Uptake study in Juncus sp. and Salicornia europaea of six pharmaceuticals by liquid chromatography quadrupole time-of-flight mass spectrometry.

In this work, eight plants of Juncus sp. and ten of Salicornia europaea were used for an uptake assay of pharmaceuticals (flumequine, cirpofloxacin, enrofloxacin, carbamazepine, diclofenac and ibuprofen) by irrigation at three concentration levels: 10 ng mL-1 (low level); 700 ng mL-1 (medium level) and 10 µg mL-1 (high level). Two plants irrigated with pharmaceutical-free water were set up as controls. For each level, two plants were watered every day with 50 mL (Juncus sp.) and every two days with 20 mL (Salicornia europaea) of aqueous solutions containing all the analytes at the described concentrations. Plants irrigated at 10 µg mL-1 were significantly the most affected, whereas the rest of the plants remained, in general, largely displayed no apparent physiological effects throughout the 30 days (Juncus sp.) and 21 days (Salicornia europaea) assays. Leaves and stems were cut every seven days and roots were collected at the end of the assay. The samples were lyophilized, submitted to a microwave assisted extraction using 5 mL of acetonitrile:water mixture (1:1, v/v) and they were analyzed (in triplicate) in a liquid chromatography-quadrupole time of flight mass spectrometry instrument. Most of the analytes were quantified in many of the samples corresponding to the three exposure levels with the highest concentrations obtained at high exposure levels. Ibuprofen was not detected in any sample and enrofloxacin, ciprofloxacin and diclofenac were not detected in the samples from Salicornia europaea.

Liquid chromatography quadrupole time-of-flight mass spectrometry determination of six pharmaceuticals in vegetal biota. Uptake study in Lavandula dentata.

A procedure based on microwave assisted extraction for the determination of 6 pharmaceuticals in samples of Lavandula dentata, Salicornia ramosissima and Juncus sp. by liquid chromatography-quadrupole time of flight mass spectrometry (LC-QTOF/MS) was optimized and validated. Best results were obtained using microwave assisted extraction of 1.0g of homogeneous lyophilized samples and 5mL of a mixture ACN:H2O (1:1 v/v) as extracting solvent. Analytical recoveries ranged from 60 to 107% with relative standard deviation (RSD) lower than 15%. Limits of quantitation (LOQ) for the 6 pharmaceuticals flumequine (FLM), carbamazepine (CBZ), ciprofloxacin (CPR), enrofloxacin (ENR), diclofenac (DCL), and ibuprofen (IBU) were in the range 20.8-125ngg-1. The method was satisfactory applied for an uptake study in Lavandula dentata samples finding quantifying concentrations of FLM and CBZ in roots, leaf and stem.