RESUMEN

A modified QuEChERS method was developed to determine multi-class pesticide and veterinary residues in aquatic products. Chitosan microspheres were conveniently synthesized and utilized as the cleanup adsorbent in the QuEChERS procedure, showcasing rapid filtration one-step pretreatment ability for the determination of drug multi-residues in aquatic products. Compared to conventional synthetic sorbents, chitosan microspheres not only have good purification performance, but also have renewable and degradable properties. This novel sorbent worked well in the simultaneous determination of 95 pesticides and veterinary drug residues in aquatic products after being combined with an improved one-step vortex oscillating cleanup method. We achieved recoveries ranging from 64.0% to 115.9% for target drugs in shrimp and fish matrix. The limits of detection and quantification were 0.5-1.0 and 1.0-2.0 µg kg-1, respectively. Notably, hydrocortisone was detected with considerable frequency and concentration in the tested samples, underscoring the necessity for stringent monitoring of this compound in aquatic products.

Asunto(s)

Quitosano , Peces , Microesferas , Espectrometría de Masas en Tándem , Drogas Veterinarias , Animales , Quitosano/química , Cromatografía Líquida de Alta Presión , Drogas Veterinarias/análisis , Drogas Veterinarias/aislamiento & purificación , Contaminación de Alimentos/análisis , Residuos de Medicamentos/análisis , Residuos de Medicamentos/aislamiento & purificación , Residuos de Medicamentos/química , Plaguicidas/aislamiento & purificación , Plaguicidas/análisis , Plaguicidas/química , Residuos de Plaguicidas/aislamiento & purificación , Residuos de Plaguicidas/análisis , Residuos de Plaguicidas/química , Adsorción , Extracción en Fase Sólida/métodos , Extracción en Fase Sólida/instrumentación , Contaminantes Químicos del Agua/aislamiento & purificación , Contaminantes Químicos del Agua/química , Contaminantes Químicos del Agua/análisis , Alimentos Marinos/análisis , Mariscos/análisis , Cromatografía Líquida con Espectrometría de Masas

RESUMEN

BACKGROUND: Excessive use of veterinary drugs causes severely environmental pollution and agricultural pollution, and poses great threat to human health. A simple method for the rapid, highly sensitive, and on-site monitoring of veterinary drug residues in complex samples remains lacking. RESULTS: In this study, we propose a catalytically enhanced colorimetric lateral flow immunoassay (LFA) based on a novel core-satellite-structured magnetic nanozyme (Fe-Au@Pt) that can simultaneously and quantitatively detect three common veterinary drugs, namely, gentamicin (GM), streptomycin (STR), and clenbuterol (CLE), within a short testing time (<30 min). The Fe-Au@Pt nanozyme was simply prepared through the self-assembly of numerous Au@Pt nanoparticles on a large Fe3O4 core via electrostatic adhesion, which exhibited the advantages of high peroxidase-like activity, strong magnetic responsiveness, and multiple catalytic sites. Under the dual-signal amplification effect of magnetic enrichment and catalytic enhancement, the proposed nanozyme-LFA allowed the multiplex detection of STR, CLE, and GM with detection limits of 10.1, 6.3, and 1.1 pg/mL, respectively. SIGNIFICANCE: The developed Fe-Au@Pt-LFA achieves direct, simultaneous, and accurate detection of three target drugs in food samples (honey, milk, and pork). The proposed assay shows great potential for application in the real-time monitoring of small-molecule pollutants in complex environment.

Asunto(s)

Colorimetría , Residuos de Medicamentos , Oro , Colorimetría/métodos , Inmunoensayo/métodos , Oro/química , Residuos de Medicamentos/análisis , Límite de Detección , Animales , Platino (Metal)/química , Nanopartículas de Magnetita/química , Leche/química , Nanopartículas del Metal/química , Contaminación de Alimentos/análisis

