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Roberto Romerogonzalez - One of the best experts on this subject based on the ideXlab platform.
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comprehensive analysis of toxics pesticides Veterinary Drugs and mycotoxins in food by uhplc ms
Trends in Analytical Chemistry, 2014Co-Authors: Antonia Garrido Frenich, Roberto Romerogonzalez, Maria Del Mar AguileraluizAbstract:This review provides an overview of current methods, based on ultra-high-performance liquid chromatography coupled to mass-spectrometry analyzers (UHPLC-MS), for the determination of organic contaminants and residues in food. Although most of the methods mainly focus on the analysis of one type of compound (e.g., pesticides, Veterinary Drugs or mycotoxins), current methods are aimed at the simultaneous determination of several families of contaminants and/or residues. These methods increase sample throughput and the capabilities of routine laboratories, because of the advantages provided by the UHPLC technique. For UHPLC-MS, generic extraction procedures can be applied, allowing the simultaneous extraction of compounds with different physicochemical properties.
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comprehensive qualitative and quantitative determination of pesticides and Veterinary Drugs in honey using liquid chromatography orbitrap high resolution mass spectrometry
Journal of Chromatography A, 2012Co-Authors: Maria Luz Gomezperez, Patricia Plazabolanos, Roberto Romerogonzalez, J L Martinezvidal, Antonia GarridofrenichAbstract:Abstract A database has been created for the simultaneous analysis of more than 350 pesticides and Veterinary Drugs (including antibiotics) using ultra-high performance liquid chromatography coupled to high resolution Orbitrap mass spectrometry (UHPLC–Orbitrap-MS). This is a comprehensive exact mass database built using the Exactive-Orbitrap analyzer. The developed database includes exact masses of the target ions and retention time data, and allows the automatic search of the included compounds. Generic chromatographic and MS conditions have been applied. The presented database is suitable for qualitative analysis, and it was also evaluated for quantitative purposes in routine analysis, after the optimization and validation of a generic extraction method in honey samples. Adequate recovery and precision values for most of the studied analytes were obtained and the limits of detection (LOD) ranged from 1 to 50 μg kg −1 . For pesticides, LODs were always lower than the MRLs established by European Union in honey, except for a few compounds. This method was applied to the analysis of 26 real honey samples and some pesticides (azoxystrobin, coumaphos, dimethoate and thiacloprid) were detected in 4 samples. Azoxystrobin and coumaphos were determined in two different samples (organic honey) at 1.5 μg kg −1 and 5.1 μg kg −1 . Veterinary Drugs were not detected in the analyzed samples.
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food contaminant analysis at high resolution mass spectrometry application for the determination of Veterinary Drugs in milk
Journal of Chromatography A, 2011Co-Authors: Roberto Romerogonzalez, Patricia Plazabolanos, Maria Del Mar Aguileraluiz, Garrido A Frenich, J Martinez L VidalAbstract:Abstract Veterinary Drugs (VDs) can remain in milk as a consequence of their use in livestock. In order to control the levels of VD residues in milk, screening methodologies can be applied for a rapid discrimination among negative and non-negative samples. In a second stage, non-negative samples are classified as negative or positive samples by using a confirmation method. Pre-target screening methods in low resolution MS (LRMS) are normally applied, but the number of analytes is limited, whereas the information obtained by full scan acquisition in high resolution mass spectrometry (HRMS) is improved. Here, three screening methods (running time
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comparison of several extraction techniques for multiclass analysis of Veterinary Drugs in eggs using ultra high pressure liquid chromatography tandem mass spectrometry
