Quick and high-throughput quantification of ß-agonist residues in bovine liver, meat, milk, kidney, poultry, and egg using dispersive solid phase extraction.

A reliable liquid chromatography coupled to quadrupole-Orbitrap high-resolution mass spectrometry (LC-Q-Orbitrap HRMS) method was developed for the simultaneous identification and quantification of 13 ß-agonist residues in bovine liver, meat, milk, kidney, poultry, and egg. Dispersive-solid phase extraction (d-SPE) using acetonitrile (ACN) was used to prepare the samples. The analyte in the extracts was separated on a reversed-phase Accucore aQ (50 mm × 2.1 mm, 2.6 µm) using a mobile phase of an aqueous solution containing 2 mM ammonium acetate and acetonitrile (ACN) 0.1 % formic acid. The method was validated in accordance with Commission Implementing Regulation (CIR) EU 2021/808 at six different concentrations ranging from 0.1 to 5 µg/kg. The mean recoveries ranged from 65 to 94 %, while repeatability and reproducibility values were all below 13 %. The linearity, as correlation coefficients (R2) ranged from 0.9955 to 0.9999. The decision limit (CCα) and detection capability (CCß) ranges were 0.11-0.13 µg/kg and 0.12-0.15 µg/kg, respectively. The limits of detection (LOD) and limits of quantification (LOQ) were in the range of 0.004-0.048 µg/kg and 0.010-0.075 µg/kg, respectively. Of the 180 samples that were collected from local markets in Egypt, 21.11 % had ß-agonist residues. The mean concentration (µg/kg) and detection frequency (%) of the most frequently found ß-agonist in the samples were as follows: terbutaline (2.63 µg/kg and 90 %), ractopamine (5.14 µg/kg and 23.3 %). The method's applicability was verified by successfully completing two rounds of proficiency testing (PT).

[Research status and rapid detection methods of antibiotic residues in agricultural products]. / å†œäº§å“æŠ—ç”Ÿç´ æ®‹ç•™çŽ°çŠ¶åŠå¿«é€Ÿæ£€æµ‹æ–¹æ³•ç ”ç©¶è¿›å±•.

Antibiotics are widely utilized in agriculture for the prevention and treatment of animal diseases. How-ever, the abuse and overuse of antibiotics progressively increase the risks of antibiotic residues and antibiotic resis-tance. The bioaccumulation and biomagnification of antibiotics through food chains will negatively affect ecological safety, and finally threaten human health. There are many shortages of traditional antibiotic detection techniques, such as complex procedures, complicated operation and time consuming, and thus are difficult to meet the demand of instant, efficient and accurate on-site detection. Therefore, it is crucial to develop rapid detection techniques of antibiotics to manage the application of antibiotics in agriculture. We reviewed the utilization, and management of antibiotics in animal husbandry, residual characteristics, and potential hazards of antibiotics in agricultural products, summarized the advancements in rapid detection techniques of antibiotics in agricultural products over the past five years, compared the advantages and disadvantages of different rapid detection techniques, and prospected the future development in this area. This review would provide a valuable reference to the control and point-of-care test of antibiotics in agricultural products.

Simultaneous determination of 68 antimicrobial compounds in pigs oral fluid by ultra-high performance liquid chromatography-tandem mass spectrometry.

