6533b821fe1ef96bd127bad6

RESEARCH PRODUCT

Multivariate optimization of the hollow fibre liquid phasemicroextraction of muscimol in human urine samples

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A liquid phase microextraction based on hollow fibre followed by liquid chromatographic determinationwas developed for the extraction and quantitation of the hallucinogenic muscimol from urine samples.Method applicability on polar hallucinogens was also tested on two alkaloids, a psychedelic hallucinogen,tryptamine and a polar amino acid, tryptophan which exists in its charged state in the entire pH range. Amultivariate design of experiments was used in which a half fractional factorial approach was applied toscreen six factors (donor phase pH, acceptor phase HCl concentration, carrier composition, stirring rate,extraction time and salt content) for their extent of vitality in carrier mediated liquid microextractions.Four factors were deemed essential for the effective extraction of each analyte. The vital factors werefurther optimized for the extraction of single-spiked analyte solutions using a central composite design.When the simultaneous extraction of analytes was performed under universal factor conditions biasedtowards maximizing the enrichment of muscimol, a good composite desirability value of 0.687 wasobtained. The method was finally applied on spiked urine samples with acceptable enrichments of 4.1,19.7 and 24.1 obtained for muscimol, tryptophan and tryptamine respectively. Matrix-based calibrationcurves were used to address matrix effects. The r2values of the matrix-based linear regression predictionmodels ranged from 0.9933 to 0.9986. The linearity of the regression line of the matrix-based calibrationcurves for each analyte was directly linked to the analyte enrichment repeatability which ranged from anRSD value of 8.3–13.1%. Limits of detection for the developed method were 5.12, 3.10 and 0.21 ng mL−1formuscimol, tryptophan and tryptamine respectively. The developed method has proven to offer a viablealternative for the quantitation of muscimol in human urine samples.