Development, validation, and implementation of an ultratrace analysis method for the determination of moenomycin A, in aquatic animal products.

Moenomycin A, an antimicrobial growth promoter widely used as an additive in aquaculture feedstuffs, has been restricted for use in the European Union and China due to its potential risk of promoting resistant strains of pathogenic bacteria and causing residues in aquatic animal products. Although methods for analyzing moenomycin A in feedstuffs have been developed, no established method exists for aquatic matrices. In this study, we present, for the first time, a sensitive and validated high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method for the determination of moenomycin A in aquatic animal products. Samples were extracted using methanol and purified with the QuEChERS method employing C18 sorbent. The aliquot was dried under a nitrogen stream, reconstituted with methanol-water solvent, and analyzed by HPLC-MS/MS. The developed method exhibited good linearity (r2 > 0.995) over a wide concentration range (1-100 µg/L) and a low limit of detection (1 µg/kg). Average recoveries ranged between 70 and 110% at spiked concentrations of 1, 50, and 100 µg/kg, with associated intra- and inter-day relative standard deviations of 1.25 to 7.32% (n = 6) and 2.91 to 10.08% (n = 3), for different representative aquatic animal production, respectively. To the best of our knowledge, this is the first reported HPLC-MS/MS method for the quantification of moenomycin A in aquatic animal products. The new approach was effectively employed in the analysis of moenomycin A across various aquatic samples.

Analysis of 14 ß-agonists in pork using an automated wooden tip-based solid-phase microextraction device and ultra-high-performance liquid chromatography-tandem mass spectrometry.

This study introduces a cost-effective, automated ultra-high-performance liquid chromatography-tandem mass spectrometry method for the detection of 14 ß-agonists in pork using a novel solid-phase microextraction probe composed of polyacrylonitrile and molecularly imprinted polymer. Integrated into an automated extraction device, the probe optimizes extraction prior to analysis while reducing expenses and time compared to traditional solid-phase extraction procedures. The method validation followed the Chinese National Standard (GB/T 27404-2008) and examined limits of detection, limits of quantification, matrix effects, linearity, intraday, and interday precision. Average recovery rates ranged from 71.6% to 82.2%, with relative standard deviations less than 15%. Limits of detection and limits of quantification ranged from 0.09 to 0.39 and 0.27 to 0.99 µg/kg, respectively. The new method identified positive samples more accurately than the current National Standard GB/T 31658.22-2022 and demonstrated its potential for routine assessment and regulatory compliance in the detection of ß-agonists in pork.

Comparison of filter membranes in the analysis of 183 veterinary and other drugs by liquid chromatography-tandem mass spectrometry.

Although filtration is one of the most common steps in sample preparation for chemical analysis, filter membrane materials can leach contaminants and/or retain some analytes in the filtered solutions. In multiclass, multiresidue analysis of veterinary drugs, it is challenging to find one type of filter membrane that does not retain at least some of the analytes before injection in ultrahigh-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS). In this study, different filter membranes were tested for use in UHPLC-MS/MS analysis of 183 diverse drugs in bovine muscle, kidney, and liver tissues. Membranes evaluated consisted of polytetrafluoroethylene (PTFE), polyvinylidene difluoride (PVDF), polyethersulfone, nylon, and regenerated cellulose. Drug classes represented among the analytes included ß-agonists, ß-lactams, anthelmintics, macrolides, tetracyclines, sulfonamides, tranquilizers, (fluoro)quinolones, anti-inflammatories, nitroimidazoles, coccidiostats, phenicols, and others. Although the presence of a matrix helped reduce the binding of analytes on surface active sites, all of the filter types partially retained at least some of the drugs in the final extracts. In testing by flow-injection analysis, all of the membrane filters were also observed to leach interfering components. Ultimately, filtration was avoided altogether in the final sample preparation approach known as the quick, easy, cheap, effective, rugged, safe, efficient, and robust (QuEChERSER) mega-method, and ultracentrifugation was chosen as an alternative.

A single exposure to sub-lethal concentrations of a glyphosate-based herbicide or fluoxetine-based agent on growth performance in Nile tilapia.

