Implementación, validación y aplicación de un nuevo método para la determinación de oxitetraciclina por HPLC en tejido muscular de salmonídeos  <span class="so-article-trans-title" dir="auto"> Translated title: Implementation, validation, and application of a new HPLC method to determine oxytetracycline in salmonid muscle tissue </span>

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Abstract

Se implementa y valida un método para identificar y cuantificar la oxitetraciclina en músculo de salmón, cuantificar los niveles de recuperación de oxitetraciclina y estudiar su fármaco cinética en diferentes órganos de salmones. La implementación correspondió a la detección y cuantificación de residuos del antibiótico en el tejido muscular de salmonídeos. El principio de la metodología HPLC incluyó la determinación de una serie de soluciones representativas de los estándares utilizados en la fortificación de las muestras. El tiempo de retención fue de 5,7 min. La validación del método, busca confirmar y documentar que los resultados entregados por el método implementado sean confiables. Para esto se llevaron a cabo análisis de parámetros tales como: selectividad, precisión, exactitud, sensibilidad e incertidumbre. Los resultados obtenidos señalan que el porcentaje de recuperación, es de un 96%. El coeficiente de correlación (R ) de la curva de calibrado es 0,9946 y el coeficiente de variación 1,86%.

Translated abstract

A method for identifying and quantifying oxytetracycline in salmon muscle, for quantifying oxytetracycline recovery levels, and for studying its pharmacokinetic in different organs of salmonids was implemented and validated. During implementation, antibiotic residues were detected and quantified in salmon muscle tissue. The principle of the HPLC methodology included determining a series of representative solutions of the standards, used to fortify the samples. The retention time was 5.7 min. The validation of the method sought to confirm and document the reliability of the results obtained with this method. For this, several parameters (selectivity, precision, accuracy, sensitivity, uncertainty) were analyzed. The results obtained indicated 96%) recovery. The coefficient of correlation (R ) of the calibration curve was 0.9946 and the coefficient of variation was 1.86%.

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Oxytetracycline sorption to organic matter by metal-bridging.

Allison MacKay, Brian Canterbury (2005)

The sorption of oxytetracycline to metal-loaded ion exchange resin and to natural organic matter by the formation of ternary complexes between polyvalent metal cations and sorbent- and sorbate ligand groups was investigated. Oxytetracycline (OTC) sorption to Ca- and Cu-loaded Chelex-100 resin increased with increasing metal/sorbate ratio at pH 7.6 (OTC speciation: 55% zwitterion, 45% anion). Greater sorption to Cu- than Ca-loaded resin was observed, consistent with the greater stability constants of Cu with both the resin sites and with OTC. Oxytetracycline sorption to organic matter was measured at pH 5.5 (OTC speciation: 1% cation, 98% zwitterion, 1% anion). No detectable sorption was measured for cellulose or lignin sorbents that contain few metal-complexing ligand groups. Sorption to Aldrich humic acid increased from "clean" < "dirty" (no cation exchange pretreatment) < Al-amended < Fe(III)-amended clean humic acid with K(d) values of 5500, 32000, 48000, and 250000 L kg(-1) C, respectively. Calcium amendments of clean humic acid suggested that a portion of the sorbed OTC was interacting by cation exchange. Oxytetracycline sorption coefficients for all humic acid sorbents were well-correlated with the total sorbed Al-plus-Fe(III) concentrations (r(2) = 0.87, log-log plot), suggesting that sorption by ternary complex formation with humic acid is important. Results of this research indicate that organic matter may be an important sorbent phase in soils and sediments for pharmaceutical compounds that can complex metals by the formation of ternary complexes between organic matter ligand groups and pharmaceutical ligand groups.