Glutenvrij ? Pils onde de loep
Sleutels, I. ; Meer, I.M. van der; Broeck, H.C. van den - \ 2014
Voedingsmiddelentechnologie 7 (2014). - ISSN 0042-7934 - p. 10 - 11.
gluten - coeliakie - glutenvrije diëten - bieren - alcoholische dranken - gerst - lc-ms - analytische methoden - coeliac syndrome - gluten free diets - beers - alcoholic beverages - barley - liquid chromatography-mass spectrometry - analytical methods
Gluten meten in gehydrolyseerde en gefermenteerde voedingsmiddelen – zoals pils – is lastig. De door de Codex Alimentarius gevalideerde test onderschat het gehalte gluten in deze producten. Een uitgebreide LC-MS/MS-analyse geeft gedetailleerde informatie over de aanwezige coeliakie-stimulerende gluten in pils. Met deze gegevens is een geschikte test te ontwikkelen.
Effect of olive mill wastewater phenol compounds on reactive carbonyl species and Maillard reaction end-products in ultrahigh-temperature-treated milk
Troise, A.D. ; Fiore, A. ; Colantuono, A. ; Kokkinidou, S. ; Peterson, D.G. ; Fogliano, V. - \ 2014
Journal of Agricultural and Food Chemistry 62 (2014)41. - ISSN 0021-8561 - p. 10092 - 10100.
advanced glycation endproducts - nonfat dry milk - amino-acids - flavor components - mass-spectrometry - heat-treatment - model systems - bovine-milk - lc-ms - protein
Thermal processing and Maillard reaction (MR) affect the nutritional and sensorial qualities of milk. In this paper an olive mill wastewater phenolic powder (OMW) was tested as a functional ingredient for inhibiting MR development in ultrahigh-temperature (UHT)-treated milk. OMW was added to milk at 0.1 and 0.05% w/v before UHT treatment, and the concentration of MR products was monitored to verify the effect of OMW phenols in controlling the MR. Results revealed that OMW is able to trap the reactive carbonyl species such as hydroxycarbonyls and dicarbonyls, which in turn led to the increase of Maillard-derived off-flavor development. The effect of OMW on the formation of Amadori products and N-e-(carboxymethyl)-lysine (CML) showed that oxidative cleavage, C2–C6 cyclization, and the consequent reactive carbonyl species formation were also inhibited by OMW. Data indicated that OMW is a functional ingredient able to control the MR and to improve the nutritional and sensorial attributes of milk
Receptor-based high-throughput screening and identification of estrogens in dietary supplements using bioaffinity liquid-chromatography ion mobility mass spectrometry
Aqai, P. ; Gómez Blesa, N. ; Major, H. ; Pedotti, P. ; Varani, L. ; Ferrero, V.E.V. ; Haasnoot, W. ; Nielen, M.W.F. - \ 2013
Analytical and Bioanalytical Chemistry 405 (2013)29. - ISSN 1618-2642 - p. 9427 - 9436.
ms-binding assays - multi-residue method - anabolic-steroids - lc-ms - nutritional supplements - chemical derivatization - native marker - contamination - transporter - validation
A high-throughput bioaffinity liquid chromatography-mass spectrometry (BioMS) approach was developed and applied for the screening and identification of recombinant human estrogen receptor a (ERa) ligands in dietary supplements. For screening, a semi-automated mass spectrometric ligand binding assay was developed applying 13C2,15¿N-tamoxifen as non-radioactive label and fast ultra-high-performance–liquid chromatography–electrospray ionisation–triple-quadrupole-MS (UPLC-QqQ-MS), operated in the single reaction monitoring mode, as a readout system. Binding of the label to ERa-coated paramagnetic microbeads was inhibited by competing estrogens in the sample extract yielding decreased levels of the label in UPLC-QqQ-MS. The label showed high ionisation efficiency in positive electrospray ionisation (ESI) mode, so the developed BioMS approach is able to screen for estrogens in dietary supplements despite their poor ionisation efficiency in both positive and negative ESI modes. The assay was performed in a 96-well plate, and all these wells could be measured within 3 h. Estrogens in suspect extracts were identified by full-scan accurate mass and collision-cross section (CCS) values from a UPLC-ion mobility-Q-time-of-flight-MS (UPLC-IM-Q-ToF-MS) equipped with a novel atmospheric pressure ionisation source. Thanks to the novel ion source, this instrument provided picogram sensitivity for estrogens in the negative ion mode and an additional identification point (experimental CCS values) next to retention time, accurate mass and tandem mass spectrometry data. The developed combination of bioaffinity screening with UPLC-QqQ-MS and identification with UPLC-IM-Q-ToF-MS provides an extremely powerful analytical tool for early warning of ERa bioactive compounds in dietary supplements as demonstrated by analysis of selected dietary supplements in which different estrogens were identified.