Improper use of antimicrobials in veterinary medicine can lead to residues in food of animal origin. Post-mortem monitoring of antibiotics in animal products is carried out as part of official EU programmes on food safety and consumer health. Oral fluid testing is a promising surveillance method to monitor appropriate treatment in pigs and to avoid residues in edible tissues. Oral fluid analysis can be implemented in an antibiotic residue control programme, thus preventing economic losses due to meat disposal as a result of drug detection in tissues after the withdrawal period. An analytical method was developed for the analysis of 68 compounds from 12 groups (penicillins, cephalosporins, sulfonamides, macrolides, fluoroquinolones, tetracyclines, aminoglycosides, pleuromutilins, diaminopyrimidines, lincosamides, polypeptides and sulfones) in pig oral fluid. Extraction of antibacterials was performed with 0.5 % formic acid. Analyses were carried out by ultra-high performance liquid chromatography with triple quadrupole mass spectrometry (UHPLC-MS/MS) detection. The chromatographic separation was achieved on a Zorbax analytical column (2.1 × 50 mm) with a mobile phase consisting of acetonitrile and heptafluorobutyric acid (HFBA). The total run time was 7 min. The method was validated as a confirmatory method according to the Commission Implementing Regulation (EU) 2021/808. The reliability of the method was verified by testing real samples from pig farms.

Rapid and Online Microvolume Flow-Through Dialysis Probe for Sample Preparation in Veterinary Drug Residue Analysis.

A rapid and online microvolume flow-through dialysis probe designed for sample preparation in the analysis of veterinary drug residues is introduced. This study addresses the need for efficient and green sample preparation methods that reduce chemical waste and reagent use. The dialysis probe integrates with liquid chromatography and mass spectrometry (LC-MS) systems, facilitating automated, high-throughput analysis. The dialysis method utilizes minimal reagent volumes per sample, significantly reducing the generation of solvent waste compared to traditional sample preparation techniques. Several veterinary drugs were spiked into tissue homogenates and analyzed to validate the probe's efficacy. A diagnostic sensitivity of >97% and specificity of >95% were obtained for this performance evaluation. The results demonstrated the effective removal of cellular debris and particulates, ensuring sample integrity and preventing instrument clogging. The automated dialysis probe yielded recovery rates between 27 and 77% for multiple analytes, confirming its potential to streamline veterinary drug residue analysis, while adhering to green chemistry principles. The approach highlights substantial improvements in both environmental impact and operational efficiency, presenting a viable alternative to conventional sample preparation methods in regulatory and research applications.

State-of-the-art nanosensors and kits for the detection of antibiotic residues in milk and dairy products.

Antibiotic resistance is increasingly seen as a future concern, but antibiotics are still commonly used in animals, leading to their accumulation in humans through the food chain and posing health risks. The development of nanomaterials has opened up possibilities for creating new sensing strategies to detect antibiotic residues, resulting in the emergence of innovative nanobiosensors with different benefits like rapidity, simplicity, accuracy, sensitivity, specificity, and precision. Therefore, this comprehensive review provides pertinent and current insights into nanomaterials-based electrochemical/optical sensors for the detection of antibitic residues (ANBr) across milk and dairy products. Here, we first discuss the commonly used ANBs in real products, the significance of ANBr, and also their binding/biological properties. Then, we provide an overview of the role of using different nanomaterials on the development of advanced nanobiosensors like fluorescence-based, colorimetric, surface-enhanced Raman scattering, surface plasmon resonance, and several important electrochemical nanobiosensors relying on different kinds of electrodes. The enhancement of ANB electrochemical behavior for detection is also outlined, along with a concise overview of the utilization of (bio)recognition units. Ultimately, this paper offers a perspective on the future concepts of this research field and commercialized nanomaterial-based sensors to help upgrade the sensing techniques for ANBr in dairy products.

Efficient porphyrin integrated UiO-66 probes for ratiometric fluorescence sensing of antibiotic residues in milk.

Dual-emissive fluorescence probes were designed by integrating porphyrin into the frameworks of UiO-66 for ratiometric fluorescence sensing of amoxicillin (AMX). Porphyrin integrated UiO-66 showed dual emission in the blue and red region. AMX resulted in the quenching of blue fluorescence component, attributable to the charge neutralization and hydrogen bonds induced energy transfer. AMX was detected using (F438/F654) as output signals. Two linear relationships were observed (from 10 to 1000 nM and 1 to 100 µM), with a limit of detection of 27 nM. The porphyrin integrated UiO-66 probe was used to detect AMX in practical samples. This work widens the road for the development of dual/multiple emissive fluorescence sensors for analytical applications, providing materials and theoretical supporting for food, environmental, and human safety.