The aim of the present study was to determine e whether a single acute 96 hr exposure of a glyphosate-based herbicide (GBH) to Nile tilapia fingerlings affected growth performance during the first 90 days of culture. This association was considered as GBH increases serotoninergic activity that affect fish anorexically. Although these findings were based upon chronic investigations, this study was designed to examine whether a single, acute, but excessive concentration GBH might impair growth performance in fish. In parallel, fish were also exposed to fluoxetine (FLU), a drug that selectively inhibits the reuptake of serotonin in brain synapses, leading to increased serotoninergic activity. Data demonstrated a decreased growth performance in fingerlings exposed to GBH or FLU compared to unexposed fingerlings. In fact, FLU-exposed fingerlings exhibited lower average weight and length, diminished weight gain, which resulted in lower final biomass. GBH-exposed fish, despite displaying a lower mean body weight, exhibited a biomass similar to biomass on controls. These body weight differences were noted after 30-60- and 90-day growth period in clean water. In an aquaculture context, these observed changes may be considered harmful to the production or economic performance of large-scale farming as currently practiced in tilapia farming.

[Health risks from crop irrigation with treated wastewater containing antibiotic residues, resistance genes, and resistant microorganisms]. / Gesundheitsrisiken durch die Bewässerung von Nutzpflanzen mit aufbereitetem Abwasser, das Antibiotikarückstände, Resistenzgene und resistente Mikroorganismen enthält.

This review describes the effects and potential health risks of resistant microorganisms, resistance genes, and residues of drugs and biocides that occur when re-using wastewater for crop irrigation. It focusses on specific aspects of these contaminants and their interactions, but does not provide a general risk assessment of the microbial load when using reclaimed water.Antimicrobial residues, antimicrobial resistant microorganisms, and resistance genes are frequently detected in treated wastewater. They have effects on the soil and plant-associated microbiota (total associated microorganisms) and can be taken up by plants. An interaction of residues with microorganisms is mainly expected before using the water for irrigation. However, it may also occur as a combined effect on the plant microbiome and all the abundant resistance genes (resistome). Special concerns are raised as plants are frequently consumed raw, that is, without processing that might reduce the bacterial load. Washing fruits and vegetables only has minor effects on the plant microbiome. On the other hand, cutting and other processes may support growth of microorganisms. Therefore, after such process steps, cooling of the foods is required.Further progress has to be made in the treatment of wastewater that will be used for crop irrigation with respect to removing micropollutants and microorganisms to minimize the risk of an increased exposure of consumers to transferable resistance genes and resistant bacteria.

[Determination of amantadine, rimantadine and dimethylamantadine residues in poultry by ultra-performance liquid chromatography-tandem mass spectrometry].

OBJECTIVE: To establish a method for determination of amantadine, rimantadine and dimethylamantadine residues in poultry matrix by ultra-performance liquid chromatography-tandem mass spectrometry. METHODS: Poultry samples were extracted with acid acetonitrile, salting out, and then the organic phase was cleaned up by C_(18) and PSA. A Waters ACQUITYTM UPLC HSS T3 column(100 mm×2.1 mm, 1.7 mm)was used for liquid chromatography separation, ESI positive ion scan was used with multiple reaction monitoring(MRM) mode and quantified by matrix-matched external standard method. RESULTS: At the spiked level of 0.5, 1.0 and 5.0 µg/kg, the recoveries of each compound were in the range of 81.3%-91.1% with the relative standard deviations of 6.5%-11.3%. The qualitative limits of detections were 0.06-0.2 µg/kg and the quantitative limits were 0.2-0.5 µg/kg for the 3 target compounds. The established method was applied to the detection of the 3 target compounds in 30 poultry samples, and none of the target compounds exceeded the residue limits. CONCLUSION: The method is simple, rapid, high sensitivity and good stability, with a wide variety and a certain development. It can be used for the daily monitoring of the veterinary drug residues in poultry.

Recent progress of personal glucose meters integrated methods in food safety hazards detection.

