Solid-phase microextraction-liquid chromatography-mass spectrometry applied to the analysis of insecticides in honey

An approach based on solid-phase microextraction-liquid chromatography-mass spectrometry (SPME-LC-MS) has been developed for determining 12 insecticides (bromophos ethyl, chlorpyrifos methyl, chlorpyrifos ethyl, diazinon, fenoxycarb, fonofos, phenthoate, phosalone, pirimiphos methyl, profenofos, pyrazophos, and temephos) in honey. The influence of several parameters on the efficiency of the SPME was systematically investigated. Under optimal conditions, the procedure provided excellent linearity (>0.990), detection and quantification limits (between 0.001 and 0.1 microg g(-1) and between 0.005 and 0.5 microg g(-1), respectively), and precision (<19% at the quantification limits and from 6 to 14% at ten times higher concentrations). However, recoveries were not so good, ranging from 19 to 92%. Honey samples were found that were contaminated with bromophos ethyl, diazinon, fonofos, pirimiphos ethyl, pyrazophos, and temephos at estimated concentrations from 6.2 +/- 1.2 to 19 +/- 3 ng g(-1).