Residue, distribution and depletion of fluralaner in egg following a single intravenous and transdermal administration in healthy shaver hens: fluralaner residue in egg.

The demand for the use of fluralaner in an extra label manner is increasing due to lack of efficacious treatment to combat mites and bed bugs in the poultry industry in the United States. Fluralaner residue data in eggs is lacking and residues might cause risks to human health. The present study aimed to determine the depletion profiles of fluralaner in eggs and estimate the drug withdrawal interval in whole eggs by adopting the US Food and Drug administration tolerance limit method with single intravenous (0.5 mg/kg) or transdermal administration (average 58.7 mg/kg) in healthy shaver hens. Hens were treated intravenously or trans-dermally with fluralaner. The eggs were collected daily for 28 d for intravenous treated and for 40 d from the transdermal route group. Fluralaner concentrations in yolk and albumen were determined by mass spectrometry. The greater percentage of fluralaner was observed in yolk when compared to the albumen for both administration routes. Noncompartmental analysis was used to calculate the pharmacokinetic parameters in yolk, albumen and whole egg. The longest apparent half-life confirmed in yolk was 3.7 d for intravenous and 14.3 d for the transdermal route. The withdrawal intervals in whole egg for fluralaner following the intravenous and transdermal administration were 7 d and 81 d, respectively, with maximum residue limits (1.3 µg/g) at 13 d and 171 d, respectively, based on the limit of quantification (0.4 µg/g) from the analytical assay reported by EMA and APVMA.

A new spectral simulating method based on near-infrared hyperspectral imaging for evaluation of antibiotic mycelia residues in protein feeds.

Antibiotic mycelia residues (AMRs) contain antibiotic residues. If AMRs are ingested in excess by livestock, it may cause health problems. To address the current problem of unknown pixel-scale adulteration concentration in NIR-HSI, this paper innovatively proposes a new spectral simulation method for the evaluation of AMRs in protein feeds. Four common protein feeds (soybean meal (SM), distillers dried grains with solubles (DDGS), cottonseed meal (CM), and nucleotide residue (NR)) and oxytetracycline residue (OR) were selected as study materials. The first step of the method is to simulate the spectra of pixels with different adulteration concentrations using a linear mixing model (LMM). Then, a pixel-scale OR quantitative model was developed based on the simulated pixel spectra combined with local PLS based on global PLS scores (LPLS-S) (which solves the problem of nonlinear distribution of the prediction results due to the 0%-100% content of the correction set). Finally, the model was used to quantitatively predict the OR content of each pixel in hyperspectral image. The average value of each pixel was calculated as the OR content of that sample. The implementation of this method can effectively overcome the inability of PLS-DA to achieve qualitative identification of OR in 2%-20% adulterated samples. In compared to the PLS model built by averaging the spectra over the region of interest, this method utilizes the precise information of each pixel, thereby enhancing the accuracy of the detection of adulterated samples. The results demonstrate that the combination of the method of simulated spectroscopy and LPLS-S provides a novel method for the detection and analysis of illegal feed additives by NIR-HSI.

Search for Biomarkers for the LC-ESI-QqQ Determination of Phenoxymethylpenicillin Treatment in Raw or Cooked Chicken Meat Samples.

The high standards required for food safety make it necessary to trace unambiguously raw or cooked food products coming from medicated animals. Nevertheless, considering the lability of ß-lactams and their degradation, the detection of the presence of antibiotics in meat either raw or submitted to a cooking process is not easily affordable. To achieve this goal, an evaluation of the effect of common domestic cooking procedures, such as boiling and grilling, on the fate of phenoxymethylpenicillin (PENV) residues was performed. Finally, in this work, the penilloic acid from PENV (MET02) and the corresponding penicilloic acid (PENV-HYDRO) are suggested as biomarkers. These compounds present the highest relative abundances 5 days after the treatment was stopped (5PT) and show enough thermal stability to be considered suitable biomarker candidates for the pharmacological treatment instead of the parent compound. Nevertheless, the peaks corresponding to MET02 are significantly more intense than those for PENV-HYDRO, which makes preferential the use of MET02 to perform the control of samples.

