Dispersive-Solid-Phase Extraction Cleanup Integrated to Dispersive Liquid-Liquid Microextraction Based on Solidification of Floating Organic Droplet for Determination of Organochlorine Pesticides in Vegetables

A simple and rapid method applying acetonitrile extraction, dispersive-solid-phase extraction (d-SPE) cleanup, and dispersive liquid-liquid microextraction based on solidification of floating organic droplet (DLLME-SFO) was developed for determination of organochlorine pesticides in vegetables. In order to simplify operation, d-SPE cleanup was integrated to DLLME-SFO concentration procedure, and a protection device for glass tube was applied to achieving high-speed centrifugation. The comparison study between the integrated d-SPE and normal d-SPE showed that the former could shorten the sample preparation time without decrease of cleanup efficiency. Subsequently, the necessity of using a high-centrifugation speed (more than 8603 g) for complete separation of the d-SPE sorbents, water phase, and organic phase was confirmed through turbidity analysis. The recoveries of the proposed method ranged from 77.2 to 112.5%, and the relative standard deviations were less than 15%. The limits of detection were in the range of 0.45 ~ 1.33 μg kg −1 , while the limits of quantitation were from 1.35 to 3.99 μg kg −1 , respectively. Finally, the method was successfully applied to analyze real vegetable samples.