Chromatographic methods for the determination of a broad spectrum of UV filters in swimming pool water (original) (raw)
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Research Square (Research Square), 2021
This paper describes an analytical approach based on Solid Phase Extraction (SPE) followed by analysis using liquid and gas chromatography coupled to mass spectrometry detectors for a simultaneous determination of 18 organic UV lters from water samples. Extraction method parameters were optimized: 250 ml of water sample loaded on Chromo-Bond C18 cartridges after adjustment to pH 4 and then eluted with acetonitrile. The mobile phase, the parameters of the mass spectrometer, as well as those of the ionization source were tested to enhance detection sensitivity. During method validation, the extracted target compounds showed good recoveries (> 68%) with acceptable values in terms of repeatability (CV r) and reproducibility (CV R), that were lower than 20%. The validated method was applied to different real water samples collected from different swimming pools located in Lebanon where nine UV lters among the eighteen targets compounds were detected at concentrations up to 1500 µg/L in some samples. Padimate-O and Octocrylene were detected frequently. This study represents the rst available data on the occurrence of UV lter residues in swimming pool in Lebanon opening hence future perspectives to evaluate their degradation by-products and their toxicity on human health and marine ecosystem.
Revista de Chimie, 2020
A liquid chromatography-tandem mass spectrometry (SPE-LC-MS/MS) method was developed and validated for the simultaneous determination of six organic compounds (2-hydroxy benzophenone, 4-hydroxy benzophenone, 2,2�,4,4�-tetrahydroxy benzophenone, 2,4-dyhydroxy benzophenone, 4,4�-dyhydroxy benzophenone, 2,2�-dyhydroxy-4-methoxy-benzophenone) used as UV filters in personal care products used to protect against UV radiation. The major concern about this type of pollutants is due to their persistence and bioaccumulation potential in the environment and aquatic organisms and for their endocrine disruptor properties. Solid phase extraction was used for sample preparation, followed by liquid chromatography tandem mass spectrometry analysis. Benzophenone derivatives were analyzed on a Phenomenex Luna C18 column (150 x 2.0 mm, 3.0 �m) with the mobile phase run in gradient mode with a mixture of aqueous 0.1% formic acid and acetonitrile as the mobile phase components (at a flow rate of 0.2 mL/m...
Chromatographia, 2012
A simple, selective and highly sensitive method was developed and optimized to determine the most commonly used UV filters with endocrine-disrupting potential in water, namely benzophenone-3 (BP-3), octocrylene (OC), ethylhexyl dimethyl p-aminobenzoate (OD-PABA), ethylhexyl methoxycinnamate, ethylhexyl salicylate (EHS) and homosalate (HMS). Samples were extracted by stir bar sorptive extraction followed by liquid desorption (SBSE-LD). The important factors influencing SBSE-LD were optimized. Under optimal conditions, assays were performed on 50 mL of water sample using stir bars (0.5 mm in film thickness, 10 mm in length) at room temperature. The analytes were determined by liquid chromatography-tandem mass spectrometry with triple quadrupole analyzer using atmospheric pressure chemical ionization. The main parameters in HPLC-APCI-MS/MS were also optimized to provide the best performances for all analytes. Moreover, matrix effect was investigated using two methods the postcolumn infusion system and the method of spiked matrices after extraction. As a result, no significant matrix effect on the analysis was observed. The method showed good linearity (R 2 coefficients greater than 0.996 in different water samples after SBSE-LD). Recoveries of the analytes were close to 90%, except for BP-3 (64%) and OC (76%) with relative standard deviation lower than 11%. Detection limits were between 0.6 and 3.3 ng L-1 for all the analytes except for HMS (94 ng L-1) and EHS (114 ng L-1). This methodology was applied to measure UV filters in seawater, river water and wastewater in different sites of Liguria; BP-3 and OC were found in most of the considered samples at rather low concentration level.
TrAC Trends in Analytical Chemistry, 2008
Organic ultraviolet (UV) filters are compounds used to absorb UV radiation and are increasingly being used as a result of growing concern about UV radiation and skin cancer. Their growing use may increase environmental contamination and exposure through the food chain. There is therefore major concern about the environmental fate and potential effect of organic UV filters used in beauty creams, hair sprays, shampoos, and other personal-care products, as well as those added to plastics and other materials to prevent degradation of polymers and pigments. This review describes the processes undergone by these compounds once released into the environment and the instrumental methods based on chromatography and mass spectrometry reported in the literature for their determination in environmental samples. We include concentrations found in the environment (e.g., water, soil, sediments, sludge and biota). The main focus is on metabolites, photodegradates and by-products of wastewater treatment.
