A simple and sensitive preconcentration strategy by coupling salting-out assisted liquid-liquid extraction with online three-step stacking for the determination of potent anti-tumour compound vinblastine and its precursor in biological samples by capillary electrophoresis.

A sensitive capillary electrophoresis strategy was developed by combining salting-out assisted liquid-liquid extraction and online three-step stacking to detect trace quantities of antitumour indole alkaloids in complex biological samples. The proposed strategy fully exploits these two technologies such that extraction, online stacking and separation are combined in a fast and efficient manner. First, salting-out assisted liquid-liquid extraction was used to extract three indole alkaloids (vinblastine sulfate, catharanthine sulfate and vindoline) from complex biomasses. An appropriate volume of acetonitrile (ACN) was mixed with a faecal aqueous solution to precipitate proteins. The mixed solution was vortexed, followed by the addition of ammonium sulfate ((NH)SO) to induce two-phase separation. Alkaloids were effectively extracted into the organic phase, which was then subjected to capillary electrophoresis (CE) analysis. The sensitivity of capillary electrophoresis was effectively improved by online three-step stacking. Good linearity of the calibration curve for each indole alkaloid was obtained in the concentration range of 0.1-1 μg/mL. Under optimal conditions, the sensitivity of ordinary injection was increased by up to 2366-fold, confirming the applicability of the proposed strategy for the sensitive determination of trace indole alkaloids in complex biological samples.