LC-MS residue analysis of antibiotics : what selectivity is adequate?
Berendsen, B.J.A. - \ 2013
Wageningen University. Promotor(en): Michel Nielen, co-promotor(en): Linda Stolker. - S.l. : s.n. - ISBN 9789461735690 - 352
antibiotica - bèta-lactam antibiotica - chlooramfenicol - ceftiofur - voedselanalyse - lc-ms - selectiviteit - antibioticumresiduen - antibiotics - beta-lactam antibiotics - chloramphenicol - ceftiofur - food analysis - liquid chromatography-mass spectrometry - selectivity - antibiotic residues
In residue analysis of antibiotics quantitative and qualitative aspects are involved in declaring a sample non-compliant. The quantitative aspect regards the determination of the amount of the compound present in the sample. Validation procedures are available to determine the uncertainty of this result, which is taken into account in the decision making process. The qualitative aspect regards the confirmation of the identity of the compound present. In this, selectivity is the main parameter which is defined as the ability of a method to discriminate the analyte being measured from other substances. A trend observed in residue analysis is towards more generic methods for the detection of a broad range of compounds in a single run. As a result, by definition, selectivity is compromised. Procedures to determine the uncertainty of the qualitative aspect are lacking and, as a result, whether or not a method is adequately selective is a matter of experts’ judgment.
In this thesis a method is presented for grading selectivity of methods using liquid chromatography coupled to tandem mass spectrometry. Based on the outcome it can be stated if selectivity is adequate and thus if a confirmatory result stands strong when challenged in a court case. If selectivity is found inadequate, additional measures can be taken like the selection of another product ion or the use of a third product ion to obtain adequate selectivity.
Furthermore, two examples of analyses are presented in which selectivity plays an important role. First, the analysis of the banned antibiotic chloramphenicol (CAP). CAP contains two chiral centers and the nitro-group can either be para- or meta-substituted. Therefore, eight different isomers of CAP occur of which only RR-p-CAP is antimicrobially active. In the analysis of CAP, extreme selectivity is needed to distinguish the antimicrobially active compound from its inactive isomers. A method applying chiral liquid chromatography with tandem mass spectrometry was developed to discriminate antimicrobially active CAP for its inactive isomers. Also the research for the possible natural occurrence of this drug is presented. It is shown that CAP can be produced in unamended soil by Streptomyces venezuelaein appreciable amounts and that crops can take up CAP from soils. Therefore, it is concluded that CAP can occur in crops and animal feed due to its natural production by soil bacteria.
Second, the development of a multi-ß-lactam method is presented. In this method a derivatization is applied to be able to effectively detect off-label ceftiofur use. In this selectivity is intentionally compromised and no unequivocal confirmation can be carried out using this method. The developed method is applicable to a wide range of ß-lactam antibiotics including penicillins, cephalosporins and carbapenems and is the best method available today for effective monitoring of off-label ß-lactam usage in poultry breeding.
The (un)certainty of selectivity in liquid chromatography tandem mass spectrometry
Berendsen, B.J.A. ; Stolker, A.A.M. ; Nielen, M.W.F. - \ 2013
Journal of the American Society for Mass Spectrometry 24 (2013). - ISSN 1044-0305 - p. 154 - 163.
drug residues - lc-ms - identification - confirmation - spectra - library - fragmentation - system - food
We developed a procedure to determine the "identification power" of an LC-MS/MS method operated in the MRM acquisition mode, which is related to its selectivity. The probability of any compound showing the same precursor ion, product ions, and retention time as the compound of interest is used as a measure of selectivity. This is calculated based upon empirical models constructed from three very large compound databases. Based upon the final probability estimation, additional measures to assure unambiguous identification can be taken, like the selection of different or additional product ions. The reported procedure in combination with criteria for relative ion abundances results in a powerful technique to determine the (un)certainty of the selectivity of any LC-MS/MS analysis and thus the risk of false positive results. Furthermore, the procedure is very useful as a tool to validate method selectivity. Figure
Phomopsin A in lupin flour and lupin-containing food in the Netherlands
Nijs, W.C.M. de; Pereboom-de Fauw, D.P.K.H. ; Rijk, T.C. de; Mol, J.G.J. - \ 2012
- p. 1819 - 1826.