RESUMEN

BACKGROUND: Antibiotic residues in food chain have raised concerns regarding their toxicity and involvement in antimicrobial resistance. However, most existing antibiotic biosensors are primarily applicable to liquid food samples. Given the complex matrix characteristics of foods, there is an urgent need for the development of effective antibiotic detection platforms that exhibit high universality and flexibility. Porous microneedles (PMN) are microdevice structures with needle-like shapes and microscale pores throughout their composition, which facilitate rapid sampling. Consequently, the integration of PMN with biosensors holds significant promise for the detection of antibiotic residues in complex food samples. RESULTS: In this study, hydrogel-forming PMN are fabricated by leveraging the oxygen-production capacity of thylakoid to generate bubbles and form porous structures. These PMN are then integrated with a fluorescence aptasensor for the quantification of the antibiotic netilmicin. The aptasensor consists of a netilmicin (NET) aptamer with stem loop and hairpin structure, which facilitated the binding of SYBR Green I to produce a fluorescent signal. In the presence of NET, the complete binding between NET and the aptamer results in a reduction of fluorescence intensity, thereby generating a detectable signal change for the detection of NET. Utilizing capillary action accelerate fluid extraction (2.9 times faster than nonporous microneedles) and a large specific surface area (5.1072 m2/g) conducive to aptasensor adsorb, the PMN achieve efficient capture and quantification of antibiotic with limits of detection and quantitation of 5.99 nM and 19.8 nM, respectively. SIGNIFICANCE: Porous microneedles with tunable porosity and desirable mechanical properties are successfully fabricated. The integration of PMN with aptasensor enable the efficient detection of netilmicin in fish, milk and river water samples, demonstrating high recovery rates. The PMN represent potential tools for the convenient and rapid detection of antibiotic residues within complex food matrices, thereby enhancing food safety monitoring.

Asunto(s)

Antibacterianos , Agujas , Antibacterianos/análisis , Porosidad , Tilacoides/química , Técnicas Biosensibles , Aptámeros de Nucleótidos/química , Animales , Contaminación de Alimentos/análisis , Residuos de Medicamentos/análisis , Límite de Detección , Tecnología Química Verde , Análisis de los Alimentos/métodos , Análisis de los Alimentos/instrumentación

RESUMEN

Drug residues that contaminate food and water represent a serious concern for human health. The major concerns regard the possible irrational use of these contaminants, since this might increase the amplitude of exposure. Multiple sources contribute to the overall exposure to contaminants, including agriculture, domestic use, personal, public and veterinary healthcare, increasing the possible origin of contamination. In this review, we focus on crop pesticides and veterinary drug residues because of their extensive use in modern agriculture and farming, which ensures food production and security for the ever-growing population around the world. We discuss crop pesticides and veterinary drug residues with respect to their worldwide distribution and impacts, with special attention on their harmful effects on human reproduction and embryo development, as well as their link to epigenetic alterations, leading to intergenerational and transgenerational diseases. Among the contaminants, the most commonly implicated in causing such disorders are organophosphates, glyphosate and antibiotics, with tetracyclines being the most frequently reported. This review highlights the importance of finding new management strategies for pesticides and veterinary drugs. Moreover, due to the still limited knowledge on inter- and transgenerational effects of these contaminants, we underlie the need to strengthen research in this field, so as to better clarify the specific effects of each contaminant and their long-term impact.

Asunto(s)

Desarrollo Embrionario , Fertilidad , Plaguicidas , Drogas Veterinarias , Humanos , Desarrollo Embrionario/efectos de los fármacos , Fertilidad/efectos de los fármacos , Exposición Dietética/efectos adversos , Animales , Residuos de Medicamentos/análisis , Epigénesis Genética/efectos de los fármacos , Residuos de Plaguicidas/análisis

RESUMEN

Boric acid-functionalized magnetic covalent organic frameworks (Fe3O4-TpBD-B) with large surface area and high porosity were prepared and applied for magnetic solid-phase extraction adsorbent of gentamicin from milk before UPLC-MS/MS detection. By utilizing a new HILIC chromatographic column with zwitterionic sulfoalkyl betaine stationary phase based on ethyl bridged hybrid particles (BEH), isomers of gentamicin (C1, C1a, and C2+C2a components). The developed methods demonstrated good linearity (R2 > 0.99), acceptable accuracy and good precision (<10 %), and low limit of quantitation (1.59 ng mL⁻1 for C1, 1.52 ng mL⁻1 for C1a and 2.72 ng mL⁻1 for C2+C2a). In addition, this method has been effectively applied to the analysis of real milk samples.

Asunto(s)

Ácidos Borónicos , Gentamicinas , Interacciones Hidrofóbicas e Hidrofílicas , Estructuras Metalorgánicas , Leche , Extracción en Fase Sólida , Espectrometría de Masas en Tándem , Leche/química , Extracción en Fase Sólida/métodos , Espectrometría de Masas en Tándem/métodos , Animales , Gentamicinas/análisis , Gentamicinas/química , Estructuras Metalorgánicas/química , Ácidos Borónicos/química , Residuos de Medicamentos/análisis , Residuos de Medicamentos/aislamiento & purificación , Contaminación de Alimentos/análisis , Límite de Detección , Cromatografía Líquida de Alta Presión/métodos