A novel electrochemical sensor for the detection of metronidazole residues in food samples.

The widespread use and misuse of antibiotics in pharmaceuticals and animal farming has resulted in their accumulation in food sources and the environment, posing significant threats to human health, the environment, and the global economy. In this study, we have developed a hypersensitive, and ultra-selective electrochemical sensor, the first of its kind, by integrating a thermally annealed gold-silver alloy nanoporous matrix (TA-Au-Ag-ANpM) with reduced graphene oxide (r-GO) and poly(glycine) at the surface of a glassy carbon electrode (GCE). This sensor aims to detect life-threatening metronidazole (MTZ) residues in food samples. TA-Au-Ag-ANpM/r-GO/poly(glycine)/GCE was thoroughly characterized using a range of analytical techniques, including UV-Vis, FT-IR, XRD, SEM, and EDX. Furthermore, its electrochemical properties were investigated by cyclic voltammetry (CV), square wave voltammetry (SWV), and electrochemical impedance spectroscopy (EIS). The sensor exhibited outstanding performance, with a broad linear range of 2.0 pM-410 µM. The limits of detection (LOD) and quantification (LOQ) were determined to be 0.0312 pM and 0.104 pM, respectively. The TA-Au-Ag-ANpM/r-GO/poly(glycine)/GCE exhibited exceptional reproducibility, repeatability, stability, and resistance to interferences. Moreover, the sensor demonstrated outstanding performance in detecting MTZ residues in milk powder, pork, and chicken meat samples, achieving very good recoveries (96.9%-101.4%) with a relative standard deviation (RSD) below 5%. This performance highlights the potential for practical applications in food safety and quality monitoring. Therefore, the developed sensor contributes to the advancement of electrochemical sensing technology and its application in ensuring food safety and integrity by combating antibiotic residues.

Development of a monoclonal antibody-based time-resolved fluorescence immunochromatographic assay strip for sensitively detecting florfenicol residues in milk and eggs: Theoretical chemical insights into unexpected high specificity.

Florfenicol (FF), with its broad-spectrum antibacterial activity, is frequently abused in the livestock and poultry industries and has aroused the growing public concern. Owing to structural similarities and varying maximum residue limits between florfenicol and other chloramphenicol (CAP)-type antibiotics, including thiamphenicol (TAP) and chloramphenicol (CAP), there is an urgent need for a rapid and effective immunoassay method to distinguish them, in order to minimize the risk of false positives. Fortunately, a highly specific monoclonal antibody (mAb), named as SF11, has been developed using hybridoma technology. Molecular simulations have revealed that the mAb SF11's specificity in recognizing florfenicol stems from the π-π stacking interaction between florfenicol and the mAb SF11 binding pocket. Using this highly specific mAb, a sensitive time-resolved fluorescence immunochromatographic assay (TRFICA) strip for rapid florfenicol detection has been developed. Under optimal conditions, this TRFICA demonstrated good analytical performance for the detection of florfenicol in milk and eggs samples, with the half-maximal inhibition concentration (IC50) values of 1.89 and 2.86 ng mL-1, the limit of detection (LOD) of 0.23 and 0.48 ng mL-1, the cut-off values of 62.50 and 31.25 ng mL-1, and the testing time of approximately thirteen minutes. Spiked recoveries in the milk and eggs samples ranged from 104.7 % to 112.3 % and 95.3 % to 116.4 %, respectively, with no obvious cross-reactions with the other analogues observed. The TRFICA results correlated well with those of high-performance liquid chromatography tandem mass spectrometry (HPLC-MS/MS) for real samples, indicating that the developed TRFICA method was sensitive, accurate and adapted for the rapid determination of florfenicol in milk and egg samples.

