Search Results (5)

A confirmatory, highly selective multi-residue method based on liquid chromatography coupled to hybrid high resolution mass spectrometry (LC-Q-Orbitrap) was developed and validated for the determination of 12 regulated coccidiostats in eggs and muscle. Particularly, ionophore antibiotics (lasalocid, maduramicin, monensin, narasin, salinomycin and semduramicin) and synthetic coccidiostats (diclazuril, halofuginone, nicarbazin as 4,4′-dinitrocarbanilide fraction, robenidine and toltrazuril as toltrazuril-sulphone) were included in the method. The sample preparation consisted in the extraction of the analytes from the matrix with acetonitrile, followed by a clean-up step with Oasis^® PRiME HLB SPE and a defatting procedure with n-hexane. Validation was successfully performed according to Commission Implementing Regulation (EU) 2021/808, starting from 1 µg kg⁻¹. The procedure was verified through the analysis of a certified reference material (CRM) and the occurrence of the residues was assessed in the context of the Italian National Residue Control Plan (NRCP). Full article

Maduramicin ammonium (MAD) is one of the most frequently used anticoccidial agents in broiler chickens. However, the high toxicity and low solubility of MAD limit its clinical application. In this study, MAD-loaded nanostructured lipid carriers (MAD–NLCs) were prepared to overcome the defects of MAD by using highly soluble nanostructured lipid carriers (NLCs). The formulation was optimized via a three-level, three-factor Box–Behnken response surface method. Then, the optimal MAD–NLCs were evaluated according to their hydrodynamic diameter (HD), zeta potential (ZP), crystal structure, encapsulation efficiency (EE), drug loading (DL), in vitro release, and anticoccidial effect. The optimal MAD–NLCs had an HD of 153.6 ± 3.044 nm and a ZP of −41.4 ± 1.10 mV. The X-ray diffraction and Fourier-transform infrared spectroscopy results indicated that the MAD was encapsulated in the NLCs in an amorphous state. The EE and DL were 90.49 ± 1.05% and 2.34 ± 0.04%, respectively, which indicated that the MAD was efficiently encapsulated in the NLCs. In the in vitro study, the MAD–NLCs demonstrated a slow and sustained drug release behavior. Notably, MAD–NLCs had an excellent anticoccidial effect against Eimeria tenella in broiler chickens. In summary, MAD–NLCs have huge potential to form a new preparation administered via drinking water with a powerful anticoccidial effect. Full article

Maduramicin (MAD) is widely introduced into aquatic environments and results in the contamination of fish products. Worryingly, the consumption of MAD-contaminated crayfish (Procambarus clarkii) may induce symptoms of Haff disease. In this study, to monitor this potential contamination and to understand the residue and elimination characteristics of MAD in edible tissues of crayfish, a sensitive and efficient ultra-performance liquid chromatography–tandem mass spectrometry method was developed, validated, and applied. After extraction with acetonitrile and purification by solid-phase extraction column, multiple-reaction monitoring mass spectrometry with positive ionization mode was used to determine MAD’s residues. The limits of detection and of quantification were 6 μg·kg⁻¹ and 20 μg·kg⁻¹, respectively. The fortified recoveries ranged from 74.2% to 110.4%, with relative standard deviation of 1.2% to 10.1%. Furthermore, MAD was completely eliminated after 3 and 5 days from abdominal muscle and hepatopancreas tissues of crayfish, respectively. The maximum residue limits (MRLs) of MAD respectively was 200 μg·kg⁻¹ in muscle and 600 μg·kg⁻¹ in the hepatopancreas, and its withdrawal time in both edible tissues was 25.8 °C·d. Collectively, the results of this study indicate the proposed method is an efficient tool to evaluate the public health risk associated with crayfish consumption. Full article

Maduramicin is a toxic ionophore antibiotic that is isolated from Streptomyces, frequently occurring in an aquatic environment. To understand the potential role of maduramicin in crayfish consumption related Haff disease, a mouse model was established in this study. Two exposure routes of maduramicin in the abdominal muscle and the hepatopancreas tissue homogenates of crayfish were given intragastrically to mice in different doses for seven days. Action changes, clinical symptoms, feed consumption, body weight, blood biochemistry, and histopathology examination of mice were observed and analyzed. In the natural exposure group, relatively low concentration of maduramicin in crayfish muscle and hepatopancreas had no obvious effects on mental state, body weight, blood biochemical indexes, or histologic appearance. However, in the artificial exposure group, with increasing concentrations, maduramicin in crayfish muscle and hepatopancreas homogenates both induced mental sluggishness and weight loss of mice. Blood biochemical examination showed that 3.5 mg·kg⁻¹ and 7 mg·kg⁻¹ maduramicin in crayfish tissue homogenates significantly increased levels of alanine aminotransferase (ALT), aspartate aminotransferase (AST), blood urea nitrogen (BUN), lactate dehydrogenase (LDH), and creatine kinase (CK). Additionally, histopathological examination showed that multiple organs were damaged by maduramicin, including degeneration of liver cells, shedding of renal epithelial cells, and disturbance and partial lysis of myocardial and skeletal muscle filaments in the mice. In summary, maduramicin may not cause Haff disease through contamination of the aquatic environment under normal conditions. Maduramicin can be used as a potential toxin tool to establish a rhabdomyolysis disease animal model for drug development. Full article

A method for the simultaneous determination of robenidine, halofuginone, lasalocid, monensin, nigericin, salinomycin, narasin, and maduramicin residues in eggs by liquid chromatography–tandem mass spectrometry (LC–MS/MS) was developed. The sample preparation method used a combination of liquid–liquid extraction (LLE) and solid-phase extraction (SPE) technology to extract and purify these target compounds from eggs. The target compounds were separated by gradient elution using high-performance liquid chromatography (HPLC) and ultra-performance liquid chromatography (UPLC). Tandem mass spectrometry was used to quantitatively and qualitatively analyze the target compounds via electrospray ionization (ESI⁺) and multiple reaction monitoring mode. The HPLC–MS/MS and UPLC–MS/MS methods were validated according to the requirements defined by the European Union and the Food and Drug Administration. The limits of detection and limits of quantification of the eight coccidiostats in eggs were 0.23–0.52 µg/kg and 0.82–1.73 µg/kg for HPLC–MS/MS, and 0.16-0.42 µg/kg and 0.81-1.25 µg/kg for UPLC–MS/MS, respectively. The eggs were spiked with four concentrations of the eight coccidiostats, and the HPLC–MS/MS and UPLC–MS/MS average recoveries were all higher than 71.69% and 72.26%, respectively. Compared with the HPLC–MS/MS method, utilizing UPLC–MS/MS had the advantages of low reagent consumption, a short detection time, and high recovery and precision. Finally, the HPLC–MS/MS and UPLC–MS/MS methods were successfully applied to detect eight coccidiostats in 40 eggs. Full article