Gas chromatographic mass spectrometry determination of geosmin and 2-methylisoborneol off-flavor in Mugil cephalus roe

Botargo is the product of the industrial management of fresh roe of the grey mullet (Mugil cephalus). This food product is actually obtained from wild fish caught in different marine areas around the word. The increasing commercial demand of botargo has brought to carry out different fishing systems, gathering the wild mullet in restricted areas, lagoons, to be caught if necessary. This operating mode has caused the appearance of new problems related to the organoleptic approval by the consumers of fish and derived products, following off-flavor contamination derived from different microorganisms present in the lagoons. The most important off-flavor compounds are represented by 2-methylisoborneol (2-MIB) and geosmin (GSM) which give a muddy/musty smell and flavor to the fish. A simple and easy-to-use GC/MS method for the determination of 2-MIB and GSM has been developed. The method has been validated with the following parameters: instrument limit of detection (LOD) and of quantification (LOQ), precision, recovery, and linearity. The method carried out showed good LOD of 1.0 μg/kg and LOQ 2.0 and 5.0 μg/kg for GSM and 2-MIB, respectively. Validation parameters were in close agreement with those reported in the EC SANCO/12571/2013. Recoveries ranged from 80.2 to 121.4 %, with percent relative standard deviation (RSD%) ranging from 0.6 to 18.6 % in the most unfavorable case. Real sample analysis showed the presence of residues of both off-flavor in all botargo samples analyzed, except for sample S0, while in fresh roe samples, only S7 showed important residues of 2-MIB.