Solid phase extraction technology combined with UPLC-MS/MS: a method for detecting 20 ß-lactamase antibiotics traces in goat's milk.

We develop and validate a method for the rapid determination and identification of 20 ß-lactamase antibiotics traces in goat's milk by combining the solid phase extraction technology with ultra-high performance liquid chromatography-tandem mass spectrometry. Goat milk samples were extracted with acetonitrile twice. The supernatant was then extracted and cleaned by solid-phase extraction using divinylbenzene and N-vinylpyrrolidone copolymer. The method was validated, with limits of quantification (LOQs) of 0.3 µg kg-1, specificities of 1/3 LOQ, linearities (R2) > 0.99, recoveries of 80-110%, repeatabilities <10.0%, and intermediate precisions <10.0%. The developed method was suitable for the routine analysis of ß-lactamase antibiotics residues in goat's milk and was used to test 76 goat milk samples produced in China.

[Simultaneous determination of 31 banned veterinary drugs during egg-laying period in poultry eggs by ultra performance liquid chromatography-tandem mass spectrometry].

The consumption of poultry eggs has increased in recent years owing to the abundance of production and improvements in living standards. Thus, the safety requirements of poultry eggs have gradually increased. At present, few reports on analytical methods to determine banned veterinary drugs during egg-laying period in poultry eggs have been published. Therefore, establishing high-throughput and efficient screening methods to monitor banned veterinary drugs during egg-laying period is imperative. In this study, an analytical method based on ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) combined with QuEChERS-based techniques was developed for the simultaneous determination of 31 banned veterinary drugs encompassing nine drug classes (macrolides, antipyretic and analgesic drugs, sulfonamides, antibacterial synergists, anticoccidials, antinematodes, quinolones, tetracyclines, amphenicols) in different types of poultry eggs. The main factors affecting the response, recovery, and sensitivity of the method, such as the extraction solvent, purification adsorbent, LC separation conditions, and MS/MS parameters, were optimized during sample pretreatment and instrumental analysis. The 31 veterinary drug residues in 2.00 g eggs were extracted with 2 mL of 0.1 mol/L ethylene diamine tetraacetic acid disodium solution and 8 mL 3% acetic acid acetonitrile solution, and salted out with 2 g of sodium chloride. After centrifugation, 5 mL of the supernatant was cleaned-up using the QuEChERS method with 100 mg of octadecylsilane-bonded silica gel (C18), 50 mg of N-propylethylenediamine (PSA), and 50 mg of NH2-based sorbents. After nitrogen blowing and redissolution, the 31 target analytes were separated on a Waters CORTECS UPLC C18 analytical chromatographic column (150 mm×2.1 mm, 1.8 µm) at a flow rate, column temperature, and injection volume of 0.4 mL/min, 30 ℃, and 5 µL, respectively. Among these analytes, 26 analytes were acquired in dynamic multiple reaction monitoring (MRM) mode under positive electrospray ionization (ESI+) conditions using (A) 5 mmol/L ammonium acetate (pH 4.5) and (B) acetonitrile as mobile phases. The gradient elution program was as follows: 0-2.0 min, 12%B-30%B; 2.0-7.5 min, 30%B-50%B; 7.5-10.0 min, 50%B; 10.0-10.1 min, 50%B-100%B; 10.1-12.0 min, 100%B; 12.0-12.1 min, 100%B-12%B; The five other target analytes were acquired in MRM mode under negative electrospray ionization (ESI-) conditions using (A) H2O and (B) acetonitrile as mobile phases. The gradient elution program was as follows: 0-2.0 min, 12%B-40%B; 2.0-6.0 min, 40%B-80%B; 6.0-6.1 min, 80%B-100%B; 6.1-8.0 min, 100%B; 8.0-8.1 min, 100%B-12%B. Matrix-matched external standard calibration was used for quantification. The results showed that all the compounds had good linear relationships within their respective ranges, with correlation coefficients of >0.99. The limits of detection (LODs) and quantitation (LOQs) were 0.3-3.0 µg/kg and 1.0-10.0 µg/kg, respectively. The average recoveries of the 31 banned veterinary drugs spiked at three levels (LOQ, maximum residue limit (MRL), and 2MRL) in poultry eggs ranged from 61.2% to 105.7%, and the relative standard deviations (RSDs) ranged from 1.8% to 17.6%. The developed method was used to detect and analyze banned veterinary drugs in 30 commercial poultry egg samples, including 20 eggs, 5 duck eggs, and 5 goose eggs. Enrofloxacin was detected in one egg with a content of 12.3 µg/kg. The proposed method is simple, economical, practical, and capable of the simultaneous determination of multiple classes of banned veterinary drugs in poultry eggs.