RESUMEN

Knowledge of amoxicillin (AMX) pharmacokinetics (PK) and tissue residues in fish, which is necessary for prudent drug use, remains limited. The study aimed to explore the PK characteristics of AMX in Nile tilapia (Oreochromis niloticus) reared at 25 and 30 °C as well as to determine optimal dosages and drug withdrawal time (WDT). In the PK investigation, the fish received a single dose of 40 mg/kg AMX via oral gavage, and the optimal dosage was determined by the pharmacokinetic-pharmacodynamic approach. In the tissue residue study, the fish were orally gavaged with 40 mg/kg/day AMX once daily for 5 days and the WDT was established by the linear regression analysis. The results revealed the temperature-dependent drug elimination; the clearance relative to bioavailability (CL/F) and elimination half-life at 30 °C (0.180 L/kg/h and 6.06 h, respectively) were about twice those at 25 °C (0.090 L/kg/h and 10.49 h, respectively). The optimal dosages at the minimum inhibitory concentration (MIC) of 2 µg/mL were 10.97 (25 °C) and 41.03 (30 °C) mg/kg/day, respectively. Finally, following the multiple oral administration, the muscle/skin residue of AMX on day 1 after the last dosing at 25 and 30 °C were 548 and 264 ng/g, respectively. The average tissue residues were depleted below the maximum residue limits (MRL) of 50 µg/kg on day 5 (25 °C) and 3 (30 °C), respectively, and the WDT were 6 and 4 days when rearing at 25 and 30 °C, respectively. This knowledge serves as a practical guideline for responsible use of AMX in treating bacterial diseases in Nile tilapia aquaculture.

Asunto(s)

Amoxicilina , Antibacterianos , Cíclidos , Temperatura , Animales , Amoxicilina/farmacocinética , Amoxicilina/administración & dosificación , Antibacterianos/farmacocinética , Antibacterianos/administración & dosificación , Residuos de Medicamentos , Pruebas de Sensibilidad Microbiana , Semivida , Relación Dosis-Respuesta a Droga

RESUMEN

Milk is an important consumer product with high nutritional value. The presence of veterinary drug residues in milk owing to the indiscriminate use of veterinary drugs may affect consumer health. In the mass spectrometric analysis of trace compounds, chromatographic co-eluting components easily interfere with the mass spectral signals obtained, affecting the accuracy of qualitative and quantitative analyses. Matrix purification is a promising method to reduce the matrix effect. Chitosan is a natural biopolymer with numerous active functional groups such as amino, acetyl, and hydroxyl groups; these groups can adsorb lipids through hydrophobic and electrostatic interactions. Chitosan also has the advantages of low production cost, stable chemical properties, and convenient modification. Novel chitosan-based materials are promising candidates for lipid purification. In this study, a chitosan membrane was modified with trimethoxyoctadecylsilane (C18-CSM). C18-CSM was prepared through one-step hydrolysis and used as a dispersive solid phase extraction (DSPE) adsorbent to purify the matrix during milk pretreatment. We combined C18-CSM with ultra-high performance liquid chromatography-quadrupole/electrostatic field orbitrap mass spectrometry (UHPLC-Q/Exactive Orbitrap MS) to develop an effective method for the extraction and determination of ofloxacin, enrofloxacin, ciprofloxacin, diazepam, and metronidazole in milk. C18-CSM was characterized using scanning electron microscopy, Fourier transform infrared spectroscopy, and water contact angle testing. The results indicated that the material has a rough surface and uniformly dense cross-section. The water contact angle of C18-CSM was 104°, indicating its good hydrophobicity. The pretreatment conditions (extraction solvent, dosage of NaCl, extraction frequency, and dosage of C18-CSM) that influenced the recoveries of the five veterinary drugs were investigated in detail. The optimal conditions were established as follows: 5% formic acid in acetonitrile, 1 g NaCl, extraction 1 time, 20 mg C18-CSM. Separation was performed on a Hypersil GOLD VANQUISH column (100 mm×2.1 mm, 1.9 µm). The mobile phase consisted of 0.1% formic acid aqueous solution and 0.1% formic acid in acetonitrile, and was flowed at a rate of 0.3 mL/min. The sample injection volume was 1 µL, and the column temperature was maintained at 25 ℃. Mass spectrometric analysis was performed in positive electrospray ionization mode. To verify the necessity of the purification material, the matrix effect was investigated using the matrix-matched standard curve method. The use of C18-CSM reduced the matrix effects of the five necessity drugs from the range of -22%-8.8% to the range of -13%-3.6%, indicating that C18-CSM is a highly efficient DSPE material. Under optimal conditions, the developed method showed good linearities within the range of 0.5-100 µg/L, with correlation coefficients (r2)≥0.9970. The limits of detection(LODs) and quantification (LOQs) were 0.2 µg/L and 0.5 µg/L, respectively. To assess the accuracy and precision of the method, we prepared milk samples with three spiked levels (low, medium, and high). The recoveries of the five veterinary drugs were ranged from 79.5% to 115%, and the intra-day and inter-day relative standard deviations were 7.0%-13% (n=6) and 1.3%-11% (n=3), respectively. This study provides a simple, accurate, and reliable method for the rapid and simultaneous determination of the five veterinary drug residues in milk.

