Validation of an analytical method that determines polycyclic aromatic hydrocarbons in water by high performance liquid chromatography

Abstract

High performance liquid chromatography has the ability to separate, identify and quantify the compounds that are present in any sample. The objective of this study was the validation of a chromatographic method that allows to define if it is reliable and reproducible according to the requirements established in ISO 17025:2017, reaching a lower level according to environmental regulations. The validation was carried out in the city of Guayaquil, Ecuador, taking 15 samples in total (natural, potable, domestic and industrial residual water), with the solid phase extraction technique (SPE) in the form of Oasis ®HLB cartridges. For the preparation of the samples, the OASIS cartridge was conditioned by adding 5 ml of HPLC grade dichloromethane, rinsed with 5 ml of HPLC grade methanol and then 5 ml of type I water, 500 ml of sample was charged at 15 ml / min, washed with 5 ml water type I, eluted with 8 ml of dichloromethane (5 ml rinse the bottle and 3 ml in the cartridge), evaporate to dryness to reconstitute with 2 ml of ACN, place in a 2 ml vial. The injection of the extract was performed in the HPLC, being the results automatically integrated by the software. The statistical parameters that were generated as a result are repeatability, intermediate accuracy, uncertainty, veracity, limit of detection and quantification. Concluding that the development of the analytical method allows us to identify 15 PAHs with good resolution and symmetry.