Directly suspended droplet microextraction combined with single drop back-extraction as a new approach for sample preparation compatible with capillary electrophoresis

A simple and novel method of directly suspended droplet microextraction (DSDME) combined with single drop back-extraction prior to capillary electrophoresis (CE) measurement is developed. In this technique, DSDME was firstly carried out under the maximum stirring rate for a desired time. Then, an aqueous droplet as back-extractive phase suspended at the needle tip was immersed in droplet of organic phase for back-extracted. After extraction, the aqueous droplet was transferred into a suitable vial and injected into CE for analysis. Three alkaloids were selected as model compounds for developing and evaluating the method performance. Under the optimum conditions, the enrichment factors ranged from 231 to 524. The relative standard deviations for five replicates were in the range of 4.8–8.1%. The calibration graph was linear in the range of 20–1000 ng mL−1 yielding correlation coefficients higher than 0.9983. The limit of detections varied from 8.1 to 14.1 ng mL−1. Human urine samples were spiked with three alkaloids standard to assess the matrix effects and satisfactory results were obtained. The advantages of this method are simplicity of operation, rapid detection, low cost, high enrichment factor and little solvent consumption.