Asunto(s)

Quitosano , Residuos de Medicamentos , Contaminación de Alimentos , Espectrometría de Masas , Leche , Drogas Veterinarias , Animales , Leche/química , Residuos de Medicamentos/análisis , Cromatografía Líquida de Alta Presión , Quitosano/química , Drogas Veterinarias/análisis , Contaminación de Alimentos/análisis

RESUMEN

Veterinary drugs play a crucial role in the treatment of various animal diseases. However, their residues, stemming from issues, such as withdrawal period lapses, overuse, or abuse, can jeopardize food safety and human health. This study addresses recent regulations in Korea concerning specific veterinary drugs (anacolin, ephedrine, menichlopholan, piperonyl butoxide, and etisazole HCl) and their ongoing discussions. This study aimed to validate two pre-developed methods for quantifying residues in livestock and fishery products using QuEChERS and liquid chromatography-tandem mass spectrometry. Both methods exhibited excellent linearity, recoveries (70.3-119%), and coefficient of variations (1.3-28%), along with low limits of detection and quantification (0.3-4 ng/g and 1-12 ng/g). This study is significant for its contribution to the detection of veterinary drugs in livestock and fishery products, given the limited research available on the methods for analyzing these substances.

Asunto(s)

Residuos de Medicamentos , Contaminación de Alimentos , Ganado , Espectrometría de Masas en Tándem , Drogas Veterinarias , Residuos de Medicamentos/análisis , Drogas Veterinarias/análisis , República de Corea , Animales , Espectrometría de Masas en Tándem/métodos , Contaminación de Alimentos/análisis , Límite de Detección , Cromatografía Líquida de Alta Presión , Explotaciones Pesqueras

RESUMEN

Based on salting-out assisted liquid-liquid extraction (SALLE) and high performance liquid chromatography tandem mass spectrometry (HPLC-MS/MS), a simple, rapid pretreatment without complex clean-up for the determination of 22 veterinary drug residues in aquatic products was developed and validated. In order to improve the efficiency of the method, the key procedural parameters of SALLE were fabricated. Na2EDTA-Mcllvaine buffer/ACN was used as the extraction solvent, anhydrous MgSO4 and NaCl as the extraction salts. The relationship between extraction efficiency and logD was initially evaluated during the optimization process. This study was well validated in various aquatic samples such as bass, large yellow croaker, carp, and shrimp, the limits of detection (LOD) and accuracy for all compounds ranged from 0.5 to 1.0 µg/kg, 71.4% to 120%. This method has the advantages of rapidity, simplicity, low cost, and high efficiency, and has broad potential for risk monitoring and evaluation of veterinary antibiotics in aquatic products.

Asunto(s)

Antibacterianos , Residuos de Medicamentos , Peces , Contaminación de Alimentos , Extracción Líquido-Líquido , Alimentos Marinos , Espectrometría de Masas en Tándem , Drogas Veterinarias , Cromatografía Líquida de Alta Presión/métodos , Espectrometría de Masas en Tándem/métodos , Extracción Líquido-Líquido/métodos , Antibacterianos/análisis , Animales , Residuos de Medicamentos/análisis , Drogas Veterinarias/análisis , Contaminación de Alimentos/análisis , Alimentos Marinos/análisis , Carpas , Límite de Detección , Perciformes , Penaeidae/química , Cromatografía Líquida con Espectrometría de Masas

RESUMEN

This study concerns the synthesis of the florfenicol (FF) metabolites florfenicol amine (FFA), florfenicol alcohol (FFOH), and monochloroflorfenicol (FFCl), for their subsequent use as reference standards in On-line solid-phase extraction-ultra high-performance liquid chromatography-tandem mass spectrometry (SPE-UHPLC-MS/MS) analysis. The metabolites were characterized using 1H and 13C NMR, as well as HRMS, and their purities were confirmed by quantitative NMR to ensure analytical reliability. Validation of the developed analytical method showed that it presented acceptable performance, with linearity >0.99 for all the target analytes, accuracies within ±10 % of nominal concentrations, and intra- and inter-day precisions within 15 %. Application of this method to fillets from fish that had been treated with florfenicol (dose of 10 mg/kg bw daily) demonstrated its effectiveness in consistently detecting FF and its metabolites throughout the treatment. The results emphasized the utility of the method for enhancing pharmacokinetic and residue depletion research. The ability to precisely monitor the drug and its metabolites in treated fish provides important insights into florfenicol metabolism, laying the groundwork for further comprehensive profiling studies of metabolites in fish tissue.