Development of personal glucose meters (PGMs) for blood glucose monitoring and management by the diabetic patients has been a long history since its first invention in 1968 and commercial application in 1975. The main reasons for its wide acceptance and popularity can be attributed mainly to the easy operation, test-to-result model, low cost, and small volume of sample required for blood glucose concentration test. During past decades, advances in analytical techniques have repurposed the use of PGMs into a general point-of-care testing platform for a variety of non-glucose targets, especially the food hazards. In this review, we summarized the recent published research using PGMs to detect the food safety hazards of mycotoxins, illegal additives, pathogen bacteria, and pesticide and veterinary drug residues detection with PGMs. The progress on PGM-based detection achieved in food safety have been carefully compared and analyzed. Furthermore, the current bottlenecks and challenges for practical applications of PGM for hazards detection in food safety have also been proposed.

Antibiotic residues in poultry tissues in Iran: A systematic review and meta-analysis.

To control the drug residues in foods, the national Maximum Residue Limits (MRLs) have been determined by the international organizations; however, no regulation has been complied for MRL in food animals in Iran. This study was a systematic review and meta-analysis about studies of antibiotic residues in slaughtered poultry carcasses, in Iran. The information was first collected and analyzed throughout six international databases, and four Iranian national databases. According to the data, the total prevalence of antibiotic residues was obtained as 39.41%, 5.40%, and 0.30% using four-plate test (FPT), High-Performance Liquid Chromatography (HPLC), and Enzyme-linked immuno_sorbent assay (ELISA) methods, respectively. The highest prevalence of the residues was shown in the liver by both methods of HPLC (47.75%) and ELISA (14.35%). Moreover, the total mean of antibiotics was recorded as 71.03 ppb and 65.86 ppb in different tissues using the HPLC and ELISA method, respectively. Based on this study, we can conclude that the prevalence of antibiotic residue in poultry meat in Iran is high and that this level does not cause health problems for consumers. It is highly recommended to execute tight surveillance strategies from the government in antibiotic monitoring.

Multiclass and multi-residue screening of mycotoxins, pharmacologically active substances, and pesticides in infant milk formulas through ultra-high-performance liquid chromatography coupled with high-resolution mass spectrometry analysis.

Infant milk formulas are designed to substitute human milk when breastfeeding is unavailable. In addition to human milk and milk-derived products, these formulas can be a vehicle of contaminants. In this work, a multiclass method based on the QuEChERS (quick, easy, cheap, effective, rugged, and safe) approach was developed for the simultaneous determination of contaminants (n = 45), including mycotoxins and veterinary drug residues, occurring in infant milk formulas. By using an ultra-high-performance liquid chromatography quadrupole-Orbitrap coupled with high-resolution mass spectrometry analysis (UHPLC-Q-Orbitrap HRMS; Thermo Fisher Scientific), further retrospective analysis of 337 contaminants, including pesticides, was achieved. The method was validated in accordance with European regulations and applied for the analysis of 54 infant milk samples. Risk assessment was also performed. Dexamethasone was detected in 16.6% of samples (range: 0.905-1.131 ng/mL), and procaine benzyl penicillin in 1 sample at a concentration of 0.295 ng/mL. Zearalenone was found in 55.5% of samples (range: 0.133-0.638 ng/mL) and α-zearalenol in 16.6% of samples (range: 1.534-10.408 ng/mL). Up to 49 pesticides, 11 veterinary drug residues, and 5 mycotoxins were tentatively identified via retrospective analysis based on the mass spectral library. These findings highlight the necessity of careful evaluation of contaminants in infant formulas, considering that they are intended for a vulnerable part of the population.

Photothermal card reader assay using the commercial colloidal gold test strip for the rapid quantitative detection of food hazards.

The simple and rapid commercial colloidal gold test strip can only be used for qualitative or semi-quantitative detection, accompanied by weak detectability and false negative experimental results. Herein, a photothermal test strip assay which combined test strip with a portable photothermal card reader was established to achieve quantitative detection with excellent detectability. According to the photothermal effect produced by gold nanoparticles (GNPs) captured on the test line, the signal could be recorded by the reader. Thirteen food hazards including veterinary drug residues and pesticide residues were tested; the photothermal detectability in actual samples were about 23 (methyl parathion), 7 (enrofloxacin), 6 (sarafloxacin), 8 (sulfadiazine), 12 (sulfamethazine), 7 (paraquat), 6 (malachite green), 11 (amantadine), 13 (nitrofurazone), 6 (diethylstilbestrol), 12 (estriol), 21 (estrone), and 26 (17ß-estradiol) times better than the visual detectability. Our results demonstrated that the photothermal test strip assay could be used for sensitive, rapid, and quantitative detection of residues of food hazards.

