Automated trace enrichment for screening and/or determination of primary, secondary and tertiary amphetamines in biological samples by liquid chromatography

Abstract

A rapid and simple liquid chromatographic method for the automated determination of amphetamines in biological fluids was developed. The proposed procedure is based on the injection of 250 microL of sample into a 20 x 2.1 mm id precolumn (packed with a 30 microns Hypersil C18 stationary phase) for enrichment and purification of the analytes. Next, the analytes are transferred to a 5 microns LiChrospher 100 RP18, 125 x 4 mm id analytical column for their separation under reversed-phase conditions. Water was used to eliminate the matrix components from the precolumn and a 0.2 M phosphate buffer (pH 3) containing 2% triethylamine was the mobile phase for the resolution of the amphetamines. The UV detector was set at 210 nm. The method was applied to the determination of different primary, secondary and tertiary amphetamines in plasma and urine: beta-phenylethylamine, norephedrine, ephedrine, N-methylpseudoephedrine, pseudoephedrine, N-methylephedrine, amphetamine, 3-phenylpropylamine and methamphetamine. The method provides satisfactory linearity and reproducibility within the tested concentration range (1.0-10.0 micrograms mL-1) and limits of detection of 50-500 ng/mL-1.

Development and evaluation of an efficient HPLC/MS/MS method for the simultaneous determination of pseudoephedrine and cetirizine in human plasma: Application to Phase-I pharmacokinetic study

“…Many methods exit for pseudoephedrine quantification in human plasma including HPLC with ultraviolet (HPLC-UV) [1,2] and GC [3]. A liquid chromatography-tandem mass spectrometry [4,5] was reported to determine the plasma level of pseudoephedrine, but the extraction recovery was all less than 80%.…”

Sensitive bioassay for the simultaneous determination of pseudoephedrine and cetirizine in human plasma by liquid-chromatography–ion trap spectrometry

“…Several gas chromatographic [4,5] and high performance liquid chromatographic (HPLC) [6][7][8][9][10] methods have been described for determination of pseudoephedrine in plasma. The limit of quantitation (LOQ) of HPLC assays ranges from 10 to 50 ng/ml.…”

“…The limit of quantitation (LOQ) of HPLC assays ranges from 10 to 50 ng/ml. Sample preparation is performed by liquid extraction [6,10], solid-phase extraction [7] or column switching [8,9]. Recently, several HPLC [11] and liquid chromatographymass spectrum (LC/MS) [1, 12,13] methods have been reported to detect cetirizine in plasma.…”

Simultaneous quantification of fexofenadine and pseudoephedrine in human plasma by liquid chromatography/tandem mass spectrometry with electrospray ionization: method development, validation and application to a clinical study

“…Various analytical procedures have been reported for separate quantitative determination of fexofenadine or pseudoephedrine in plasma. These include high‐performance liquid chromatography (HPLC) with ultraviolet (UV) detection for pseudoephedrine,6–10 HPLC with fluorescence detection for fexofenadine,11–14 gas chromatography (GC) for pseudoephedrine,15–17 LC/mass spectrometry (MS) for fexofenadine18 and pseudoephedrine,19 and LC/tandem mass spectrometry (MS/MS) for fexofenadine 20, 21…”