Single particle-inductively coupled plasma mass spectrometry (SP-ICPMS) is a promising technique able to generate the number based-particle size distribution (PSD) of nanoparticles (NPs) in aqueous suspensions. However, SP-ICPMS analysis is not consolidated as routine-technique yet and is not typically applied to real test samples with unknown composition. This work presents a methodology to detect, quantify and characterise the number-based PSD of Ag-NPs in different environmental aqueous samples (drinking and lake waters), aqueous samples derived from migration tests and consumer products using SP-ICPMS. The procedure is built from a pragmatic view and involves the analysis of serial dilutions of the original sample until no variation in the measured size values is observed while keeping particle counts proportional to the dilution applied. After evaluation of the analytical figures of merit, the SP-ICPMS method exhibited excellent linearity (r2>0.999) in the range (1-25) × 104 particlesmL-1 for 30, 50 and 80nm nominal size Ag-NPs standards. The precision in terms of repeatability was studied according to the RSDs of the measured size and particle number concentration values and a t-test (p = 95%) at the two intermediate concentration levels was applied to determine the bias of SP-ICPMS size values compared to reference values. The method showed good repeatability and an overall acceptable bias in the studied concentration range. The experimental minimum detectable size for Ag-NPs ranged between 12 and 15nm. Additionally, results derived from direct SP-ICPMS analysis were compared to the results conducted for fractions collected by asymmetric flow-field flow fractionation and supernatant fractions after centrifugal filtration. The method has been successfully applied to determine the presence of Ag-NPs in: lake water; tap water; tap water filtered by a filter jar; seven different liquid silver-based consumer products; and migration solutions (pure water and sweat simulant) from plasters. Results obtained by SP-ICPMS were supported by transmission electron microscopy and energy dispersive spectroscopy characterisation, suggesting that the proposed methodology can be applied as a positive screening test in the simultaneous quantification and size characterisation of Ag-NPs in samples of environmental interest.

This work describes the analysis of 15 pharmaceutical compounds, belonging to different therapeutic classes (anti-inflammatory/analgesics, lipid regulators, antiepileptics, β-blockers and antidepressants) and with diverse physical–chemical properties, in Spanish soils with different farmland uses. The studied compounds were extracted from soil by ultrasound-assisted extraction (UAE) and determined, after derivatization, by gas chromatography with mass spectrometric detection (GC–MS). The limits of detection (LODs) ranged from 0.14 ng g⁻¹ (naproxen) to 0.65 ng g⁻¹ (amitriptyline). At least two compounds where detected in all samples, being ibuprofen, salicylic acid, and paracetamol, the most frequently detected compounds. The highest levels found in soil were 47 ng g⁻¹ for allopurinol and 37 ng g⁻¹ for salicylic acid. The influence of the type of crop and the sampling area on the levels of pharmaceuticals in soil, as well as their relationship with soil physical–chemical properties, was studied. The frequent and widespread detection of some of these compounds in agricultural soils show a diffuse contamination, although the low levels found do not pose a risk to the environment or the human health.

A multiresidue method was developed for the simultaneous determination of 31 emerging contaminants (pharmaceutical compounds, hormones, personal care products, biocides, and flame retardants) in aquatic plants. Analytes were extracted by ultrasound-assisted matrix solid-phase dispersion (UA-MSPD) and determined by gas chromatography-mass spectrometry after sylilation, The method was validated for different aquatic plants (Typha angustifolia, Arundo donax, and Lemna minor) and a semiaquatic cultivated plant (Oryza sativa) with good recoveries at concentrations of 100 and 25 ng g⁻¹ wet weight, ranging from 70 to 120 %, and low method detection limits (0.3 to 2.2 ng g⁻¹ wet weight). A significant difference of the chromatographic response was observed for some compounds in neat solvent versus matrix extracts, and therefore, quantification was carried out using matrix-matched standards in order to overcome this matrix effect. Aquatic plants taken from rivers located at three Spanish regions were analyzed, and the compounds detected were parabens, bisphenol A, benzophenone-3, cyfluthrin, and cypermethrin. The levels found ranged from 6 to 25 ng g⁻¹ wet weight except for cypermethrin that was detected at 235 ng g⁻¹ wet weight in O. sativa samples.

In this work, an analytical method was developed for the determination of pharmaceutical drugs in biosolids. Samples were extracted with an acidic mixture of water and acetone (1:2, v/v) and supported liquid extraction was used for the clean-up of extracts, eluting with ethyl acetate:methanol (90:10, v/v). The compounds were determined by gas chromatography-tandem mass spectrometry using matrix-match calibration after silylation to form their t-butyldimethylsilyl derivatives. This method presents various advantages, such as a fairly simple operation for the analysis of complex matrices, the use of inexpensive glassware and low solvent volumes. Satisfactory mean recoveries were obtained with the developed method ranging from 70 to 120% with relative standard deviations (RSDs) ≤ 13%, and limits of detection between 0.5 and 3.6 ng g(-1). The method was then successfully applied to biosolids samples collected in Madrid and Catalonia (Spain). Eleven of the sixteen target compounds were detected in the studied samples, at levels up to 1.1 μg g(-1) (salicylic acid). Ibuprofen, caffeine, paracetamol and fenofibrate were detected in all of the samples analyzed.