Asunto(s)

Extracción en Fase Sólida , Espectrometría de Masas en Tándem , Tianfenicol , Tianfenicol/análogos & derivados , Tianfenicol/análisis , Tianfenicol/metabolismo , Tianfenicol/farmacocinética , Tianfenicol/química , Animales , Espectrometría de Masas en Tándem/métodos , Cromatografía Líquida de Alta Presión/métodos , Extracción en Fase Sólida/métodos , Reproducibilidad de los Resultados , Modelos Lineales , Límite de Detección , Cíclidos/metabolismo , Residuos de Medicamentos/análisis , Residuos de Medicamentos/metabolismo , Antibacterianos/análisis , Antibacterianos/química , Antibacterianos/farmacocinética , Antibacterianos/metabolismo , Alimentos Marinos/análisis

RESUMEN

High-density polyethylene tablet containers are potentially very suitable for recycling, but no data are publicly available on active pharmaceutical ingredients' (API) residues in empty containers and if they affect the recyclability of pharmaceutical packaging. Plastic tablet containers represented 15 % of pharmaceutical primary packages sold in Finland in 2020 and 2021, equalling 350 tons of plastic per year. We studied the residues of six APIs remaining or adsorbed inside plastic tablet containers. The effects of tablet coating and usage in dose-dispensing services versus households on the API residues, and rinsing water's ability to remove the residues were evaluated. Up to 940,000 µg/kg of carbamazepine was detected in a container of uncoated carbamazepine tablets. The residues from coated tablets containing the other five APIs were 2.4-6,100 µg/kg. Ten times higher paracetamol residues were obtained in containers from household use than from a dose-dispensing unit. Rinsing can remove most API residues, but it leads to environmental emissions. For example, rinsing water can double carbamazepine emissions from a Finnish wastewater treatment plant where plastic packaging waste effluents are processed. Considering the API concentrations, decreasing residues by rinsing and dilution with other plastic packaging waste, the residues of the studied APIs are not considered an obstacle to the recycling of plastic tablet containers. However, further research is needed on more toxic APIs and the fate of APIs in the plastics recycling process.

Asunto(s)

Plásticos , Reciclaje , Comprimidos , Reciclaje/métodos , Finlandia , Plásticos/análisis , Plásticos/química , Embalaje de Medicamentos , Residuos de Medicamentos/análisis , Carbamazepina/análisis , Preparaciones Farmacéuticas/análisis , Ambiente

RESUMEN

Sulfonamides are not only widely applied in clinics but also highly valued in animal husbandry. Recently, it has become common for sulfonamide residues to exceed the standard limits in food, which can affect human health. Current regulations limit these residues. Therefore, we constructed a new limit test method to rapidly determine the levels of sulfonamide residues. Six sulfonamides were detected using the latest method called TLC-SERS, namely, sulfamethasone (A), sulfamethazine (B), sulfadoxine (C), sulfamethoxydiazine (D), sulfamethoxazole (E), and sulfathiazole (F). The optimal conditions for SERS detection were investigated for these six drugs, and the separation effects of different TLC spreaders on them were compared. Then, we successfully established a separation system using dichloromethane-methanol-ammonia in a ratio of 5:1:0.25 (v/v/v), which provided good separation effects on the six drugs. The residues were preliminarily separated via TLC. A silver sol solution was added to the spot on the silica gel G plate at the corresponding specific shift values, and SERS detection was performed. The sample solution was placed on the spot under a 532 nm laser, and the SERS spectrum was collected and analyzed for the six sulfonamides. The results showed obvious variations in the SERS spectrum among the six sulfonamides, with the LODs being 12.5, 6.4, 6.3, 7.1, 18.8, and 6.2 ng/mL from A to F, respectively, and an RSD of <3.0%. Within 48 h, the SERS signal for each sulfonamide drug was kept stable, with an RSD of <3.0%. The detection results of 20 samples using the TLC-SERS method were consistent with those obtained by UPLC-MS/MS. The established TLC-SERS method is simple and fast, providing a useful reference for the rapid detection of residue limits in food.