Methamphetamine pollution elicits addiction in wild fish.

Illicit drug abuse presents pervasive adverse consequences for human societies around the world. Illicit drug consumption also plays an unexpected role in contamination of aquatic ecosystems that receive wastewater discharges. Here, we show that methamphetamine, considered as one of the most important global health threats, causes addiction and behavior alteration of brown trout Salmo trutta at environmentally relevant concentrations (1 µg l-1). Altered movement behavior and preference for methamphetamine during withdrawal were linked to drug residues in fish brain tissues and accompanied by brain metabolome changes. Our results suggest that emission of illicit drugs into freshwater ecosystems causes addiction in fish and modifies habitat preferences with unexpected adverse consequences of relevance at the individual and population levels. As such, our study identifies transmission of human societal problems to aquatic ecosystems.

Advanced materials on sample preparation for safety analysis of aquatic products.

Safety analysis of aquatic products has been a challenge in recent years due to the serious matrix interference, complex characteristics, and ultra-low content of analytes. Introducing advanced materials to sample preparation technique can greatly improve the extraction, enrichment, and separation for further qualification and quantification of target analytes by coupling with consequent analytical technologies. Based on this scope, this review is mainly introducing advanced materials on the sample preparation for safety analysis of aquatic products in the past decade. After introducing the importance of the corresponding advanced materials, advanced materials are used for the sample preparation and in the improvement of safety analysis result of aquatic products. Advanced materials for sample preparation of aquatic products were reviewed including carbon materials, metal organic frameworks, covalent organic frameworks, molecularly/ions imprinted polymers, etc. Then, applications of the advanced materials for the analysis of specific fishery analytes (antibiotics, anesthetic, preservatives, etc.) were briefly introduced. Conclusions and perspectives on advanced materials for sample preparation and safety analysis of aquatic products were also presented.

Antimicrobial drug residues in animal-derived foods: Potential impact on the human intestinal microbiome.

The use of veterinary drugs in food-producing animals may result in the presence of low levels of drug residues in these edible, animal-derived foods, with potential dietary exposure to humans. Since therapeutic doses of antibiotics have been shown to affect bacterial populations in the gastrointestinal tract microbiome and can also promote the emergence of antibiotic-resistant bacteria, there is concern that animal drugs at residue level concentrations could also perturb the intestinal microbiome composition and modify the antimicrobial resistance profile of the human intestinal microbiota. This review provides updated information on the VICH GL#36(R2), on evaluating the safety of veterinary drug residues in animal-derived foods and their effects on the human intestinal microbiome; discusses critical research knowledge gaps and challenges in evaluating the impact of drug residues in animal-derived foods on the human intestinal microbiome; and analyzes integrated basic and applied research approaches, currently being conducted at FDA, on studies that specifically address key regulatory science questions. Moreover, this review aims to emphasize future research needs on scientific methodology and provides general recommendations on drug inactivation, bioavailability, and antimicrobial resistance, to improve the safety evaluation and risk assessment of antimicrobial residues and their impact on the gastrointestinal microbiota, with the goal of ensuring food safety.

Validated Simultaneous Gradient Ultra-Performance Liquid Chromatographic Quantification of Some Proton Pump Inhibitor Drug Residues in Saudi Pharmaceutical Industrial Wastewater.

