Micellar electrokinetic chromatographic screening of letrozole and its metabolite in human urine: validation and robustness/ruggedness evaluation

Electrophoresis
Juana Rodríguez-FloresLorena Muñoz Fernández

Abstract

A simple, rapid, and sensitive method has been proposed and validated to directly quantify letrozole (LE) and its metabolite, bis-4-cyanophenylmethanol (ME) in urine samples (without any additional treatment) by micellar electrokinetic capillary chromatography (MEKC). In an effort to improve the selectivity and sensitivity of the method, the chemical and instrumental parameters were optimized. The best conditions were: 70 mM borate buffer (pH 9.2) and 40 mM SDS as BGE, 25 kV and 20 degrees C as working voltage and temperature, respectively, with hydrodynamic injection for 6 s. The reliability of the proposed method was also proved by means of a validation procedure based on precision, accuracy, linearity, LOD (15 microg/L for both of them) and LOQ studies. Moreover, an innovatory experimental and statistical design approach, upon a Plackett-Burman fractional factorial model, which involves the simultaneous evaluation of the global robustness and ruggedness effects, was applied. As it has been already stated, the proposed method has been successfully used to directly quantify both compounds in human urine samples, without any additional treatment, but the previously reached LOD and LOQ values can be improved by applying an SPE p...Continue Reading

References

Mar 15, 2001·Journal of Pharmaceutical and Biomedical Analysis·Y Vander HeydenD L Massart
Jan 17, 2002·The Journal of Urology·Jay D Raman, Peter N Schlegel
May 5, 2004·Epilepsy & Behavior : E&B·Cynthia Harden, Neil J MacLusky
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