phomopsinen - mycotoxinen - lupinen - voedselveiligheid - lc-ms - phomopsins - mycotoxins - lupins - food safety - liquid chromatography-mass spectrometry
Survey on the occurrence of phomopsin A in lupin flour and lupin containing foods using an LC-MS/MS method.
MetAlign 3.0: performance enhancement by efficient use of advances in computer hardware
Lommen, A. ; Kools, H.J. - \ 2012
Metabolomics 8 (2012)4. - ISSN 1573-3882 - p. 719 - 726.
metabolomics approach - mass-spectrometry - lc-ms - identification - arabidopsis - metabolites - volatiles
A new, multi-threaded version of the GC-MS and LC-MS data processing software, metAlign, has been developed which is able to utilize multiple cores on one PC. This new version was tested using three different multi-core PCs with different operating systems. The performance of noise reduction, baseline correction and peak-picking was 8-19 fold faster compared to the previous version on a single core machine from 2008. The alignment was 5-10 fold faster. Factors influencing the performance enhancement are discussed. Our observations show that performance scales with the increase in processor core numbers we currently see in consumer PC hardware development.
"Design and application of a data-independent precursor and product ion repository."
Thalassinos, K. ; Vissers, J.P. ; Tenzer, S. ; Levin, Y. ; Thompson, J.W. ; Daniel, D. ; Mann, D. ; Delong, M.R. ; Moseley, M.A. ; America, A.H.P. ; Ottens, A.K. ; Cavey, G.S. ; Efstathiou, G. ; Scrivens, J.H. ; Langridge, J.I. ; Geromanos, S.J. - \ 2012
Journal of the American Society for Mass Spectrometry 23 (2012)10. - ISSN 1044-0305 - p. 1808 - 1820.
tandem mass-spectrometry - large-scale proteomics - peptide identification - protein identification - spectral library - lc-ms - ms/ms spectra - quantification - acquisition - resolution
The functional design and application of a data-independent LC-MS precursor and product ion repository for protein identification, quantification, and validation is conceptually described. The ion repository was constructed from the sequence search results of a broad range of discovery experiments investigating various tissue types of two closely related mammalian species. The relative high degree of similarity in protein complement, ion detection, and peptide and protein identification allows for the analysis of normalized precursor and product ion intensity values, as well as standardized retention times, creating a multidimensional/orthogonal queryable, qualitative, and quantitative space. Peptide ion map selection for identification and quantification is primarily based on replication and limited variation. The information is stored in a relational database and is used to create peptide- and protein-specific fragment ion maps that can be queried in a targeted fashion against the raw or time aligned ion detections. These queries can be conducted either individually or as groups, where the latter affords pathway and molecular machinery analysis of the protein complement. The presented results also suggest that peptide ionization and fragmentation efficiencies are highly conserved between experiments and practically independent of the analyzed biological sample when using similar instrumentation. Moreover, the data illustrate only minor variation in ionization efficiency with amino acid sequence substitutions occurring between species. Finally, the data and the presented results illustrate how LC-MS performance metrics can be extracted and utilized to ensure optimal performance of the employed analytical workflows.
Phomopsin A in food samples in The Netherlands
Nijs, W.C.M. de; Pereboom-de Fauw, D.P.K.H. ; Rijk, T.C. de; Egmond, H.J. van; Mol, J.G.J. - \ 2011
mycotoxinen - phomopsinen - lupinen - lc-ms - voedselveiligheid - mycotoxins - phomopsins - lupins - liquid chromatography-mass spectrometry - food safety
Phomopsin A (PHA) is a mycotoxin, mainly occurring in lupin. A straightforward LC/MS-MS method has been developed to investigate several lupin-containing food products available in the Netherlands.
