scholarly journals Determination of Florfenicol, Thiamfenicol and Chloramfenicol at Trace Levels in Animal Feed by HPLC–MS/MS

Antibiotics ◽  
2019 ◽  
Vol 8 (2) ◽  
pp. 59 ◽  
Author(s):  
Rosa Elvira Gavilán ◽  
Carolina Nebot ◽  
Ewelina Patyra ◽  
Beatriz Vazquez ◽  
Jose Manuel Miranda ◽  
...  
Keyword(s):  
Ethyl Acetate ◽  
Animal Feed ◽  
Simultaneous Detection ◽  
The European Union ◽  
European Regulation ◽  
Official Control ◽  
Liquid Chromatography Tandem Mass ◽  
Residue Levels ◽  
Low Levels

Administration of florfenicol and thiamfenicol through medicated feed is permitted within the European Union, always following veterinary prescription and respecting the withdrawal periods. However, the presence of low levels of florfenicol, thiamfenicol, and chloramfenicol in non-target feed is prohibited. Since cross-contamination can occur during the production of medicated feed and according to Annex II of the European Regulation 2019/4/EC, the control of residue levels of florfenicol and thiamfenicol in non-target feed should be monitored and avoided. Based on all the above, a sensitive and reliable method using liquid chromatography tandem mass spectrometry was developed for the simultaneous detection of chloramfenicol, florfenicol, and thiamfenicol at trace levels in animal feed. Analytes were extracted from minced feed with ethyl acetate. Then, the ethyl acetate was evaporated, the residue was resuspended in Milli-Q water and the extract filtered. The method was in-house validated at carryover levels, with concentration ranging from 100 to 1000 µg/kg. The validation was conducted following the European Commission Decision 2002/657/EC and all performance characteristics were successfully satisfied. The capability of the method to detect amfenicols at lower levels than any prior perspective regulation literature guarantees its applicability in official control activities. The developed method has been applied to non-compliant feed samples with satisfactory results.

scholarly journals Validated Method for Determination of Eight Banned Nitroimidazole Residues in Natural Casings by LC/MS/MS with Solid-Phase Extraction

2009 ◽  
Vol 92 (2) ◽  
pp. 612-621 ◽  
Author(s):  
Hanwen Sun ◽  
Fengchi Wang ◽  
Lianfeng Ai ◽  
Chunhai Guo ◽  
Ruichun Chen
Keyword(s):  
Solid Phase Extraction ◽  
Ethyl Acetate ◽  
Solid Phase ◽  
Multiple Reaction Monitoring ◽  
Phase Extraction ◽  
The European Union ◽  
Detection Capability ◽  
Accuracy And Precision ◽  
Liquid Chromatography Tandem Mass

Abstract A sensitive method based on solid-phase extraction-liquid chromatography-tandem mass spectrometry interfaced with electrospray ionization (SPE-LC-MS/MS-ESI) was developed for the simultaneous determination of 8 banned nitroimidazole (NOZ) drugs including metronidazole (MNZ), ronidazole (RNZ), dimetridazole (DMZ), tinidazole, ornidazole, secnidazole, metronidazole-OH (MNZOH, the metabolite of MNZ), and 2-hydroxymethyl-1-methyl-5-nitroimidazole (HMMNI, the metabolite of RNZ and DMZ) in natural casings. After extraction with ethyl acetate and evaporation, the NOZs were reconstituted in ethyl acetate and purified on a strong cation-exchange SPE column, and then LC/MS/MS analysis was performed by positive ESI applying multiple reaction monitoring of 2 transition reactions for each compound. The method was validated according to the European Union requirements (Commission Decision 2002/657/EC). Specificity, linearity, decision limit (CC), detection capability (CC), accuracy, and precision were determined. Average recoveries of the 8 NOZs from natural animal casing fortified at 3 levels (0.1, 0.5, and 1 g/kg) ranged from 87.3 to 116.5. The calculated CC for NOZs ranged from 0.029 to 0.049 g/kg, and CC ranged from 0.049 to 0.083 g/kg. Repeatability was in the range of 3.3510.1, and within-laboratory reproducibility was <10.3.