[Determination of 12 prohibited veterinary drug residues in pig urine by ultra high performance liquid chromatography-tandem mass spectrometry].

A method was established for the simultaneous detection of 12 prohibited veterinary drugs, including ß2-receptor agonists, nitrofuran metabolites, nitroimidazoles, chlorpromazine, and chloramphenicol, in pig urine. The sample was pretreated by enzymolysis, acid hydrolysis/derivatization, and liquid-liquid extraction combined with solid-phase extraction. Detection was performed using ultra high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS). Ammonium acetate solution (0.2 mol/L, 4.5 mL) and ß-glucuronidase/aryl sulfatase (40 µL) were added to the sample, which was subsequently enzymolized at 37 ℃ for 2 h. Then, 1.5 mL of 1.0 mol/L hydrochloric acid solution and 100 µL of 0.1 mol/L o-nitrobenzaldehyde solution were added to the sample. The mixture was incubated at 37 ℃ for 16 h, and the analytes were extracted with 8 mL of ethyl acetate by liquid-liquid extraction. The lower aqueous phase obtained after extraction was extracted and purified using a mixed cation-exchange solid-phase extraction column. The extracts were combined, the extraction solution was blow-dried with nitrogen, and the residue was redissolved for determination. The samples were analyzed under multiple-reaction monitoring mode with both positive and negative electrospray ionization, and quantified using an isotope internal standard method. The correlation coefficients (r) of the 12 compounds were >0.99. The limits of detection (LODs) and quantification (LOQs) of chloramphenicol were 0.05 and 0.1 µg/L, respectively, and the LODs and LOQs of the other compounds were 0.25 and 0.5 µg/L, respectively. The mean recoveries and RSDs at 1, 2, and 10 times the LOQ were 83.6%-115.3% and 2.20%-12.34%, respectively. The proposed method has the advantages of high sensitivity, good stability, and accurate quantification; thus, it is suitable for the simultaneous determination of the 12 prohibited veterinary drug residues in pig urine.

Screening of 152 Veterinary Drug Residues in Animal Source Foods by LC-MS/MS, Multilaboratory Validation Study: Final Action 2020.04.