Monitoring and quantification of active pharmaceutical ingredients (APIs) in the environment constitute important and challenging tasks, as they are directly associated with human health. Three commonly used proton pump inhibitors (PPIs), namely, omeprazole sodium (OMP), pantoprazole sodium (PNT), and lansoprazole sodium (LNZ) are well separated and quantified using ultra-performance liquid chromatography (UPLC) in pharmaceutical industrial wastewater. The separation of the studied drugs was performed on a stationary phase with a WatersTM column (100 × 2.1 mm, 1.7 µm). The mobile phase was composed of methanol:0.05 M potassium dihydrogen phosphate buffer (adjusted to pH 7.5 using NaOH) (50:50, v/v). The elution process was done in gradient mode by changing the relative proportions of the mobile phase components with time to get an optimum separation pattern. The flow rate of the developing system was adjusted to 0.8 mL/minute. Detection of the separated drugs was performed at 230 nm. The studied drugs were quantified in the concentration range of 10-200 ng/mL for all drugs. The cited method was fully validated according to the international conference on harmonization (ICH-Q2B) guidelines, then it was applied successfully for quantification of the studied PPIs in real wastewater samples after their solid phase extraction (SPE).

Development and validation of an LC-MS/MS screening method for macrolide and quinolone residues in baby food.

A simple, rapid and sensitive screening method by liquid chromatography-tandem mass spectrometry (LC-MS/MS) was developed for the identification of 7 macrolides (clarithromycin, erythromycin, oleandomycin, spiramycin, tilmicosin, troleandomycin and tylosin) and 8 quinolones (ciprofloxacin, difloxacin, enrofloxacin, flumequine, moxifloxacin, nalidixic acid, norfloxacin and ofloxacin) in meat and egg-based baby foods. Sample preparation was performed using an alkaline modified QuEChERS (Quick, Easy, Cheap, Effective, Rugged, Safe) extraction method without additional clean-up steps. A simplex-lattice mixture experimental design was used in the optimization of the QuEChERS extraction solvent. The developed method was successfully validated according to the Commission Decision 2002/657/EC and the European Community Reference Laboratories Residues Guidelines regarding the validation of screening methods 20/01/2010, adopting a fixed permited tolerance for relative ion ratio. Samples of baby food (n = 44) commercialized in Rio de Janeiro, Brazil, were analyzed using the validated method and none of them presented residues of the searched macrolides and quinolones, with a screening target value of 5 µg kg-1.

Screening and Analysis of Multiclass Veterinary Drug Residues in Animal Source Foods using UPLC-Q-Exactive Orbitrap/MS.

A rapid, simple, and sensitive method of detecting veterinary drug residues in animal food sources, including poultry and pork, was developed and validated. The method was optimized for over 155 veterinary drugs of 21 different classes. Sample pretreatment included a simple solid-liquid extraction step with 0.2% formic acid-acetonitrile-water and a purification step with a PRiME HLB (hydrophile-lipophile balance) solid-phase extraction cartridge. Data were collected using ultra-high-performance liquid chromatography coupled to Quadrupole-Exactive Orbitrap mass spectrometry. The limits of detection of 155 veterinary drugs ranged from 0.1 µg/kg to 10 µg/kg. The recovery rates were between 79.2 and 118.5 % in all matrices studied, with relative standard deviation values less than 15% (n = 6). The evaluated method allows the reliable screening, quantification, and identification of 155 veterinary drug residues in animal source food and has been successfully applied in authentic samples.

Influenza A/H4N2 mallard infection experiments further indicate zanamivir as less prone to induce environmental resistance development than oseltamivir.

Neuraminidase inhibitors (NAIs) are the gold standard treatment for influenza A virus (IAV). Oseltamivir is mostly used, followed by zanamivir (ZA). NAIs are not readily degraded in conventional wastewater treatment plants and can be detected in aquatic environments. Waterfowl are natural IAV hosts and replicating IAVs could thus be exposed to NAIs in the environment and develop resistance. Avian IAVs form the genetic basis for new human IAVs, and a resistant IAV with pandemic potential poses a serious public health threat, as NAIs constitute a pandemic preparedness cornerstone. Resistance development in waterfowl IAVs exposed to NAIs in the water environment has previously been investigated in an in vivo mallard model and resistance development was demonstrated in several avian IAVs after the exposure of infected ducks to oseltamivir, and in an H1N1 IAV after exposure to ZA. The N1 and N2 types of IAVs have different characteristics and resistance mutations, and so the present study investigated the exposure of an N2-type IAV (H4N2) in infected mallards to 1, 10 and 100 µg l-1 of ZA in the water environment. Two neuraminidase substitutions emerged, H274N (ZA IC50 increased 5.5-fold) and E119G (ZA IC50 increased 110-fold) at 10 and 100 µg l-1 of ZA, respectively. Reversion towards wild-type was observed for both substitutions in experiments with removed drug pressure, indicating reduced fitness of both resistant viruses. These results corroborate previous findings that the development of resistance to ZA in the environment seems less likely to occur than the development of resistance to oseltamivir, adding information that is useful in planning for prudent drug use and pandemic preparedness.