Analytica Chimica Acta, 2010Co-Authors: Antonia Garrido Frenich, Maria Del Mar Aguileraluiz, Jose Luis Martinez Vidal, Roberto RomerogonzalezAbstract:: This study compared four extraction methods for the simultaneous determination of tetracyclines, macrolides, quinolones, sulphonamides and anthelmintics (including benzimidazoles and avermectins) in eggs by ultra-high pressure liquid chromatography coupled to tandem mass spectrometry (UHPLC-MS/MS). Solvent extraction, solid-phase extraction (SPE), matrix solid-phase dispersion (MSPD) and modified QuEChERS procedure were compared in terms of recovery and number of Veterinary Drugs extracted. The solvent extraction procedure with a clean-up step provided better results than the other tested procedures. The QuEChERS procedure was simpler and faster, but extracted fewer compounds than solvent extraction. MSPD did not extract tetracyclines and quinolones, whereas macrolides and tetracyclines were not extracted when SPE was applied. The solvent extraction procedure was validated, obtaining recoveries ranging from 60% (sulfaquinoxaline) to 119% (levamisole) with repeatability values (expressed as relative standard deviations, RSDs) lower than 20% at two concentration levels (10 and 100 microg kg(-1)), except for erythromycin, emamectin and ivermectin that showed RSD values close to 25% at 10 microg kg(-1). Limits of quantification (LOQs) were always equal or lower than 5 microg kg(-1). Finally the method was applied to egg samples, and erythromycin, enrofloxacin, difloxacin, thiabendazole, emamectin and fenbendazole were detected in four samples.
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multi residue determination of Veterinary Drugs in milk by ultra high pressure liquid chromatography tandem mass spectrometry
Journal of Chromatography A, 2008Co-Authors: Maria Del Mar Aguileraluiz, Roberto Romerogonzalez, Jose Luis Martinez Vidal, Antonia Garrido FrenichAbstract:A simple, selective and fast multi-residue method was developed to determine 18 Veterinary Drugs in milk by ultra-high-pressure liquid chromatography coupled to tandem quadrupole mass spectrometry. The selected antibiotics include quinolones, sulphonamides, macrolides, anthelmintics and one tetracycline. An extraction procedure based on QuEChERS methodology (quick, easy, cheap, effective, rugged and safe), consisting of a liquid extraction of the milk samples with acetonitrile without sample clean up was performed. The extract was centrifuged and the supernatant was filtered prior to chromatographic analysis. Several chromatographic conditions were optimized in order to obtain a fast separation (less than 10 min). The antibiotics were detected by electrospray ionization in positive ion mode with multiple reaction monitoring (MRM) and mass spectrometric conditions were optimized in order to increase selectivity and sensitivity. The developed method was validated in terms of linearity, trueness, precision, limits of detection (LODs) and quantification. Mean recoveries ranged from 70% to 110% and interday precision was lower than 21%. LODs ranged from 1 to 4 μg/kg. Finally, the method was applied to real samples and only traces of tylosin and fenbendezol were detected in two samples.
Vicent Yusa - One of the best experts on this subject based on the ideXlab platform.
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target analysis and retrospective screening of Veterinary Drugs ergot alkaloids plant toxins and other undesirable substances in feed using liquid chromatography high resolution mass spectrometry
Talanta, 2016Co-Authors: Nuria Leon, Agustin Pastor, Vicent YusaAbstract:Abstract A comprehensive strategy combining a quantitative method for 77 banned Veterinary Drugs, mycotoxins, ergot alkaloids and plant toxins, and a post-target screening for 425 substances including pesticides and environmental contaminants in feed were developed using a QuEChERS-based extraction and an ultra-high performance liquid chromatography coupled to high-resolution mass spectrometry (UHPLC–HRMS). The quantitative method was validated after previous statistical optimisation of the main parameters governing ionisation, and presented recoveries ranging, in general, from 80 to 120%, with a precision in terms of Relative Standard Deviation (RSD) lower than 20%. The full-scan accurate mass data were acquired with a resolving power of 50000 FWHM and a mass accuracy lower than 5 ppm. The method LOQ was lower than 12.5 µg kg −1 for the majority of the Veterinary Drugs and plant toxins and 20 µg kg −1 for ergot alkaloids. For post-target screening a customised theoretical database including the exact mass, the polarity of acquisition and the expected adducts was built and used for post-run retrospective screening. The analytical strategy was applied to 32 feed samples collected from farms of the Valencia Region (Spain). Florfenicol, zearalenone and atropine were identified and quantified at concentrations around 10 µg kg −1 . In the post-target screening of the real samples, Sulfadiazine, Thrimetoprin and Pirimiphosmethyl were tentatively identified.