scholarly journals Multi LC-MS/MS and LC-HRMS Methods for Determination of 24 Mycotoxins including Major Phase I and II Biomarker Metabolites in Biological Matrices from Pigs and Broiler Chickens

Toxins ◽  
2019 ◽  
Vol 11 (3) ◽  
pp. 171 ◽  
Author(s):  
Marianne Lauwers ◽  
Siegrid De Baere ◽  
Ben Letor ◽  
Michael Rychlik ◽  
Siska Croubels ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Phase I ◽  
Ethyl Acetate ◽  
Broiler Chickens ◽  
High Resolution Mass Spectrometry ◽  
Screening Study ◽  
Liquid Chromatography Tandem Mass ◽  
Alternaria Mycotoxins ◽  
Phase I And Ii

A reliable and practical multi-method was developed for the quantification of mycotoxins in plasma, urine, and feces of pigs, and plasma and excreta of broiler chickens using liquid chromatography–tandem mass spectrometry. The targeted mycotoxins belong to the regulated groups, i.e., aflatoxins, ochratoxin A and Fusarium mycotoxins, and to two groups of emerging mycotoxins, i.e., Alternaria mycotoxins and enniatins. In addition, the developed method was transferred to a LC-high resolution mass spectrometry instrument to qualitatively determine phase I and II metabolites, for which analytical standards are not always commercially available. Sample preparation of plasma was simple and generic and was accomplished by precipitation of proteins alone (pig) or in combination with removal of phospholipids (chicken). A more intensive sample clean-up of the other matrices was needed and consisted of a pH-dependent liquid–liquid extraction (LLE) using ethyl acetate (pig urine), methanol/ethyl acetate/formic acid (75/24/1, v/v/v) (pig feces) or acetonitrile (chicken excreta). For the extraction of pig feces, additionally a combination of LLE using acetone and filtration of the supernatant on a HybridSPE-phospholipid cartridge was applied. The LC-MS/MS method was in-house validated according to guidelines defined by the European and international community. Finally, the multi-methods were successfully applied in a specific toxicokinetic study and a screening study to monitor the exposure of individual animals.

Application of the CEN/ISO Standard for Phytase Activity Measurements to a New Phytase Product: Determination of a Robust Conversion Factor by an Interlaboratory Study for Screening Feed Samples

2019 ◽  
Vol 102 (6) ◽  
pp. 1808-1813
Author(s):  
María José González de la Huebra ◽  
Piotr Robouch ◽  
Håkan Emteborg ◽  
Stefano Bellorini ◽  
Aneta Cizek-Stroh ◽  
...  
Keyword(s):  
Conversion Factor ◽  
Feed Additives ◽  
Phytase Activity ◽  
Feed Additive ◽  
The European Union ◽  
Iso Standard ◽  
Official Control ◽  
Activity Measurements ◽  
Feed Samples

Abstract Background: Phytase-based preparations are important feed additives currently authorised in the European Union (EU). The European Standard (EN) and International Organization for Standardization (ISO) standard 30024 describes a harmonized method for the determination of phytase activity and is fit-for-purpose for official control of a group of phytase products. However, it is not suitable for the determination of the phytase activity of a new feed additive encoded as 4a16 in the EU Register of Feed Additives, to which a slightly different phytase activity definition has been attributed. Objective: To establish a robust conversion factor to support official control laboratories that apply the EN ISO method when monitoring feed products containing 4a16. Methods: The phytase activity of test materials was determined by the participants using the EN ISO and/or the “applicant” methods. Results: Robust relative SDs for repeatability and for reproducibility of the methods applied for the determination of the phytase activity in the materials containing the 4a16 feed additive ranged from 2.6 to 22% (EN ISO method) and from 2.4 to 39% (applicant method). Conclusions: The data obtained confirmed the performance characteristics published for other phytase-based feeds in the related standard methods. These results allowed us to estimate a factor of 2.68 to convert phytase activities measured with the EN ISO method into the enzyme activity measured with the applicant method. Highlights: The obtained conversion factor will allow EU official laboratories to screen feed samples supplemented with the 4a16 phytase by applying EN ISO Standard 30024.

