Barley husk carbon as the fiber coating for the solid-phase microextraction of twelve pesticides in vegetables prior to gas chromatography-mass spectrometric detection

•The barley husk biomaterial carbon (BHBC) was successfully prepared by hydrothermal method.•The BHBC was immobilized onto a stainless steel wire for the SPME of twelve pesticides.•The BHBC fiber had a good extraction capability.

In this work, a barley husk biomaterial was successfully carbonized by hydrothermal method. The carbon had a high specific surface area and good stability. It was coated onto a stainless steel wire through sol-gel technique to prepare a solid-phase microextraction fiber for the extraction of trace levels of twelve pesticides (tsumacide, fenobucarb, indoxacarb, diethofencarb, thimet, terbufos, malathion, thiamethoxam, imidacloprid, buprofezin, acetamiprid, thiamethoxam) from vegetable samples prior to gas chromatography-mass spectrometric (GC-MS) detection. The main experimental parameters that could influence the extraction efficiency such as extraction time, extraction temperature, sample pH, sample salinity, stirring rate, desorption temperature and desorption time, were investigated. Under the optimized conditions, the linearity was observed in the range of 0.2-75.0 μg kg−1 for tomato samples, and 0.3-60.0 μg kg−1 for cucumber samples, with the correlation coefficients (r) ranging from 0.9959 to 0.9983. The limits of detection of the method were 0.01-0.05 μg kg−1 for tomato samples, and 0.03-0.10 μg kg−1 for cucumber samples. The recoveries of the analytes for the method from spiked samples were in the range of 76%-104%, and the precision, expressed as the relative standard deviations, was less than 12%.