European Analytical Criteria: Past, Present and Future
Vanhaecke, L. ; Gowik, P. ; Bizec, B. Le; Ginkel, L.A. van; Bichon, E. ; Blokland, M.H. ; Brabander, H.F. de - \ 2011
Journal of AOAC International 94 (2011)2. - ISSN 1060-3271 - p. 360 - 372.
ratio mass-spectrometry - carbon-isotope analysis - performance liquid-chromatography - meat-producing animals - veterinary drugs - urinary steroids - residue analysis - bovine urine - cattle urine - lc-ms
In this paper, the past, present, and (possible) future of the European analytical criteria for residues are described. The elaboration of the revision of Commission Decision 93/256/EC was a long process starting in 1996 and ending with the formation of a European Commission (EC) working group in 1998. This working group took account of developments in scientific and technical knowledge at that time and produced a draft version of the revision within 6 months. The revision, finally published in 2002 (2002/657/EC), includes new ideas on the identification of analytes and the criteria for performance assessment as well as validation procedures. Currently (2009), the evolution in analytical equipment and progress in scientific research, accompanied by recent European regulatory changes, demands an update or revision of the 2002/657/EC.
Quantitative determination of marine lipophilic toxins in shellfish using LC-MS/MS : international validation study - final report
Top, H.J. van den; Gerssen, A. ; Egmond, H.P. van - \ 2011
Wageningen : RIKILT (Report / Rikilt 2011.008)
bepaling - kwantiteitscontrole - mariene biologie - toxinen - schaaldieren - lc-ms - determination - quantity controls - marine biology - toxins - shellfish - liquid chromatography-mass spectrometry
Identification of anabolic steroids and derivatives using bioassay-guided fractionation,UHPLC/TOFMS analysis and accurate mass database searching
Peters, R.J.B. ; Rijk, J.C.W. ; Bovee, T.F.H. ; Nijrolder, A.W.J.M. ; Lommen, A. ; Nielen, M.W.F. - \ 2010
Analytica Chimica Acta 664 (2010)1. - ISSN 0003-2670 - p. 77 - 88.
liquid-chromatography - androgen bioassay - directed identification - veterinary drugs - screening method - human urine - hplc-uv - lc-ms - spectrometry - testosterone
Biological tests can be used to screen samples for large groups of compounds having a particular effect, but it is often difficult to identify a specific compound when a positive effect is observed. The identification of an unknown compound is a challenge for analytical chemistry in environmental analysis, food analysis, as well as in clinical and forensic toxicology. In this study bioassay-guided fractionation, ultra high performance liquid chromatography combined with time-of-flight mass spectrometry (UHPLC/TOFMS) and accurate mass database searching was tested to detect and identify unknown androgens. Herbal mixtures and sport supplements were tested using an androgen bioassay and modifications in sample preparations were carried out in order to activate inactive pro-androgens, androgen esters and conjugated androgens to enable their detection in the bioassay. Two of the four herbal mixtures tested positive and bioassay-guided fractionation followed by UHPLC/TOFMS of positive fractions resulted in the identification of nortestosterone phenylpropionate, testosterone cyclohexanecarboxylate and methyltestosterone. Three of the four sport supplements reacted toxic in the bioassay or gave inconclusive results and were further investigated using UHPLC/TOFMS in combination with data processing software and an accurate mass database having approximately 40,000 entries. This accurate mass database was derived from the PubChem database on the internet and coupled to the TOFMS software. This resulted in the tentative identification of several androgens, including methylboldenone, testosterone and the androgen esters methyltestosterone propionate or testosterone isobutyrate, testosterone buciclate and methylenetestosterone acetate. The study showed that bioassay-guided fractionation in combination with UHPLC/TOFMS analysis is a useful procedure to detect, isolate and identify unknown androgens in suspected samples. As an alternative, the use of data processing software in combination with an accurate mass database and coupled on-line with the TOFMS instrument software enabled the identification of androgens and androgen esters in the chromatogram even without bioassay-guided fractionation.
The analysis of lipophilic marine toxins : development of an alternative method
Gerssen, A. - \ 2010
Wageningen University. Promotor(en): Ivonne Rietjens; J. de Boer, co-promotor(en): Patrick Mulder. - [S.l. : S.n. - ISBN 9789085857198 - 199
toxinen - marien milieu - algen - alternatieven voor dierproeven - lc-ms - toxins - marine environment - algae - animal testing alternatives - liquid chromatography-mass spectrometry
Lipophilic marine toxins are produced by certain algae species and can accumulate in filter feeding shellfish such as mussels, scallops and oysters. Consumption of contaminated shellfish can lead to severe intoxications such as diarrhea, abdominal cramps and vomiting. Methods described in European Union (EU) legislation to test for the presence of these toxins are based on a mouse or rat bioassay. These assays are unethical and have a poor sensitivity and selectivity. The aim of this thesis is to develop an alternative method based on liquid chromatography - tandem mass spectrometry (LC-MS/MS) for the quantitative analysis of lipophilic marine toxins.
