Universal method to determine acidic licit and illicit drugs and personal care products in water by liquid chromatography quadrupole time-of-flight (original) (raw)

Method details Many different types of pollutants have been found in environmental compartments as water. Licit and illicit drugs or personal care products are some of the so-called emerging contaminants extensively used by humans [1,2]. A number of analytical methods are already available [3-9] to determine emerging contaminants in environmental matrices at low concentrations. However, these methods are only reported for one type of instrument. In this study, we proposed a procedure to analyse pharmaceuticals, illicit drugs, personal care products and others contaminants on different water matrices through a common method for a triple quadrupole (QqQ) and a quadrupole time-offlight (QqTOF) mass spectrometers. Reagents and materials Acetaminophen, bezafibrate, bisphenol A, butylparaben, chloramphenicol, clofibric acid, diclofenac, ethylparaben, flufenamic acid, gemfibrozil, ibuprofen, indomethacin, methylparaben, naproxen, propylparaben, salicylic acid, thiamphenicol, triclocarban, triclosan and warfarin from Sigma-Aldrich (The Woodlands,Texas, USA) and tetrahydrocannabinol (THC) and 11-nor-9-carboxy-9-tetrahydrocannabinol (THC-COOH) from LoGiCal (Luckenwalde, Germany) were used as target analytes for QqQ analysis. Calibration standards were prepared by serial dilution of the mixed working solution. Stock and working solutions were stored at À20 C in the dark [10]. Water used for preparation of calibration standards and LC-MS mobile phase was purified by an Elix Milli-Q system (Millipore, Billerica, MA, USA). Methanol was purchased from Panreac (Castellar del Vallès, Barcelona, Spain) and formic acid was purchased from Amresco (Solon, OH, USA). Ammonium fluoride was acquired from Alfa Aesar GmbH & Co KG (Karlsruhe, Germany). Extraction procedure (1) Vacuum filter the samples (250 mL) through 0.45 mm retention capacity glass fiber filter of 90 mm diameter by Advantec (Toyo Roshi Kaisha, Ltd., Japan) using a Bücher funnel (with the filter) over a 250 mL Kitasato flask with 400 mbar h À1 Pa À1 of vacuum, to remove solid particles before the solid phase extraction (SPE). (2) Put the Phenomenex Strata-X 33u Polymeric Reversed Phase (200 mg/6 mL) cartridges (Phenomenex, Torrance, Ca, USA) into a 12 port vacuum manifold Supelco Visiprep 57030-U of Sigma-Aldrich (St. Louis, MO, EEUU). (3) Condition the cartridge with 6 mL methanol and 6 mL of Milli-Q water both with 400 mba h À1 Pa À1 vacuum. (4) Pass the samples through the cartridges under previous vacuum at a flow rate of 10 mL min À1. (5) Wash the cartridges with 6 mL of Milli-Q water. (6) Dry the cartridges under vacuum for 15 min. (7) Elute the analytes on a 15 mL Falcon tube VWR