BACKGROUND: The presence of veterinary drug residues in food-producing animals and animal products is regulated through the enforcement of maximum residue limits (MRLs). To answer the need of the food sector to monitor these substances in a wide range of food commodities, stakeholders at AOAC INTERNATIONAL identified the need for a reliable confirmatory screening method. Such a qualitative approach is required for compliance checking and to support product release in manufacturing. OBJECTIVE: Data were collected from five independent laboratories that applied the First Action Official Method 2020.04 to demonstrate adequate performance under reproducibility conditions. The probability of detection (POD) was calculated in blank test samples and test samples spiked at the screening target concentration (STC) level, with the objective to achieve PODs ≤10% and ≥90%, respectively. Additionally, the effectiveness of the screening method was evaluated by participating in 92 proficiency tests. METHODS: Four streams were optimized to screen for 152 veterinary drug residues by LC-MS/MS in a wide variety of food commodities including milk-based ingredients and related products (e.g., milk fractions, infant formula, infant cereals, and baby foods), meat- and fish-based ingredients and related products (fresh, powdered, cooked, infant cereals, and baby foods), and other ingredients based on eggs, animal fat, and animal byproducts. The four streams covered 105 antibiotic residues, anti-inflammatory and antiparasitic agents (stream A), 23 beta-lactams (stream B), 14 aminoglycosides (stream C), and 10 tetracyclines (Stream D). RESULTS: The multilaboratory validation led to PODs at the STC ≥94% and PODs in the blank ≤9%. Further application of the multilaboratory validated method to 92 proficiency tests provided more than 99% satisfactory submitted results (n = 784). CONCLUSION: The interlaboratory reproducibility determined for this method met the acceptance criteria defined in AOAC Standard Method Performance Requirement (SMPR®) 2018.010. HIGHLIGHTS: AOAC has approved the method for Final Action status.

A high-throughput UPLC-MS-MS Bio-analytical method for the analysis of veterinary pharmaceutical residues in Chicken Tissues, Application of efficient-valid-green (EVG) Framework as a Competence Tool.

Antibacterial medications are receiving the most attention due to hypersensitivity reactions and the emergence of bacterial mutants resistant to antibiotics. Treating Animals with uncontrolled amounts of antibiotics will extend beyond their lives and affect humans. This study aims to determine the concentration of the residues of sulfadimidine, sulfaquinoxaline, diaveridine, and vitamin K3 in the tissues of poultry (muscles and liver) after treatment with the combined veterinary formulation. A UPLC-MS-MS method was developed using Poroshell 120 ECC18 and a mobile phase composed of acetonitrile and distilled water, containing 0.1 % formic acid, in the ratio of (85:15 v/v) at a flow rate of 0.6 mL/min. Sample extraction solvent was optimized using response surface methodology (RSM) to be acetonitrile: methanol in the ratio (49.8: 50.2 v/v), and the method was validated according to the FDA bioanalytical method validation protocol over the range (50-1000 µg/Kg) for sulfaquinoxaline and (50-750 µg/Kg) for the other 3 drugs. The greenness of the sample preparation and analytical method was assessed by applying Analytical Eco-scale (AES) and AGREE coupled with AGREEprep. The Competence of the study was evaluated via the EVG framework known as Efficiency, validation, and greenness, to achieve a balance point represented by a radar chart. The method was applied to decide the time required for poultry products to be safe for human use after administration of the studied drugs. It was found that, after the administration of the last dose, minimally 7 days are required till the levels of the drugs drop to the maximum residue limit determined by the FDA/WHO in animal tissues.

Stability of thirteen antimicrobials in incurred samples of animal tissues, milk, eggs, and honey after freeze-storage.

Monitoring of antimicrobials residues in food of animal origin is performed by control laboratories to ensure public health, and knowledge of the stability of antimicrobials during storage is essential for the reliability of results. For stability studies, analysis of incurred samples is preferential to fortified samples due to the possible conversion of antimicrobial metabolites back to parent compounds during sample preparation, storage, and analysis of the incurred samples, resulting in an increased concentration of the analyte. We have analyzed the concentrations of 13 antimicrobials from 8 groups (tetracyclines, fluoroquinolones, phenicols, sulfonamides, aminoglycosides, penicillins, macrolides, and nitroimidazoles) at different time points of freeze-storage (1 week; 1, 2, and 3 months) using HPLC-MS/MS. Incurred samples were prepared from muscle tissue, liver, kidneys, eggs, and milk taken from different animals (cows, pigs, poultry, goats, and fish). Incurred and fortified samples of honey were investigated as well. The results have shown that all analytes in all samples were stable during the investigated periods regardless of animal species, matrix, and concentration levels.