Rapid Multi-Residue Detection Methods for Pesticides and Veterinary Drugs.

The excessive use or abuse of pesticides and veterinary drugs leads to residues in food, which can threaten human health. Therefore, there is an extremely urgent need for multi-analyte analysis techniques for the detection of pesticide and veterinary drug residues, which can be applied as screening techniques for food safety monitoring and detection. Recent developments related to rapid multi-residue detection methods for pesticide and veterinary drug residues are reviewed herein. Methods based on different recognition elements or the inherent characteristics of pesticides and veterinary drugs are described in detail. The preparation and application of three broadly specific recognition elements-antibodies, aptamers, and molecular imprinted polymers-are summarized. Furthermore, enzymatic inhibition-based sensors, near-infrared spectroscopy, and SERS spectroscopy based on the inherent characteristics are also discussed. The aim of this review is to provide a useful reference for the further development of rapid multi-analyte analysis of pesticide and veterinary drug residues.

[Determination of 20 kinds of ß-receptor blockers in animal foods by ultra high performance liquid chromatography-tandem mass spectrometry].

OBJECTIVE: To establish an analytical method for determination of 20 kinds of ß-receptor blockers residues in animal foods by ultra high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS). METHODS: The samples of animal foods were enzymatic hydrolysis by trichloroacetic acid(TCA), purified by MCX column. The separation was performed on a Waters ACQUITYTM BEH C_(18 )column(100 mm×2. 1 mm, 1. 7 µm), then the target compounds were detected by UPLC-MS/MS with ESI positive ion scan in mode of multiple reaction monitoring(MRM) and quantified by matrix matched external standard method. RESULTS: At the spiked level of 1, 2 and 4 µg/kg, the recoveries of each compound were in the range of 61. 9%-119. 1% with the relative standard deviations of 1. 5%-28. 4%(n=6). The qualitative limits of detections were 0. 01-0. 15 µg/kg and the quantitative limits were 0. 03-0. 50 µg/kg for the 20 targets compounds. By using the established method, the target compounds in 30 animal foods were detected, and no excessive veterinary drug residue were detected. CONCLUSION: The established method is simple, rapid, high sensitivity and good stability, with a wide variety and a certain development. It can provide more convenient and fast detection method support for the daily monitoring of veterinary drug residues in animal foods.

[Determination of α_2-agonists in animal food by ultra high performance liquid chromatography -tandem mass spectrometry].

OBJECTIVE: To establish an analytical method for determination of 6 kinds of α_2-agonists in animal foods by ultra high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS). METHODS: The samples of animal food were enzymatic hydrolysis by ß-glucosidase/arylsulfatase, purified by MCX column. The separation was performed on a Dikma leapsil C_(18) column(2. 1 mm×100 mm, 2. 7 µm), then the target compound were detected by ultra high performance liquid chromatography-tandem mass spectrometry with electron spray ionization(ESI) positive ion scan in mode of multiple reaction monitoring(MRM) and quantified by matrix matched external standard method. RESULTS: At the spiked level of 1, 2 and 4 µg/kg, the recoveries of each compound were in the range of 70. 4%-111. 2% with the relative standard deviations of 2. 3%-18. 8%. The qualitative limits of detections were 0. 06-0. 3 µg/kg and the quantitative limits were 0. 2-1. 0 µg/kg for the 6 targets compounds. By using the established method, the target compound in 30 samples including pork, pig liver, pig kidney, beef and mutton were detected, and no excessive veterinary drug residue were detected. CONCLUSION: The established method is simple, rapid, high sensitivity and good stability, with a wide variety and a certain development. It can provide more convenient and fast detection method support for the daily monitoring of veterinary drug residues in animal food.