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qualitative screening of 116 Veterinary Drugs in feed by liquid chromatography high resolution mass spectrometry potential application to quantitative analysis
Food Chemistry, 2014Co-Authors: C Boix, Nuria Leon, Vicent Yusa, Maria Ibanez, Juan V Sancho, Felix HernandezAbstract:Abstract Veterinarian and human pharmaceuticals may be intentionally added to animal feed to enhance animal production. Monitoring these substances is necessary for protecting the consumers. In this work, a screening method covering 116 human and Veterinary Drugs has been developed and validated in five types of animal feed at 0.02 and 0.2 mg kg−1. After a simple extraction and dilution, the samples were analysed by ultra-high performance liquid chromatography coupled to quadrupole time-of-flight mass spectrometry (UHPLC-QTOF MS). Nearly all compounds tested were detected at 0.02 mg kg−1, based on the presence of the accurate-mass (de)protonated molecule. However, the identification using a second accurate-mass ion was more problematic at this level. Finally, the procedure was applied to 22 feed samples, where trimethoprim, robenidine, or α- and β-nandrolone were detected and identified. The potential applicability of the method to quantitative analysis of the compounds detected in the samples was also evaluated.
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wide range screening of banned Veterinary Drugs in urine by ultra high liquid chromatography coupled to high resolution mass spectrometry
Journal of Chromatography A, 2012Co-Authors: Nuria Leon, Agustin Pastor, Claudia P B Martins, Marta Roca, Carmen Igualada, Vicent YusaAbstract:Abstract In this work, an ultra high performance liquid chromatography–high resolution mass spectrometry (UHPLC–HRMS) methodology is proposed for the multi-class multi-residue screening of banned and unauthorized Veterinary Drugs in bovine urine, using an Orbitrap Exactive™ analyzer working at a resolving power of 50,000 FWHM in full scan, both in positive and negative mode. The method currently covers 87 analytes belonging to different families such as steroid hormones, β-agonists, resorcylic acid lactones (RAL), stilbens, tranquillizers, nitroimidazoles, corticosteroids, NSAIDs, amphenicoles, thyreostatics and other substances such as dapsone. A database including the elemental composition, the polarity of acquisition, retention time and expected adducts was built for the targeted analysis, and a high mass accuracy (
Xi Xia - One of the best experts on this subject based on the ideXlab platform.
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multi class analysis of Veterinary Drugs in eggs using dispersive solid phase extraction and ultra high performance liquid chromatography tandem mass spectrometry
Food Chemistry, 2021Co-Authors: Chengfei Wang, Yingyu Wang, Lan Zhou, Xi XiaAbstract:Abstract A multi-residue method has been developed for the identification and quantification of 78 compounds from seven different classes of Veterinary Drugs in eggs. This method was based on dispersive solid phase extraction where mixed-mode cation exchange sorbent was used to combine the isolation of compounds and sample purification. The analysis was performed using ultra-high performance liquid chromatography-tandem mass spectrometry, and the chromatographic run time of one injection was 9.5 min. The mean recovery ranged from 70.5% to 119.2% and inter-day relative standard deviation was less than 17.0%. The limit of quantification ranged between 0.1 and 1 μg/kg, which was sufficient to support surveillance monitoring. Lastly, the method was successfully used to detect residues of Veterinary drug in real samples. The dietary exposure risk was subsequently assessed using the results of the survey, indicating that the evaluated daily intake and percentage of acceptable daily intake were at toxicologically acceptable levels.