Asunto(s)

Espectrometría Raman , Sulfonamidas , Sulfonamidas/análisis , Cromatografía en Capa Delgada/métodos , Espectrometría Raman/métodos , Contaminación de Alimentos/análisis , Análisis de los Alimentos/métodos , Residuos de Medicamentos/análisis , Límite de Detección , Animales

RESUMEN

Antibiotic residues are widely recognized as major pollutants in the aquatic environment on a global scale. As a significant class of pharmaceutically active compounds (PhACs), antibiotics are extensively consumed worldwide. The primary sources of these residues include hospitals, municipal sewage, household disposal, and manures from animal husbandry. These residues are frequently detected in surface and drinking waters, sewage effluents, soils, sediments, and various plant species in countries such as China, Japan, South Korea, Europe, the USA, Canada, and India. Antibiotics are used medicinally in both humans and animals, with a substantial portion excreted into the environment as metabolites in feces and urine. With the advancement of sensitive and quantitative analytical techniques, antibiotics are consistently reported in environmental matrices at concentrations ranging from nanograms per liter (ng/L) to milligrams per liter (mg/L). Agricultural soils, in particular, serve as a significant reservoir for antibiotic residues due to their strong particle adsorption capacities. Plants grown in soils irrigated with PhAC-contaminated water can uptake and accumulate these pharmaceuticals in various tissues, such as roots, leaves, and fruits, raising serious concerns regarding their consumption by humans and animals. There is an increasing need for research to understand the potential human health risks associated with the accumulation of antibiotics in the food chain. The present reviews aims to shed light on the rising environmental pharmaceutical contamination concerns, their sources in the environment, and the potential health risks as well as remediation effort. To discuss the main knowledge gaps and the future research that should be prioritized to achieve the risk assessment. We examined and summarized the available data and information on the antibiotic resistance associated with antibiotic residues in the environment. As studies have indicated that vegetables can absorb, transport, and accumulate antibiotics in edible parts when irrigated with wastewater that is either inadequately treated or untreated. These residues and their metabolites can enter the food chain, with their persistence, bioaccumulation, and toxicity contributing to drug resistance and adverse health effects in living organisms.

Asunto(s)

Antibacterianos , Contaminantes Químicos del Agua , Antibacterianos/análisis , Contaminantes Químicos del Agua/análisis , Humanos , Medición de Riesgo , Animales , Residuos de Medicamentos/análisis , Monitoreo del Ambiente

RESUMEN

A new sensitive method of liquid chromatography-tandem mass spectrometry (LC-MS/MS) analysis for nine fasciolicides (closantel, rafoxanide, oxyclozanide, niclosamide, nitroxinil, ioxynil, 4-nitro-3-(trifluoromethyl)phenol, salicylanilide, and triclabendazole) and three metabolite residues (ketotriclabnedazole, triclabendazole sulfone, and triclabendazole sulfoxide) in milk and infant formula was established. The samples were extracted and purified through solid-phase extraction and analyzed using LC-MS/MS. The proposed method demonstrated high accuracy (the average recoveries ranged from 70.5 % to 107.4 %) and high sensitivity (the limits of quantification ranged from 1.0 to 25.0 µg/kg). This method was successfully applied to determine nine fasciolicides and three metabolite residues in 45 milk and infant formula, providing technical support for the safety and quality evaluation of dairy products.

Asunto(s)

Contaminación de Alimentos , Fórmulas Infantiles , Leche , Extracción en Fase Sólida , Espectrometría de Masas en Tándem , Espectrometría de Masas en Tándem/métodos , Extracción en Fase Sólida/métodos , Fórmulas Infantiles/química , Leche/química , Animales , Cromatografía Liquida/métodos , Contaminación de Alimentos/análisis , Humanos , Lactante , Reproducibilidad de los Resultados , Residuos de Medicamentos/análisis , Límite de Detección

RESUMEN

Norfloxacin is an antibacterial compound that belongs to the fluoroquinolone family. Currently, hyperspectral imaging (HSI) for the detection of antibiotic residues focuses mostly on individual systems. Attempts to integrate different HSI systems with complementary spectral ranges are still lacking. This study investigates the feasibility of applying data fusion strategies with two HSI techniques (Visible near-infrared and near-infrared) in combination to predict norfloxacin residue levels in mutton. Spectral data from the two spectral techniques were analyzed using partial least squares regression (PLSR), support vector regression (SVR) and stochastic configuration networks (SCN), respectively, and the two data fusion strategies were fused at the data level (low-level fusion) and feature level (middle-level fusion, mid-level fusion). The results indicated that the modeling performance of the two fused datasets was better than that of the individual systems. Mid-level fusion data achieved the best model based on uninformative variable elimination (UVE) combined with SCN, in which the determination coefficient of prediction set (R2p) of 0.9312, (root mean square error of prediction set) RMSEP of 0.3316 and residual prediction deviation (RPD) of 2.7434, in comparison with all others. Therefore, two HSI systems with complementary spectral ranges, combined with data fusion strategies and feature selection, could be used synergistically to improve the detection of norfloxacin residues. This study may provide a valuable reference for the non-destructive detection of antibiotic residues in meat.