Application of the CEN/ISO Standard for Phytase Activity Measurements to a New Phytase Product: Determination of a Robust Conversion Factor by an Interlaboratory Study for Screening Feed Samples

2019 ◽  
Vol 102 (6) ◽  
pp. 1808-1813
Author(s):  
María José González de la Huebra ◽  
Piotr Robouch ◽  
Håkan Emteborg ◽  
Stefano Bellorini ◽  
Aneta Cizek-Stroh ◽  
...  
Keyword(s):  
Conversion Factor ◽  
Feed Additives ◽  
Phytase Activity ◽  
Feed Additive ◽  
The European Union ◽  
Iso Standard ◽  
Official Control ◽  
Activity Measurements ◽  
Feed Samples

Background: Phytase-based preparations are important feed additives currently authorised in the European Union (EU). The European Standard (EN) and International Organization for Standardization (ISO) standard 30024 describes a harmonized method for the determination of phytase activity and is fit-for-purpose for official control of a group of phytase products. However, it is not suitable for the determination of the phytase activity of a new feed additive encoded as 4a16 in the EU Register of Feed Additives, to which a slightly different phytase activity definition has been attributed. Objective: To establish a robust conversion factor to support official control laboratories that apply the EN ISO method when monitoring feed products containing 4a16. Methods: The phytase activity of test materials was determined by the participants using the EN ISO and/or the “applicant” methods. Results: Robust relative SDs for repeatability and for reproducibility of the methods applied for the determination of the phytase activity in the materials containing the 4a16 feed additive ranged from 2.6 to 22% (EN ISO method) and from 2.4 to 39% (applicant method). Conclusions: The data obtained confirmed the performance characteristics published for other phytase-based feeds in the related standard methods. These results allowed us to estimate a factor of 2.68 to convert phytase activities measured with the EN ISO method into the enzyme activity measured with the applicant method. Highlights: The obtained conversion factor will allow EU official laboratories to screen feed samples supplemented with the 4a16 phytase by applying EN ISO Standard 30024.

scholarly journals New Method for Simultaneous Determination of Microcystins and Cylindrospermopsin in Vegetable Matrices by SPE-UPLC-MS/MS

Toxins ◽  
2018 ◽  
Vol 10 (10) ◽  
pp. 406 ◽  
Author(s):  
Leticia Díez-Quijada ◽  
Remedios Guzmán-Guillén ◽  
Ana Prieto Ortega ◽  
María Llana-Ruíz-Cabello ◽  
Alexandre Campos ◽  
...  
Keyword(s):  
Chemical Structure ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Simultaneous Detection ◽  
Ultra Performance Liquid Chromatography ◽  
Limit Of Quantification ◽  
Worldwide Distribution ◽  
Exposure Estimation ◽  
Liquid Chromatography Tandem Mass

Cyanotoxins are a large group of noxious metabolites with different chemical structure and mechanisms of action, with a worldwide distribution, producing effects in animals, humans, and crop plants. When cyanotoxin-contaminated waters are used for the irrigation of edible vegetables, humans can be in contact with these toxins through the food chain. In this work, a method for the simultaneous detection of Microcystin-LR (MC-LR), Microcystin-RR (MC-RR), Microcystin-YR (MC-YR), and Cylindrospermopsin (CYN) in lettuce has been optimized and validated, using a dual solid phase extraction (SPE) system for toxin extraction and ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) for analysis. Results showed linear ranges (5–50 ng g−1 f.w.), low values for limit of detection (LOD) (0.06–0.42 ng g−1 f.w.), and limit of quantification (LOQ) (0.16–0.91 ng g−1 f.w.), acceptable recoveries (41–93%), and %RSDIP values for the four toxins. The method proved to be robust for the three variables tested. Finally, it was successfully applied to detect these cyanotoxins in edible vegetables exposed to cyanobacterial extracts under laboratory conditions, and it could be useful for monitoring these toxins in edible vegetables for better exposure estimation in terms of risk assessment.