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Determination of 82 Veterinary Drugs in swine waste lagoon sludge by ultra-high performance liquid chromatography-tandem mass spectrometry.
Journal of chromatography. A, 2017Co-Authors: Ping Guo, Yawen Shan, Yingyu Wang, Tianhe Liu, Xi XiaAbstract:This work reports the development of a multi-residue method for the identification and quantification of 82 Veterinary Drugs belonging to different chemical classes in swine waste lagoon. The proposed method applies a solid-phase extraction procedure with Oasis PRiME HLB cartridges that combines isolation of the compounds and sample clean-up in a single step. Analysis is performed by ultra-high performance liquid chromatography-tandem mass spectrometry, in one single injection with a chromatographic run time of only 9.5min. Linearity was studied in the range between 1 and 500μgkg-1 using standards prepared both in pure solvent and in the presence of matrix, showing coefficients of determination higher than 0.99 for all the analytes except for cefapirin in matrix. The average recoveries were in the range of 60-110% for most of the compounds tested with inter-day relative standard deviations below 17%. More than 97% of the investigated compounds had less or equal to a 5μgkg-1 quantitation limit in the studied matrix. Finally, the method was used with success to detect and quantify Veterinary Drugs residues in real samples with sulfonamides, quinolones, and tetracyclines being the most frequently determined compound groups.
Mirjam Widmer - One of the best experts on this subject based on the ideXlab platform.
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development of an improved high resolution mass spectrometry based multi residue method for Veterinary Drugs in various food matrices
Analytica Chimica Acta, 2011Co-Authors: Anton Kaufmann, Patrick Butcher, Kathryn Maden, S Walker, Mirjam WidmerAbstract:Abstract Multi-residue methods for Veterinary Drugs or pesticides in food are increasingly often based on ultra performance liquid chromatography (UPLC) coupled to high resolution mass spectrometry (HRMS). Previous available time of flight (TOF) technologies, showing resolutions up to 15,000 full width at half maximum (FWHM), were not sufficiently selective for monitoring low residue concentrations in difficult matrices (e.g. hormones in tissue or antibiotics in honey). The approach proposed in this paper is based on a single stage Orbitrap mass spectrometer operated at 50,000 FWHM. Extracts (liver and kidney) which were produced according to a validated multi-residue method (time of flight detection based) could not be analyzed by Orbitrap because of extensive signal suppression. This required the improvement of established extraction and clean-up procedures. The introduced, more extensive deproteination steps and dedicated instrumental settings successfully eliminated these detrimental suppression effects. The reported method, covering more than 100 different Veterinary dugs, was validated according to the EU Commission Decision 2002/657/EEC. Validated matrices include muscle, kidney, liver, fish and honey. Significantly better performance parameters (e.g. linearity, reproducibility and detection limits) were obtained when comparing the new method with the older, TOF based method. These improvements are attributed to the higher resolution (50,000 versus 12,000 FWHM) and the superior mass stability of the of the Orbitrap over the previously utilized TOF instrument.
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quantitative multiresidue method for about 100 Veterinary Drugs in different meat matrices by sub 2 μm particulate high performance liquid chromatography coupled to time of flight mass spectrometry
Journal of Chromatography A, 2008Co-Authors: Anton Kaufmann, Patrick Butcher, Kathryn Maden, Mirjam WidmerAbstract:Abstract A quantitative multiresidue method covering more than 100 Veterinary Drugs, belonging to different drug families, has been developed. The proposed approach uses an liquid–liquid–solid extraction technique (bi-polarity extraction) which is capable in recovering polar, medium polar and apolar compounds. A thorough generic reversed phase solid-phase extraction (SPE) clean-up removes interfering proteins and provides clean and stable extracts. Dedicated rinsing steps are proposed to reduce analyte adsorption on glass walls and on precipitating proteins. The resulting extract is analyzed by ultra-performance liquid chromatography (UPLC) coupled to time of flight mass spectrometry (TOF). The method was validated according to the Commission Decision 2002/657/EEC. Validation coved the relevant meat matrices (muscle, kidney and liver).