Asunto(s)

Norfloxacino , Espectroscopía Infrarroja Corta , Norfloxacino/análisis , Espectroscopía Infrarroja Corta/métodos , Imágenes Hiperespectrales/métodos , Análisis de los Mínimos Cuadrados , Antibacterianos/análisis , Máquina de Vectores de Soporte , Residuos de Medicamentos/análisis

RESUMEN

BACKGROUND: Lincomycin (LIN) is extensively used for treating diseases in livestock and promoting growth in food animal farming, and it is frequently found in both the environment and in food products. Currently, most of the methods for detecting lincomycin either lack sensitivity and precision or require the use of costly equipment such as mass spectrometers. RESULT: In this study, we developed a reliable high-performance liquid chromatography-ultraviolet detection (HPLC-UVD) method and used it to detect LIN residue in 11 types of matrices (pig liver and muscle; chicken kidney and liver; cow fat, liver and milk; goat muscle, liver and milk; and eggs) for the first time. The tissue homogenates and liquid samples were extracted via liquid-liquid extraction, and subsequently purified and enriched via sorbent and solid phase extraction (SPE). After nitrogen drying, the products were derivatized with p-toluene sulfonyl isocyanic acid (PTSI) (100 µL) for 30 min at room temperature. Finally, the derivatized products were analyzed by HPLC at 227 nm. Under the optimized conditions, the method displayed impressive performance and demonstrated its reliability and practicability, with a limit of detection (LOD) and quantification (LOQ) of LIN in each matrix of 25-40 µg/kg and 40-60 µg/kg, respectively. The recovery ranged from 71.11% to 98.30%. CONCLUSIONS: The results showed that this method had great selectivity, high sensitivity, satisfactory recovery and cost-effectiveness-fulfilling the criteria in drug residue and actual detection requirements-and proved to have broad applicability in the field of detecting LIN in animal-derived foods.

Asunto(s)

Lincomicina , Cromatografía Líquida de Alta Presión/métodos , Animales , Lincomicina/análisis , Análisis de los Alimentos/métodos , Leche/química , Porcinos , Pollos , Límite de Detección , Contaminación de Alimentos/análisis , Reproducibilidad de los Resultados , Análisis Costo-Beneficio , Cabras , Bovinos , Huevos/análisis , Residuos de Medicamentos/análisis

RESUMEN

The application of biosolids, manure, and slurry onto agricultural soils and the growing use of treated wastewater in agriculture result in the introduction of human and veterinary pharmaceuticals to the environment. Once in the soil environment, pharmaceuticals may be taken up by crops, resulting in consequent human exposure to pharmaceutical residues. The potential side effects of pharmaceuticals administered in human medicine are widely documented; however, far less is known regarding the risks that arise from incidental dietary exposure. The aim of this study was to evaluate human exposure to pharmaceutical residues in crops and assess the associated risk to health for a range of pharmaceuticals frequently detected in soils. Estimated concentrations of carbamazepine, oxytetracycline, sulfamethoxazole, trimethoprim, and tetracycline in soil were used in conjunction with plant uptake and crop consumption data to estimate daily exposures to each compound. Exposure concentrations were compared to Acceptable Daily Intakes (ADIs) to determine the level of risk. Generally, exposure concentrations were lower than ADIs. The exceptions were carbamazepine, and trimethoprim and sulfamethoxazole under conservative, worst-case scenarios, where a potential risk to human health was predicted. Future research therefore needs to prioritize investigation into the health effects following exposure to these compounds from consumption of contaminated crops.

Asunto(s)

Productos Agrícolas , Contaminantes del Suelo , Humanos , Productos Agrícolas/química , Contaminantes del Suelo/análisis , Medición de Riesgo , Residuos de Medicamentos/análisis , Exposición Dietética , Preparaciones Farmacéuticas/análisis

RESUMEN

To achieve rapid detection of enramycin in feed, we employed the competitive inhibition method to develop a colloidal gold immunochromatographic test strip based on the anti-enramycin A monoclonal antibody (anti-Er.A-mAb). Colloidal gold probes were prepared with a laboratory-prepared high-purity anti-Er.A-mAb. The effects of pH, antibody titer, and antigen concentration (test line) on the test strip performance were investigated. The colloidal gold test strip prepared with 8 µL potassium carbonate addition, 4 µg/mL antibody, 1.0 mg/mL antigen (test line), and 3 µL gold-labeled antibody showed acceptable specificity and a low limit of detection. The test strip showed the detection limit of 25 ng/mL for enramycin A, with a linear range of 25-300 ng/mL. The experiments on the feed with positive sample addition proved that the test strip had good repeatability and was more sensitive than high-performance liquid chromatography, being applicable for the rapid detection of enramycin in large batches of feed samples.

