Abstract

We report on the use of hollow fiber liquid-liquid-liquid microextraction (HF-LLLME) followed by corona discharge ion mobility spectrometry for the determination of dextromethorphan and pseudoephedrine in urine and plasma samples. The effects of pH of the donor phase, stirring rate, ionic strength and extraction time on HF-LLLME were optimized. Under the optimized conditions, the linear range of the calibration curves for dextromethorphan in plasma and urine, respectively, are from 1.5 to 150 and from 1 to 100 ng mL−1. The ranges for pseudoephedrine, in turn, are from 30 to 300 and from 20 to 200 ng mL−1. Correlation coefficients are better than 0.9903. The limits of detection are 0.6 and 0.3 ng mL−1 for dextromethorphan, and 8.6 and 4.2 ng mL−1 for pseudoephedrine in plasma and urine samples, respectively. The relative standard deviations range from 6 to 8%.

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