Detection of selected antimicrobial residues in red meat and kidney of beef cattle slaughtered at Nekemte municipal abattoir, Ethiopia.

BACKGROUND: Antibiotics are commonly used drugs in farm animals for therapeutic, prophylactic and diagnosis purposes. As a result of the use of antibiotics in livestock, residues of antibiotics may be present in animal-derived foods, especially in meat. This study aimed at determining the antibiotic residues in cattle slaughtered at Nekemte municipal abattoir and assessing the knowledge, attitude and practice (KAP) level of the community about antibiotic residue in food of cattle origin. MATERIALS AND METHODS: A cross-sectional study was conducted on randomly selected kidney and muscle samples slaughtered at Nekemte municipal abattoir. The samples were collected aseptically and analysed using liquid chromatography mass spectrometer. In addition the KAP of cattle handlers, butcher men and meat users were collected using structured questionnaire. The data was analysed by SPSS and intercooled Stata version 7.0, 2001. RESULTS: Results are presented as percentages and frequency distributions in tabular and graphical form. From 120 individuals interviewed, only 25.83% knew about withdrawal time and had limited knowledge on effect of antibiotic residue on human health, whereas about 47.5% did not heard about antibiotic residue in meat. Tetracycline was detected in all the sampled meat 60 (100%), whereas oxytetracycline residues were detected in half 15 (50%) of the samples. In the current study doxycycline, sulphadiazine, penicillin G and enrofloxacin were not detected in all samples. Oxytetracycline residue levels ranged from 0.00 to 463.35 µg/kg for the kidney and 0.00 to 354.55 µg/kg for muscle samples. About 10% of kidney and 3.33% muscle samples collected had oxytetracycline residues above maximum residue limits. CONCLUSION: In general, the study revealed that oxytetracycline residues were prevalent among antimicrobial residues analysed from the study area. The study indicated the presence of high antimicrobial residue and hence exposes for antimicrobial resistance of pathogens warranting coordinated effort to mitigate its health effect on the animal and hence human being.

Extention and interlaboratory comparison of an LC-MS/MS multi-class method for the determination of 15 different classes of veterinary drug residues in milk and poultry feed.

An HPLC-MS/MS multi-class method for quantitation of 15 different classes of veterinary drug residues (>140 analytes) in milk and poultry feed was developed and validated. Accuracy criteria for routine laboratories were met for the majority of analytes, > 83 % in milk and between 50 and 60 % in chicken feed, with an apparent recovery of 60-140 %. Extraction efficiency criteria were met for >95 % of the analytes for milk and > 80 % for chicken feed. Intermediate precision meets the SANTE criterion of RSD < 20 % for 80-90 % of the analytes in both matrices. For all analytes with an existing MRL in milk, the LOQ was below the related MRL. Twenty-nine samples of commercial milk and chicken feed were analyzed within the interlaboratory comparison. No residues of veterinary drugs were found in the milk samples. However, the feed samples exhibited high levels of nicarbazin, salinomycin, and decoquinate.

Advances in magnetic analytical extraction techniques for detecting antibiotic residues in edible samples.

The widespread use of antibiotics in agricultural and animal husbandry to treat bacterial illnesses has resulted in a rise in antibiotic-resistant bacteria. These bacteria can grow when antibiotic residues are present in food items, especially in edible animal products. As a result, it is crucial to monitor and regulate the amounts of antibiotics in food. Magnetic analytical extractions (MAEs) have emerged as a potential approach for extracting antibiotic residues from food using magnetic nanoparticles (MNPs). Recent improvements in MAEs have resulted in the emergence of novel MNPs with better selectivity and sensitivity for the extraction of antibiotic residues from food samples. Consequently, this review paper addresses current developments in MAE for extracting antibiotic residues from edible samples. It also provides a critical analysis of contemporary MAE practices. The current issues and potential future developments in this field are also discussed, thereby providing a framework for future study paths.