Asunto(s)

Alimentación Animal , Anticuerpos Monoclonales , Cromatografía de Afinidad , Oro Coloide , Oro Coloide/química , Anticuerpos Monoclonales/inmunología , Anticuerpos Monoclonales/química , Cromatografía de Afinidad/métodos , Alimentación Animal/análisis , Nebramicina/análisis , Nebramicina/análogos & derivados , Contaminación de Alimentos/análisis , Residuos de Medicamentos/análisis

RESUMEN

An integrated method combining solid-phase extraction (SPE) with ultra-performance liquid tandem mass spectrometry (UPLC-MS/MS) has been established for quantifying bacitracin (BTC), bacitracin zinc (BZ), and bacitracin methylene disalicylate (BMD) in animal feed. A pretreatment procedure that can effectively, quickly, and simultaneously extract and purify BTC, BZ, or BMD in feed was developed for the first time through the optimization of extraction and SPE conditions. After extraction with acetonitrile + methanol + 15 % ammonia solution (1:1:1, v:v:v) and dilution with EDTA solution (1.5 mmol/L, pH 7.0), a SPE procedure was carried out with C18 cartridge. Following LC-MS/MS analysis utilized a Waters Peptide BEH C18 column with a gradient elution of 0.1 % formic acid in water/acetonitrile with. This method demonstrated a strong linear correlation (R2 > 0.9980) across a 0.01-1.0 mg/L concentration span, based on a matrix-matched standard curve. Satisfactory recoveries of BTC (bacitracin A, B1, B2, and B3), BZ, and BMD in different feeds were obtained from 80.7 % to 108.4 %, with relative standard deviations below 15.7 %. Low limits of quantification ranging within 7.2-20 µg/kg were achieved for bacitracin A, B1, B2, and B3. This method provided an effective and reliable detection method to prevent the addition of BTC and different BTC formulations in feeds.

Asunto(s)

Alimentación Animal , Bacitracina , Límite de Detección , Espectrometría de Masas en Tándem , Bacitracina/análisis , Espectrometría de Masas en Tándem/métodos , Alimentación Animal/análisis , Cromatografía Líquida de Alta Presión/métodos , Modelos Lineales , Reproducibilidad de los Resultados , Extracción en Fase Sólida/métodos , Salicilatos/análisis , Animales , Residuos de Medicamentos/análisis

RESUMEN

Background: Antibiotic residues that come from food of animal origin, such as broiler chicken, have a variety of consequences on human health and increase the likelihood of antibiotic resistance. Lincomycin residue investigations in broiler chicken especially in plasma broiler chicken should be undertaken utilizing the validation method analysis. Aim: The purpose of this study is to determine the high-performance liquid chromatography (HPLC) as a validation method for calculating the residual concentration of lincomycin in broiler chicken blood plasma and compare it with the minimum Inhibitor Concentration (MIC) and Maximum Residue Limits (MRLs) standards for lincomycin. Methods: Thirty-five-day-old broiler chickens cobb 700 were weighed and randomly allocated to and separated into control (placebo) and six treatment groups of varying doses and duration. The treatment group's suggested dosage of lincomycin was 50, 100, or 150 mg/kg/day given to 18-day-old chicken, along with drinking water for a week (A group) and 2 weeks (P group). Lincomycin levels in blood plasma were validated using HPLC. The residual lincomycin concentrations 24 hours and 1 week after injection were compared to the lincomycin MIC and the Indonesian National Standard of MRL. Result: The validation of linscomycin reveals a linear value in blood plasma with an R2 of 0.9983. Precision and accuracy levels indicate promising results for detecting lincomycin. The retention duration for 100 µg/ml lincomycin was 10.0-10.5 minutes. Lincomycin had LOD and LOQ values of 13.98 and 4.86 µg/ml, respectively. After 1 week of dosing at 50 and 100 mg/kg dosages, lincomycin residue detection was 0.00, which was below the MRL criterion of <0.1 ppm. The study found that the residual concentration of 150 mg/kg dosages for a week and 100/150 mg/kg doses for 2 weeks above the lincomycin MIC limits against Mycoplasma synoviae, Staphylococcus aureus, and Salmonella enteritidis. Conclusion: Lincomycin detection by HPLC in chicken blood plasma showed promising results in terms of linearity, accuracy, precision, specificity, and sensitivity. Lincomycin administration for 1 week at doses of 50 and 100 mg/kg resulted in the lowest residual concentration below the lincomycin MIC and MRL standards.

Asunto(s)

Antibacterianos , Pollos , Lincomicina , Animales , Lincomicina/sangre , Lincomicina/análisis , Pollos/sangre , Cromatografía Líquida de Alta Presión/veterinaria , Antibacterianos/sangre , Antibacterianos/análisis , Antibacterianos/administración & dosificación , Antibacterianos/farmacocinética , Residuos de Medicamentos/análisis , Reproducibilidad de los Resultados