The Effect of Preanalytical Factors on Stability of the Proteome and Selected Metabolites in Cerebrospinal Fluid (CSF)
Rosenling, T. ; Slim, C.L. ; Christin, C. ; Coulier, L. ; Shi, S. ; Stoop, M.P. ; Bosman, J. ; Suits, F. ; Horvatovich, P.L. ; Stockhofe, N. ; Vreeken, R. ; Hankemeier, T. ; Gool, A.J. ; Luider, T.M. ; Bischoff, R. - \ 2009
Journal of Proteome Research 8 (2009)12. - ISSN 1535-3893 - p. 5511 - 5522.
chromatography-mass spectrometry - multiple-sclerosis - liquid-chromatography - biomarker discovery - cystatin-c - storage-conditions - sample collection - clinical-practice - lc-ms - serum
To standardize the use of cerebrospinal fluid (CSF) for biomarker research, a set of stability studies have been performed on porcine samples to investigate the influence of common sample handling procedures on proteins, peptides, metabolites and free amino acids. This study focuses at the effect on proteins and peptides, analyzed by applying label-free quantitation using microfluidics nanoscale liquid chromatography coupled with quadrupole time-of-flight mass spectrometry (chipLC-MS) as well as matrix-assisted laser desorption ionization Fourier transform ion cyclotron resonance mass spectrometry (MALDI-FT-ICR-MS) and Orbitrap LC-MS/MS to trypsin-digested CSF samples, The factors assessed were a 30 or 120 min time delay at room temperature before storage at -80 degrees C after the collection of CSF in order to mimic potential delays in the clinic (delayed storage), storage at 4 degrees C after trypsin digestion to mimic the time that samples remain in the cooled autosampler of the analyzer, and repeated freeze-thaw cycles to mimic storage and handling procedures in the laboratory. The delayed storage factor was also analyzed by gas chromatography mass spectrometry (GC-MS) and liquid chromatography mass spectrometry (LC-MS) for changes of metabolites and free amino acids, respectively. Our results show that repeated freeze/thawing introduced changes in transthyretin peptide levels. The trypsin digested samples left at 4 degrees C in the autosampler showed a time-dependent decrease of peak areas for peptides from prostaglandin D-synthase and serotransferrin. Delayed storage of CSF led to changes in prostaglandin D-synthase derived peptides as well as to increased levels of certain amino acids and metabolites. The changes of metabolites, amino acids and proteins in the delayed storage study appear to be related to remaining white blood cells. Our recommendations are to centrifuge CSF samples immediately after collection to remove white blood cells, aliquot, and then snap-freeze the supernatant in liquid nitrogen for storage at -80 degrees C. Preferably samples should not be left in the autosampler for more than 24 h and freeze/thaw cycles should be avoided if at all possible.
MetAlign: Interface-Driven, Versatile Metabolomics Tool for Hyphenated Full-Scan Mass Spectrometry Data Preprocessing
Lommen, A. - \ 2009
Analytical Chemistry 81 (2009)8. - ISSN 0003-2700 - p. 3079 - 3086.
liquid-chromatography - differential analysis - plant metabolomics - lc-ms - alignment - identification - extraction - profile - lc/ms
Hyphenated full-scan MS technology creates large amounts of data. A versatile easy to handle automation tool aiding in the data analysis is very important in handling such a data stream. MetAlign software-as described in this manuscript-handles a broad range of accurate mass and nominal mass GC/MS and LC/MS data. It is capable of automatic format conversions, accurate mass calculations, baseline corrections, peak-picking, saturation and mass-peak artifact filtering, as well as alignment of up to 1000 data sets. A 100 to 1000-fold data reduction is achieved. MetAlign software output is compatible with most multivariate statistics programs.