Determination of Eight Sulfonylurea Herbicide Residues by LC/MS/MS Using a Sample Separation Technique with Ethyl Acetate

2019 ◽  
Vol 102 (1) ◽  
pp. 239-245
Author(s):  
Eleftheria Bempelou ◽  
Petros Kappatos ◽  
Konstantinos Liapis
Keyword(s):  
Ethyl Acetate ◽  
Correlation Coefficients ◽  
Analytical Techniques ◽  
Growth Stages ◽  
Quechers Method ◽  
Validation Criteria ◽  
Maximum Residue Limits ◽  
Low Levels ◽  
Sample Separation

Abstract Background: Sulfonylureas are an important group of systemic herbicides mainly used for the control of weeds in cereals and other crops in early growth stages of their cultivations. Sulfonylureas are characterized by their broad spectrum weed control and their good crop selectivity. Objective: In the present study, the determination of eight sulfonylureas has been tested in wheat flour by applying the SweEt multiresidue method modified for dry products. Method: The method involves sample preparation with extraction with ethyl acetate (EEA) and determination of the analytes with LC/MS/MS-electrospray ionization. Its performance was compared with the quick, easy, cheap, effective, rugged, and safe (QuEChERS) method. Both methods were validated in three fortification levels according to European Union requirements. Results: The proposed method gave acceptable results as far as validation criteria are concerned, while QuEChERS did not result in successful recoveries in the lowest validation level, which is equal to the respective maximum residue limits (MRLs). Conclusions: The obtained results showed that the tested method showed good separation, sensitivity, linearity, precision, and accuracy for quantitative and qualitative analysis of sulfonylurea herbicides in cereals at low levels, as required by legislation. The analytical techniques were successfully applied to different samples of cereals, and no residues were determined above the reporting limit, as established at the lowest concentration level of each analyte being validated with acceptable accuracy. Highlights: Low recoveries for QuEChERS in the concentrations equal to the MRL. Acceptable recoveries for the EEA method in all fortification levels. Correlation coefficients above 0.99. Positive findings only with EEA in real samples.

scholarly journals Comparative Analysis of Verification Parameters of Event-Specific Methods in GMO Maize

2018 ◽  
Vol 2 (1) ◽  
pp. 8
Author(s):  
Anesa Ahatović ◽  
Adaleta Durmić-Pašić
Keyword(s):  
Limit Of Detection ◽  
Certified Reference Materials ◽  
Simultaneous Detection ◽  
Specific Marker ◽  
The European Union ◽  
Gm Crop ◽  
Gm Maize ◽  
Absolute Limit ◽  
Multiplex Reaction

The second most dominant genetically modified (GM) crop is maize. Increasing number of GM maize events puts significant pressure on GMO testing laboratories to achieve the level of competence necessary to fulfill legal requirements. In the European Union, Polymerase Chain Reaction (PCR) is the method of choice for identification and quantification of GMOs. We performed verification of validated methods for identification of four GM maize events. Additionaly we aimed to explore the option of designing a method for simultaneous detection of these events in a multiplex PCR reaction. DNA was extracted from certified reference materials (CRM) using validated CTAB extraction protocol. Concentration of DNA was measured using Qubit dsDNA Broad Range Assay. Amplification of taxon specific marker for maize and all event-specific methods was performed according to the JRC Compendium of Reference Methods for GMO Analysis. Absolute limit of detection (LODabs) was determined for taxon specific and four event specific RealTime PCR based methods. DNA extracted from CRMs showed sufficient concentration for downstream analyses and preparation of dilutions for determination of LODabs. Determined LODabs for all tested methods meet acceptance criteria. As expected, the methods performance with respect to the repeatability and precision decline with the decrease in concentration of the target. Event-specific GA21 and NK603 methods show high Ct values at the determined LODabs. However, by adjusting the concentrations of primers and probes sensitivity of these two methods should be improved. Considering that the amplicons for all five methods are quite short (<120 bp) optimization of multiplex reaction conditions for simultaneous amplification should be feasible

scholarly journals Distribution, source apportionment and health risk assessment of organochlorine pesticides in drinking groundwater

