A comprehensive approach to the determination of two benzimidazoles in environmental samples

Among the various pharmaceuticals regarded as emerging pollutants, benzimidazoles – represented by flubendazole and fenbendazole – are of particular concern because of their large-scale use in veterinary medicine and their health effects on aquatic organisms. For this reason, it is essential to have reliable analytical methods which can be used to simultaneously monitor their appearance in environmental matrices such as water, sediment and tissue samples. To date, however, such methods relating to these three matrices have not been available. In this paper we present a comprehensive approach to the determination of both drugs in the mentioned above matrices using liquid chromatography–ion trap mass spectrometry (LC–MS/MS). Special attention was paid to the sample preparation step. The optimal extraction methods were further validated by experiments with spiked water, sediment and fish tissue samples. Matrix effects were established. The following absolute recoveries of flubendazole and fenbendazole were achieved: 96.2% and 95.4% from waters, 103.4% and 98.3% from sediments, and 98.3% and 97.6% from fish tissue samples, respectively. Validation of the LC–MS/MS methods enable flubendazole and fenbendazole to be determined with method detection limits: 1.6 ng L−1 and 1.7 ng L−1 in water samples; 0.3 ng g−1 for both compounds in sediment samples, and 3.3 ng g−1 and 3.5 ng g−1 in tissue samples, respectively. The proposed methods were successfully used for analysing selected pharmaceuticals in real samples collected in northern Poland. There is first data on the concentration in the environment of the target compounds in Poland.