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ultra performance liquid chromatography coupled to time of flight mass spectrometry uplc tof a novel tool for multiresidue screening of Veterinary Drugs in urine
Analytica Chimica Acta, 2007Co-Authors: Anton Kaufmann, Patrick Butcher, Kathryn Maden, Mirjam WidmerAbstract:A multiresidue method for the screening of Veterinary Drugs in urine with ultra-performance liquid chromatography (UPLC) coupled to time of flight mass spectrometry (TOF) is proposed. The method covers currently more than 100 analytes belonging to different families of Veterinary Drugs. Urine samples are simply diluted and injected unfiltered into the UPLC-TOF. The short run time permit high-throughput of large series under a routine environment. The suggested approach includes the detection of some metabolites which are relevant to the urine matrix. The paper discusses the usefulness of metabolites as additional confirmation criteria for positive findings and suggests a revisiting of the identification point system in the light of additional resolution, as provided by the TOF and the UPLC technology. The proposed multiresidue approach was further broadened by monitoring drug group specific collision induced fragments (CID). Examples show the monitoring of generic CID fragments typical for sulfonamides and penicillins.
Renato Zanella - One of the best experts on this subject based on the ideXlab platform.
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optimization of sample preparation by central composite design for multi class determination of Veterinary Drugs in bovine muscle kidney and liver by ultra high performance liquid chromatographic tandem mass spectrometry
Food Chemistry, 2018Co-Authors: Tiele M Rizzetti, Maiara P De Souza, Osmar D Prestes, Martha B Adaime, Renato ZanellaAbstract:Abstract In this study a simple and fast multi-class method for the determination of Veterinary Drugs in bovine liver, kidney and muscle was developed. The method employed acetonitrile for extraction followed by clean-up with EMR-Lipid® sorbent and trichloracetic acid. Tests indicated that the use of TCA was most effective when added in the final step of the clean-up procedure instead of during extraction. Different sorbents were tested and optimized using central composite design and the analytes determined by ultra-high-performance liquid chromatographic-tandem mass spectrometry (UHPLC-MS/MS). The method was validated according the European Commission Decision 2002/657 presenting satisfactory results for 69 Veterinary Drugs in bovine liver and 68 compounds in bovine muscle and kidney. The method was applied in real samples and in proficiency tests and proved to be adequate for routine analysis. Residues of abamectin, doramectin, eprinomectin and ivermectin were found in samples of bovine muscle and only ivermectin in bovine liver.
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optimization of sample preparation by central composite design for multi class determination of Veterinary Drugs in bovine muscle kidney and liver by ultra high performance liquid chromatographic tandem mass spectrometry
Food Chemistry, 2018Co-Authors: Tiele M Rizzetti, Maiara P De Souza, Osmar D Prestes, Martha B Adaime, Renato ZanellaAbstract:Abstract In this study a simple and fast multi-class method for the determination of Veterinary Drugs in bovine liver, kidney and muscle was developed. The method employed acetonitrile for extraction followed by clean-up with EMR-Lipid® sorbent and trichloracetic acid. Tests indicated that the use of TCA was most effective when added in the final step of the clean-up procedure instead of during extraction. Different sorbents were tested and optimized using central composite design and the analytes determined by ultra-high-performance liquid chromatographic-tandem mass spectrometry (UHPLC-MS/MS). The method was validated according the European Commission Decision 2002/657 presenting satisfactory results for 69 Veterinary Drugs in bovine liver and 68 compounds in bovine muscle and kidney. The method was applied in real samples and in proficiency tests and proved to be adequate for routine analysis. Residues of abamectin, doramectin, eprinomectin and ivermectin were found in samples of bovine muscle and only ivermectin in bovine liver.
