcontracting. KATAKRI is also intended to help companies and corporations when they are developing their own security level. The purpose of this case study is to find out: what is expected from the security auditing process and from the leading auditor; what kind of competence the auditor should have; and how the security auditing training and qualification should be developed to correspond with the needs of the security field. The empirical research was conducted in the form of interviews, questionnaires and observations made as a student during the first KATAKRI leading auditor course executed 2/2/2012-12/12/2012. The combined results showed that deep knowledge of the security field and competence to manage overall security is required from security auditors. Furthermore, it was concluded that qualifications for security auditors should be created in accordance with ISO Standard 19011:2011, which provides a very strong competence model. In light of the above, it is recommended that the academic level, content and requirements of future audit and security auditing training should be clearly defined, and the quality of the training should be standardised and certified. The results also indicate that KATAKRI version II still has defects due to its inconsistency. One task of auditing processes should be collecting information about KATAKRI's shortcomings, and they should be systematically analysed. Future leading auditor courses would be suitable scenes to analyse shortcomings and to propose improvements to KATAKRI. KATAKRI should be revised every second or third year. Source


Handy R.D.,University of Plymouth | Van Den Brink N.,Wageningen University | Chappell M.,U.S. Army | Muhling M.,TU Bergakademie Freiberg | And 11 more authors.
Ecotoxicology | Year: 2012

This review paper reports the consensus of a technical workshop hosted by the European network, NanoImpactNet (NIN). The workshop aimed to review the collective experience of working at the bench with manufactured nanomaterials (MNMs), and to recommend modifications to existing experimental methods and OECD protocols. Current procedures for cleaning glassware are appropriate for most MNMs, although interference with electrodes may occur. Maintaining exposure is more difficult with MNMs compared to conventional chemicals. A metal salt control is recommended for experiments with metallic MNMs that may release free metal ions. Dispersing agents should be avoided, but if they must be used, then natural or synthetic dispersing agents are possible, and dispersion controls essential. Time constraints and technology gaps indicate that full characterisation of test media during ecotoxicity tests is currently not practical. Details of electron microscopy, dark-field microscopy, a range of spectroscopic methods (EDX, XRD, XANES, EXAFS), light scattering techniques (DLS, SLS) and chromatography are discussed. The development of user-friendly software to predict particle behaviour in test media according to DLVO theory is in progress, and simple optical methods are available to estimate the settling behaviour of suspensions during experiments. However, for soil matrices such simple approaches may not be applicable. Alternatively, a Critical Body Residue approach may be taken in which body concentrations in organisms are related to effects, and toxicity thresholds derived. For microbial assays, the cell wall is a formidable barrier to MNMs and end points that rely on the test substance penetrating the cell may be insensitive. Instead assays based on the cell envelope should be developed for MNMs. In algal growth tests, the abiotic factors that promote particle aggregation in the media (e.g. ionic strength) are also important in providing nutrients, and manipulation of the media to control the dispersion may also inhibit growth. Controls to quantify shading effects, and precise details of lighting regimes, shaking or mixing should be reported in algal tests. Photosynthesis may be more sensitive than traditional growth end points for algae and plants. Tests with invertebrates should consider non-chemical toxicity from particle adherence to the organisms. The use of semi-static exposure methods with fish can reduce the logistical issues of waste water disposal and facilitate aspects of animal husbandry relevant to MMNs. There are concerns that the existing bioaccumulation tests are conceptually flawed for MNMs and that new test(s) are required. In vitro testing strategies, as exemplified by genotoxicity assays, can be modified for MNMs, but the risk of false negatives in some assays is highlighted. In conclusion, most protocols will require some modifications and recommendations are made to aid the researcher at the bench. © Springer Science+Business Media, LLC 2012. Source


A disease survey in Finnish oilseed Brassica (OSR) fields in 2007-09 revealed the widespread occurrence and several fold increase of necrotic stem base lesions and severely injured blackened roots in comparison to a corresponding survey carried out in 1984-89. Rhizoctonia solani was the predominant fungi detected in the isolations and was followed by several species of Fusarium and Thielaviopsis basicola. In 60% of the samples all three species were detected together. Only the R. solani AG 2-1 strains isolated from OSR and other cruciferous hosts caused damping off or stem base symptoms on turnip rape in a greenhouse experiment. Therefore R. solani AG 2-1 was considered the main pathogen associated with the observed symptoms in OSR crops. Cultural practices changed significantly between the 1980s and 2000s. In the 2007-09 survey there was an increase in the cultivation of oilseed rape instead of turnip rape, increase in the use of no soil or reduced soil tillage and of chemical control of weeds, but a reduction in macronutrient fertilization, especially P and K, when compared to the 1980s survey. The risk for high incidence of stem base lesions and blackened roots was affected by different cultural practices. No tillage and maintaining sufficient soil pH and NPK fertilisation decreased the risk for both types of R. solani induced symptoms. Late sowing date increased the risk for high incidence of stem base lesions, while application of fungicides against Sclerotinia reduced it. The incidence of R. solani damages in many fields was very high in spite of relatively long crop rotations and therefore the average effect of crop rotation in the disease was insignificant. Current turnip rape cultivars are vulnerable to root rot while oilseed rape is vulnerable to stem base symptoms. The higher incidence of R. solani induced diseases could be associated with the decline in productivity of OSR crops in Finland. This study showed that cultural practices such as reduced or no soil tillage, adequate levels of pH and of NPK fertilization could reduce the severity of the symptoms in OSR fields. © 2016 Association of Applied Biologists. Source


Nathanail A.V.,Finnish Food Safety Authority | Syvahuoko J.,Finnish Food Safety Authority | Malachova A.,University of Natural Resources and Life Sciences, Vienna | Jestoi M.,Finnish Food Safety Authority | And 6 more authors.
Analytical and Bioanalytical Chemistry | Year: 2015

Abstract A reliable and sensitive liquid chromatography-tandem mass spectrometric method was developed for the simultaneous quantitative determination in cereals of the Fusarium mycotoxins HT-2 toxin, T-2 toxin, deoxynivalenol, nivalenol and zearalenone, as well as the modified metabolites 3-acetyl-deoxynivalenol, α-zearalenol, β-zearalenol, deoxynivalenol-3-glucoside, HT-2-3-glucoside, nivalenol-3-glucoside, zearalenone-14-glucoside, zearalenone-14-sulphate, zearalenone-16-glucoside, α-zearalenol-14-glucoside and β-zearalenol-14-glucoside. The 'dilute and shoot' approach was used for sample preparation after extraction with acetonitrile:water:acetic acid (79:20:1, v/v/v). Separation was carried out using reversed-phase liquid chromatography, and detection was performed using tandem mass spectrometry in the selected reaction monitoring mode. The method was in-house validated according to performance characteristics, established in Commission Regulation EC No 401/2006 and Commission Decision EC No 657/2002, prior to its application in a nationwide survey for the analysis of barley, oat and wheat samples (n=95) harvested in Finland during 2013. Deoxynivalenol and its glucosylated form were the most abundant of the analytes, being detected in 93 and 81 % of the samples, respectively. Concentrations of deoxynivalenol were unusually high in 2013, especially in oats, with some cases exceeding the maximum legislative limits for unprocessed oats placed on the market for first-stage processing. All modified mycotoxins analysed were detected, and the natural occurrence of some of these compounds (e.g. zearalenone-16-glucoside and nivalenol-3-glucoside) in barley, oats and/or wheat was documented for the first time. © 2015 The Author(s). Source

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