Development of a liquid chromatography-tandem mass spectrometry method with modified QuEChERS extraction for the quantification of mebendazole and its metabolites, albendazole and its metabolites, and levamisole in edible tissues of aquatic animals.

A liquid chromatography-tandem mass spectrometry quantitative method was developed for determining mebendazole and its metabolites, albendazole and its metabolites, and levamisole in muscles of bluntnose black bream, shrimp, eel and turtle based on modified QuEChERS methodology. The method included 2 g of the muscle matrix with 10 mL acetonitrile, and 0.8 g of magnesium sulphate and 0.2 g of sodium chloride for liquid-liquid partitioning. After vortex and centrifugation, the resulting liquid (5.5 mL) was purified by C18 (50 mg) and Al-N (50 mg). The limits of detection were lower than 0.3 µg kg-1 and the limits of quantitation were no more than 1 µg kg-1 for all analytes. The recoveries of the analytes ranged from 80.0% to 113.7% with the relative standard derivation less than 10.0%. The preparation procedure provided efficient extraction and purification that enabled a sensitive and rugged determination of target compounds.

Levamisol: un peligroso adulterante de la cocaína muy presente en nuestro medio / No disponible

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Electromembrane extraction of levamisole from human biological fluids.

Electromembrane extraction coupled with high-performance liquid chromatography (HPLC) and ultraviolet (UV) detection was developed for the determination of levamisole in some human biological fluids. Levamisole migrated from 4 mL of different acidized biological matrices, through a thin layer of 2-nitrophenyl octyl ether containing 5% tris-(2-ethylhexyl) phosphate immobilized in the pores of a porous hollow fiber, into a 20-µL acidic aqueous acceptor solution present inside the lumen of the fiber. The parameters influencing electromigration were investigated and optimized. Within 15 min of operation at 200 V, levamisole was extracted from different biological fluid samples with recoveries in the range of 59-65%, which corresponded to preconcentration factors in the range of 118-130. The calibration curves showed linearity in the range of 0.5-10, 0.2-10 and 0.1-10 µg/mL for plasma, urine and saliva, respectively. Limits of detection of 0.1, 0.07 and 0.05 µg/mL and limits of quantification of 0.5, 0.2 and 0.1 µg/mL were obtained for plasma, urine and saliva, respectively. The relative standard deviations of the analysis were found to be in the range of 5.6-9.7% (n = 3). Electromembrane extraction was successfully processed for determination of levamisole in plasma, urine and saliva samples.

Evaluation of a single step extraction procedure for enzymatic assay of levamisole in calf serum.

A single step extraction procedure for recovery of the anthelmintic drug levamisole (LEV) from aqueous solutions and calf serum was evaluated. Levamisole was extracted from aqueous solutions and calf serum with 1.5 ml of ethyl acetate. After evaporation to dryness, the LEV content of extracts was estimated by measuring LEV inhibition of bovine milk fat globule membrane alkaline phosphatase. Lipid interference with absorbance readings was eliminated by the addition of 1.0 ml of chloroform to the assay mixtures. The recovery of LEV from both aqueous samples and serum samples by this single step extraction procedure coupled with enzymatic assay was 90%. The effective range for serum LEV determination was 0.3 to 20 micrograms/ml.

Metabolism of levamisole, an anti-colon cancer drug, by human intestinal bacteria.

1. Anaerobic incubation of levamisole with human intestinal flora resulted in the formation of three thiazole ring-opened metabolites, namely, levametabol-I, II and III. These new hydroxamic lactam-type metabolites were isolated and characterized by various spectroscopic methods. 2. Various pure cultures of human intestinal bacterial strains were shown, by quantitative h.p.l.c. analysis, to have ring-opening ability. Strong metabolizers include Bacteroides and Clostridium spp. Bacterial mixtures prepared from human faeces showed much greater ability to transform levamisole (74% in 48 h) than any pure strain culture. 3. Greatly decreased levamisole-transforming activity was observed with autoclaved bacterial cultures, and no activity was found with broth medium alone. This indicates that metabolism requires the presence of anaerobic bacteria and involves, at least in part, a non-enzymic process.