Journal of Chromatography A, 2010
For the first time, an automatic sample pre-treatment/detection method is proposed for the multiclass determination of UV filters (namely, benzophenone-3, ethylhexylmetoxycinnamate, butylmethoxydibenzoylmethane and homosalate) in environmental samples. The new methodology comprises in-line solid-phase extraction (SPE) of the target analytes by exploiting the bead injection (BI) concept in a mesofluidic lab-on-valve (LOV) format, with subsequent determination by liquid chromatography (LC). The proposed microanalytical system, using a multisyringe burette as propulsion unit, automatically performed the overall SPE steps, including the renewal of the sorbent in each analytical cycle to prevent sample cross-contamination and the post-extraction adjustment of the eluate composition to prevent chromatographic band broadening effects. In order to expedite the LC separation, a C 18 monolithic column was applied and an accelerated isocratic elution was carried out by using a cationic surfactant as mobile phase additive. The LOV-BI-LC method was proven reliable for handling and analysis of complex matrices, e.g., spiked swimming pool water and seawater, with limits of detection ranging between 0.45 and 3.2 g L −1 for 9 mL sample volume. Linear calibration was attained up to 160 g L −1 for homosalate and up to 35 g L −1 for the other target analytes, with good reproducibility (RSD < 13%, for 5 different SPE columns). The hyphenated scheme is able to process a given sample simultaneously and within the same time frame than the chromatographic separation/determination of the formerly pre-treated sample, providing concentration values every 9 min. Hence, the sample throughput was enhanced up to 33 times when compared with previously reported off-line SPE methods. A drastic reduction in reagent consumption and effluent production was also attained, contributing to the development of an environment-friendly analyzer. (M.A. Segundo). considered contaminants of emerging concern [2,3] and reviews focused on this novel problem have been recently published .
Analytical and Bioanalytical Chemistry, 2011
This work describes an effective, low solvent consumption and affordable sample preparation approach for the determination of eight UV filters in surface and wastewater samples. It involves sorptive extraction of target analytes in a disposable, technical grade silicone disc (5 mm diameter×0.6 mm thickness) followed by organic solvent desorption, large volume injection (LVI), and gas chromatography-mass spectrometry determination. Final working conditions involved overnight extraction of 100-mL samples, containing 10% of methanol, followed by analytes desorption with 0.2 mL of ethyl acetate. The method provides linear responses between the limits of quantification (from 0.003 to 0.040 ng mL −1) and 10 ng mL −1 , an intra-day precision below 13%, and low matrix effects for surface, swimming pool, and treated sewage water samples. Moreover, the extraction yields provided by silicone discs were in excellent agreement with those achieved using polydimethylsiloxane-covered stir bars. Several UV filters were found in surface and sewage water samples, with the maximum concentrations corresponding to octocrylene.
Environmental Chemistry, 2013
Environmental context The increasing use of sun-creams containing UV-filtering chemicals has led to increased inputs of these compounds to the aquatic environment. Chlorinated waters can convert these chemicals into chlorinated products whose toxic effects are of primary concern. To better understand the environmental fate of sun-cream chemicals, we studied the stability of two UV-filtering compounds under varying conditions of pH, chlorine concentration, temperature, dissolved organic matter and solar irradiation. The stability of the UV filters 2-ethylhexyl-4-methoxycinnamate (EHMC) and 4-tert-butyl-4′-methoxydibenzoylmethane (BDM) in chlorinated water was studied. High-performance liquid chromatography (HPLC)-UV-diode array detection (DAD) was used to follow the reaction kinetics of both UV filters and HPLC-tandem mass spectrometry (MS/MS) was used to tentatively identify the major transformation by-products. Under the experimental conditions used in this work both UV filters rea...
Determination of UV filters in river water samples by in-line SPE-CE-MS
ELECTROPHORESIS, 2013
The use of SPE coupled in-line to CE using electrospray MS detection (in-line SPE-CE-ESI-MS) was investigated for the preconcentration and separation of four UV filters: benzophenone-3, 2,2-dihydroxy-4-methoxybenzophenone, 2,4-dihydroxybenzophenone and 2-phenylbenzimidazole-5-sulphonic acid. First, a CE-ESI-MS method was developed and validated using standard samples, obtaining LODs between 0.06 g/mL and 0.40 g/mL. For the in-line SPE-CE-ESI-MS method, three different sorbents were evaluated and compared: Oasis HLB, Oasis MCX, and Oasis MAX. For each sorbent, the main parameters affecting the preconcentration performance, such as sample pH, volume, and composition of the elution plug, and sample injection time were studied. The Oasis MCX sorbent showed the best performance and was used to validate the in-line SPE-CE-ESI-MS methodology. The LODs reached for standard samples were in the range between 0.01 and 0.05 ng/mL with good reproducibility and the developed strategy provided sensitivity enhancement factors between 3400-fold and 34 000-fold. The applicability of the developed methodology was demonstrated by the analysis of UV filters in river water samples.