Capillary gas chromatographic determination of Tamoxifen in the presence of a number of antidepressants in urine

Abstract

A capillary gas chromatographic method with flame ionisation detection is described for the determination of Tamoxifen in association with the antidepressants Fluoxetine, Fluvoxamine, and Clomipramine, using Anastrozole as the internal standard. Optimal conditions were investigated: column head pressure (110 kPa), injector and detector temperature (2308C and 2508C, respectively), time and temperature of the splitless step (1.25 min and 808C), injected volume (2 lL), and oven temperature programme. This provided analysis times of under 11 minutes. Good results were obtained for different aspects including stability of the solutions, linearity, accuracy, and precision. Detection limits between 2.4 and 12 lg L -1 were obtained for all the studied compounds. A ruggedness test of the method was carried out using the Plackett-Burman fractional factorial model with a matrix of fifteen experiments. The method which has been developed is easy, rapid and sensitive and has been used to determine Tamoxifen, Fluoxetine, Fluvoxamine, and Clomipramine present at clinically relevant levels in urine. Before GC-FID determination, it was necessary to apply a simple extraction preconcentration step to the urine using a C 18 cartridge with methanol as eluent.

Relevant Issues in the Monitoring and the Toxicology of Antidepressants

“…226 GC combined with detectors such as FID, 227 151 as well as in APC2 mode. 153 When using UV detection, fluvoxamine gives a maximum absorption at 254 nm.…”

Electroanalytical study of fluvoxamine

“…The main disad-vantages of HPLC are the relatively long analysis times and high acquisition and maintenance costs. Several other methods, based on electrophoresis [23,24], micellar electrokinetic capillary chromatography [25], isotachophoresis [26], gas chromatography [27][28][29][30], ultraviolet-visible [31][32][33][34][35][36], infrared [31], and nuclear magnetic resonance [31,37] spectrometry, have also --1 Fig. 1 Chemical structure of FVX been described, mainly for determination of FVX in pharmaceutical products.…”

A method by homemade OH/TSO-PMHS fibre solid-phase microextraction coupling with gas chromatography–mass spectrometry for analysis of antiestrogens in biological matrices

“…At present, many analytical methods have been used to analyze tamoxifen in therapeutic classes and environmental pollution issues, such as high performance liquid chromatography (HPLC) [6], liquid chromatography tandem mass spectrometry (LC/MS/MS) [7][8][9][10], gas chromatography (GC) [11], gas chromatography-mass spectrometry (GC-MS) [12], capillary electrophoresis (CE) [13], capillary electrophoresis-mass spectrometry (CE-MS) [14,15] and so on. So far as CC, there were no reported methods for determination of clomiphene isomers in plasma except HPLC [16][17][18] and liquid chromatography-mass spectrometry (LC-MS) [19].…”