Pre-study and in-study validation of a SPE-LC-MS-MS method for the determination of 5-S-cysteinyldopa, a melanoma biomarker, in human plasma |
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Authors: | Martin Gaëlle Mansion François Houbart Virginie Paquet Philippe Rorive Andrée Chiap Patrice Crommen Jacques Servais Anne-Catherine Fillet Marianne |
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Affiliation: | a Laboratory of Analytical Pharmaceutical Chemistry and Bioanalysis, Department of Pharmacy, CIRM, University of Liège, CHU, B36, B-4000 Liège, Belgium b Dermathopathology, CHU, Liège, Belgium c Medical Oncology, CHU, Liège, Belgium d Advanced Technology Corporation (A.T.C.), CHU, B23, Liège, Belgium |
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Abstract: | The incidence of malignant melanona has increased over the past decades, particularly in Caucasian population. This disease presents defavourable prognosis in terms of survey, especially when detection occurs at the metastatic phase. Reliable analytical methods for biomarker determination are thus an interesting tool in pathology detection and follow-up. In this context, a method using SPE-LC-ESI-MS-MS for the determination of 5-S-cysteinyldopa (5-SCD) in human plasma was optimized. The presence of matrix effect was investigated in details while 5-SCD stability was studied according to FDA requirements for the validation of bioanalytical methods. Pre-study and in-study validations of the entire method were then successfully performed by applying the approach based on total measurement error and accuracy profiles over a concentration ranges from 1.6 to 200 ng/ml. Good results with respect to accuracy, trueness and precision were obtained. The maximum risk of observing future measurements falling outside the acceptance limits during routine analysis was also estimated. |
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Keywords: | 5-SCD, 5-S-cysteinyldopa AAPS, American Association of Pharmaceutical Scientists ESI, electrospray ionization DA, food and drug administration LC, liquid chromatography LLOQ, lower limit of quantification MeD, methyldopa MRM, multiple reaction monitoring MS, mass spectrometry SPE, solid phase extraction ULOQ, upper limit of quantification |
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