ABSTRACT
A two-dimensional liquid chromatography system coupled to triple quadrupole tandem mass spectrometer (2D LC-MS/MS) was employed for the determination of fluoxetine (FLU) and norfluoxetine (N-FLU) in colostrum and mature milk by direct sample injection. With a run time of 12â¯min representing a gain in throughput analysis, the validated methods furnished selectivity, extraction efficiency, accuracy, and precision in accordance with the criteria preconized by the European Medicines Agency guidelines. With a linear range of 3.00-150â¯ng/mL for FLU and 4.00-200â¯ng/mL for N-FLU they were applied to the analysis of colostrum and mature milk samples from nursing mothers. The paper discusses the differences and similarity of sample preparation for this two sample matrices. The herein reported methods are an advance in sample preparation procedures providing waste reduction and a sustainable approach.
Subject(s)
Chromatography, Liquid/methods , Colostrum/chemistry , Fluoxetine/analogs & derivatives , Milk, Human/chemistry , Tandem Mass Spectrometry , Calibration , Chromatography, Liquid/standards , Female , Fluoxetine/analysis , Humans , Limit of Detection , Linear Models , Reference Standards , Reproducibility of Results , Tandem Mass Spectrometry/standards , WorkflowABSTRACT
This review presents an update on the use of restricted-access materials (RAMs) for direct injection of biological samples. The fundamental improvements in the preparation of tailored RAMs and the diversity of applications with these phases are presented. Insights into diminishing the matrix effect by the use of RAM supports in methods by LC-MS and into the low number of methods for enantiomeric separations by direct injections of biological samples are addressed. The diversity of systems that incorporate RAMs for selective sample clean-up or fractionation in proteome and peptidome analysis is also covered.