Metabolomics technologies applied to the identification of compounds in plants : a liquid chromatography-mass spectrometry - nuclear magnetic resonance perspective over the tomato fruit
Moco, S.I.A. - \ 2007
Wageningen University. Promotor(en): Raoul Bino; Sacco de Vries, co-promotor(en): Jacques Vervoort; Ric de Vos. - [S.l.] : S.n. - ISBN 9789085047421 - 222
solanum lycopersicum - tomaten - metabolieten - fytochemicaliën - kernmagnetische resonantiespectroscopie - metabolomica - lc-ms - solanum lycopersicum - tomatoes - metabolites - phytochemicals - nuclear magnetic resonance spectroscopy - metabolomics - liquid chromatography-mass spectrometry
A new era of plant biochemistry at the systems level is emerging in which the detailed description of biochemical phenomena, at the cellular level, is important for a better understanding of physiological, developmental, and biomolecular processes in plants. This emerging field is oriented towards the characterisation of small molecules (metabolites) that act as substrates, products, ligands or signalling entities in cells. This thesis concerns the development and establishment of such metabolomics strategies for screening and identifying metabolites in biological systems. Most technological strategies were applied to the assignment of metabolites from tomato (Solanum lycopersicum) fruit. Tomato was chosen for being a widely consumed crop with nutritional attributes, representing a model for the Solanaceae family. In order to achieve both high coverage of detected metabolites and valuable information for identification purposes, liquid chromatography coupled to mass spectrometry (LC-MS) and nuclear magnetic resonances (NMR) technologies were used. In addition, metabolite databases, based on experimental data (mass-based, in the case of LC-MS and chemical shift-based, in the case of NMR) were initiated, in order to systemize the extensive metabolite information. The chapters in this thesis describe method developments and their applications in plant metabolomics that are also feasible to be implemented on other biological systems. A review on the technologies used for metabolomics with a perspective on compound identification is presented in Chapter 1. In Chapter 2, a robust large scale LC-MS method for the analysis of metabolites in plants is described in detail. It presents a step-by-step protocol with thorough information about the reagents used, sample preparation, instrument setup, methods of analysis and data processing strategies. The described analytical method combines LC with photo diode array (PDA) and MS detection, and allows the analysis of mostly semi-polar secondary metabolites present in plants, such as phenolic acids, flavonoids, glucosinolates, saponins, alkaloids and derivatives thereof. Chapter 3 presents an application of the LC-PDA-MS method for the profiling of metabolites present in tomato fruit. The metabolites putatively identified in this fruit were included in a tomato dedicated-database (the MoTo DB) that is available for public search on the web (see: http://appliedbioinformatics.wur.nl). A comparison between two tomato fruit tissues, peel and flesh, for their metabolite content was made using this MoTo DB. Using the same LC-PDA-MS setup, several different tomato fruit tissues were compared in more detail, along the fruit ripening timeline, in Chapter 4. The presence of tissue-specific metabolites, at determined ripening stages, suggests developmental control of metabolite biosynthesis. Such tissue-specific metabolomics approach may give rise to a biological view over metabolite compartmentalisation. Chapters 5 and 6 describe the implementation of a NMR database for secondary metabolites, mostly including flavonoids, the Flavonoid Database (see: Flavonoid Database under http://www.wnmrc.nl). The acquisition of a large data set of related standard compounds allowed the analysis of shifts in NMR characteristics by the presence of certain functional groups or substituents in the flavonoid backbone. In addition, a 1H NMR-based prediction model was iteratively trained from the acquired experimental data and can be used for the prediction of unknown related molecules. This approach greatly increases the efficiency in the identification of (flavonoid) metabolites. Chapter 7 describes correlations of metabolomics data derived from LC-MS and NMR analyses of a large number of different tomato cultivars. The identification of metabolites is obtained among other available sources, the MoTo DB and the Flavonoid Database. This approach illustrates the complementariness and coincidence of NMR and MS as analytical techniques, applied to the detection of metabolites in tomato fruit. The summarizing discussion and conclusions, sets the work presented in this thesis into a biochemical perspective, and prospects suggestions for the future.
