[Analysis of pesticide multiresidues in rice by gas chromatography-mass spectrometry coupled with solid phase extraction].

A new analytical method was developed to simultaneously determine multiple pesticide residues in rice including organophosphorus, organochlorine, carbamate and pyrethroid. First, the solvents for pesticide extraction were selected for optimization. Eight solvents were screened to find that the extraction efficiency with dichloromethane was the best. Second, clean-up was performed by solid phase extraction using a Florisil cartridge. Various mixtures of hexane and acetone were tested to show that the mixture of hexane-acetone (4:1, v/v) had the best performance. The clean-up helped the sample purification significantly. The prepared sample was analyzed using gas chromatography-mass spectrometry (GC-MS) in selected ion monitoring (SIM) mode. The pesticides were identified with retention time and selected ions and their relative abundances, and they were quantified based on extract of spiking standards in a blank sample. The limits of detection (LODs) were evaluated on the values of the lower concentration fortified sample under the signal-to-noise ratio of 3:1. The recoveries and relative standard deviations (RSDs) were checked by adding pesticide standard solution at two levels to untreated samples, and the triplicate analysis of the samples were carried out for each spiked level. The LODs were at microg/kg level. The average recoveries of most pesticides were from 75% to 120 %. The RSDs were less than 10.4% (n = 3). These results indicated that this method is simple, rapid, sensitive for the simultaneous determination requirements of multiple pesticide residues in rice.