Hollow fiber-based liquid-phase microextraction combined with on-line sweeping for trace analysis of Strychnos alkaloids in urine by micellar electrokinetic chromatography

A new method for the enrichment of Strychnos alkaloids in biological samples via liquid-phase microextraction (LPME) based on porous polypropylene hollow fibers combined with on-line sweeping in micellar electrokinetic chromatography (MEKC) was developed. Strychnos alkaloids were first extracted from urine sample which was adjusted to alkaline conditions (0.5 mol l−1 NaOH). The unionized analytes were subsequently extracted into 1-octanol impregnated in the pores of hollow fibers, and then into an acidic acceptor solution (100 mmol l−1 H3PO4) inside the hollow fiber. The extract was analyzed directly by on-line sweeping in MEKC. In the method, the compound berberine was used as the internal standard (I.S.) for the improvement of the experimental reproducibility. The calibration curve was linear over a range of 20–200 ng ml−1 for both strychnine and brucine in human urine sample, with a correlation coefficient of 0.996 and 0.997, respectively. The detection limits (S/N = 3:1) for strychnine and brucine were 1 and 2 ng ml−1, respectively. The LPME-sweeping method has been successfully applied to the analysis of strychnine and brucine in real urine sample, indicating that LPME-sweeping-MEKC is a promising combination for analysis of basic drugs present at low levels in some biological matrices.