Gehaltebepaling van T2816 in waterige oplossingen met behulp van LC-MS
Rhijn, J.A. van - \ 1993
Wageningen : RIKILT-DLO (Rapport / RIKILT 93.01) - 16
oppervlaktespanningsverlagende stoffen - analytische methoden - lc-ms - analytische scheikunde - surfactants - analytical methods - liquid chromatography-mass spectrometry - analytical chemistry
Ontwikkelen van een massaspectrometrische confirmatie methode voor het aantonen van chlooramphenicol in vlees
Kienhuis, P.G.M. ; Traag, W.A. ; Aerts, M.M.L. ; Tuinstra, L.G.M.Th. - \ 1988
Wageningen : RIKILT (Rapport / RIKILT 88.40) - 12
chlooramfenicol - vlees - bevestigingstesten - massaspectrometrie - lc-ms - gc-ms - vloeistofchromatografie - hplc - analytische methoden - chloramphenicol - meat - confirmatory tests - mass spectrometry - liquid chromatography-mass spectrometry - gc-ms - liquid chromatography - hplc - analytical methods
In de EEG zijn onlangs een aantal criteria opgesteld, waaraan voldaan moet worden bij massaspectrametrische analyses, waarbij naast criteria voor de retentietijd, criteria voor het aantal te meten ionen, in relatie tot de ionisatietechniek worden gegeven. Op verzoek van de afdeling diergeneesmiddelen is recentelijk, onder andere in verband met een Nationaal plan en de algemene wens om bij de uitvoeringen van bepalingen met een wettelijke grondslag een confirmatiemethode ter beschikking te hebben, het onderzoek weer opgepakt. Onderzoek is verricht naar een aantal aspecten om te komen tot een goede confirmatie methode. Aandacht is gegeven aan het maken van derivaten, zowel met als zonder matrix, de uniekheid van de bijbehorende spectra, het opwerken van HPLC fracties welke chlooramphenicol bevatten, de lineariteit en reproduceerbaarheld van de GC-MS bij verschillende ionisatie-technieken en -omstandigheden. Parallel aan dit onderzoek zijn er experimenten uitgevoerd met de solid probe, waarbij chlooramphenicol, in vaste vorm , direct via een probe in de bron is gebracht. Ook is er onderzoek verricht naar de toepassing van LC-MS met betrekking tot chlooramphenicol. De resultaten van bovengenoemd onderzoek zullen t.z.t. apart worden gerapporteerd.
Ontwikkeling van een FAST-LC methode voor een aantal nitrofuranen in ei
Beek, W.M.J. ; Aerts, M.M.L. - \ 1986
Wageningen : RIKILT (Rapport / RIKILT 86.73) - 5
nitrofuranen - eieren - lc-ms - vloeistofchromatografie - nitrofurans - eggs - liquid chromatography-mass spectrometry - liquid chromatography
Doel van dit onderzoek was: Het bepalen en/of screenen van de belangrijkste nitrofuranen in ei met behulp van FAST-LC op een meetniveau van 10 ppb. Er is een FAST-LC methode voor nitrofurantoine, nitrofurazon, furazolidon en furaltadon in ei ontwikkeld. Evenals bij vlees en melk worden door toepassing van het FAST-LC systeem monsters "on-line" automatisch geanalyseerd.
Overzicht stand van zaken m.b.t. het ontwikkelen van analysemethoden voor het bepalen van enkele hormonen m.b.v. GC-MS
Traag, W.A. ; Keukens, H.J. ; Tuinstra, L.G.M.Th. ; Ruig, W.G. de - \ 1982
Wageningen : RIKILT (Verslag / RIKILT 82.80) - 17
hormonen - gaschromatografie - lc-ms - massaspectrometrie - urine - urine-analyse - diagnostische technieken - hormones - gas chromatography - liquid chromatography-mass spectrometry - mass spectrometry - urine - urine analysis - diagnostic techniques
Het vastleggen van enkele relevante gegevens voor de gaschromatografie- massaspectrometrische analyse van hormonen i.v.m. de bepaling in urine. Een achttal anabole stoffen zijn geselecteerd als zijnde mogelijke verbindingen welke in de toekomst met behulp van GC-MS onderzocht zullen moeten worden. Uitgegaan is van de in een eerder stadium ontwikkelde methode voor de bepaling van Diethylstilbestrol in runderurine. Teneinde na te gaan of deze methode geschikt is als multimethode en zo neen welke modificaties toegepast dienen te worden zijn alle facetten van de eerder beschreven methode (81.61) nagewerkt. Aanwijzingen, welke moeten leiden tot een zo'n uitgebreid mogelijke multimethode, worden gegeven.