High-throughput dynamic microwave-assisted extraction on-line coupled with solid-phase extraction for analysis of nicotine in mushroom

Abstract

A simple and low-cost high-throughput dynamic microwave-assisted extraction (HTDMAE) device was firstly assembled and validated by the extraction of nicotine in mushroom samples. In this device, a household microwave oven was applied to provide the microwave energy; a vacuum pump was used to deliver the solvent. Compared with traditional dynamic microwave-assisted extraction method, the sample throughput and microwave energy utilization were improved by the HTDMAE, up to 20 samples could be treated simultaneously in 9min. Taking extraction of nicotine in mushroom sample as an example, a method was established with extraction, separation and enrichment of nicotine in a single step by the device on-line coupled with solid-phase extraction (SPE). Nicotine was first extracted from the mushroom samples with water under the action of microwave energy, and then directly introduced into the SPE column which was packed with cation-exchange resins. Subsequently, the nicotine trapped on the resins was eluted with methanol–ammonia (95:5, v/v) and determined by high-performance liquid chromatography. The limit of detection of nicotine obtained is 5.6μgkg−1 in fresh mushroom sample. The recovery of nicotine in mushroom samples is in the range of 87.4–104.0%. The proposed method which significantly reduced the overall analysis time and increased sample throughput should be favored for routine analyse of complex solid sample.