2021 ◽  
Author(s):  
John A. O. Oyekunle ◽  
Abiodun O. Adegunwa ◽  
Odunayo T. Ore
Keyword(s):  
Risk Assessment ◽  
Health Risk ◽  
Organochlorine Pesticides ◽  
Health Risk Assessment ◽  
The European Union ◽  
Groundwater Samples ◽  
Maximum Residue Levels ◽  
Residue Levels ◽  
High Concentrations

Abstract Groundwater samples of Ile-Ife, Osun State, Nigeria were investigated for their organochlorine pesticides (OCPs) levels. Probable sources of the OCPs and health risks associated with their consumption along with the water were determined in order to establish the potability of the groundwater samples. Quantitative determination of the OCPs was carried out by Gas Chromatography coupled with Electron Capture Detector (GC-ECD) after liquid-liquid extraction with dichloromethane (DCM). Results indicated that all the analyzed OCPs except p,p'-dichlorodiphenylethane were detected with high concentrations in the groundwater. Heptachlor (14.60±3.60 µg L-1) and methoxychlor (12.60±2.20 µg L-1) showed dominant concentrations that were higher than 0.02 ng L-1 maximum residue levels (MRLs) recommended by the European Union. Levels of the OCPs in the samples followed the decreasing trend: cyclodienes > diclorophehylethanes > chlorinated cyclohexanes, while the predominant source of the analyzed pesticides could be ascribed to aerial transportation from fresh applications in homes within the community. The carcinogenic health risk assessment also revealed consistent higher values of HQ and CR in children as opposed to adults, indicating that children are the more vulnerable population to the analyzed environmental contaminants.

scholarly journals Simultaneous Determination of Ergot Alkaloids in Swine and Dairy Feeds Using Ultra High-Performance Liquid Chromatography-Tandem Mass Spectrometry

Toxins ◽  
2021 ◽  
Vol 13 (10) ◽  
pp. 724
Author(s):  
Saranya Poapolathep ◽  
Narumol Klangkaew ◽  
Zhaowei Zhang ◽  
Mario Giorgi ◽  
Antonio Francesco Logrieco ◽  
...  
Keyword(s):  
High Performance ◽  
Ergot Alkaloids ◽  
The European Union ◽  
Chromatography Tandem Mass Spectrometry ◽  
Occurrence Data ◽  
Performance Recovery ◽  
Liquid Chromatography Tandem Mass ◽  
Swine Feed ◽  
Feed Samples

Ergot alkaloids (EAs) are mycotoxins mainly produced by the fungus Claviceps purpurea. EAs are known to affect the nervous system and to be vasoconstrictors in humans and animals. This work presents recent advances in swine and dairy feeds regarding 11 major EAs, namely ergometrine, ergosine, ergotamine, ergocornine, ergocryptine, ergocristine, ergosinine, ergotaminine, ergocorninine, ergocryptinine, and ergocristinine. A reliable, sensitive, and accurate multiple mycotoxin method, based on extraction with a Mycosep 150 multifunctional column prior to analysis using UHPLC-MS/MS, was validated using samples of swine feed (100) and dairy feed (100) for the 11 targeted EAs. Based on the obtained validation results, this method showed good performance recovery and inter-day and intra-day precision that are in accordance with standard criteria to ensure reliable occurrence data on EA contaminants. More than 49% of the swine feed samples were contaminated with EAs, especially ergocryptine(-ine) (40%) and ergosine (-ine) and ergotamine (-ine) (37%). However, many of the 11 EAs were not detectable in any swine feed samples. In addition, there were contaminated (positive) dairy feed samples, especially for ergocryptine (-ine) (50%), ergosine (-ine) (48%), ergotamine (-ine), and ergocristine (-ine) (49%). The mycotoxin levels in the feed samples in this study almost complied with the European Union regulations.

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