A simple and automated method to determine macrocyclic musk fragrances in sewage sludge samples by headspace solid-phase microextraction and gas chromatography-mass spectrometry

10.1016/j.chroma.2013.09.03

An automated headspace solid-phase microextraction followed by gas chromatography-mass spectrometry method to determine macrocyclic musk fragrances in wastewater samples

A fully automated method has been developed for determining eight macrocyclic musk fragrances in wastewater samples. The method is based on a headspace solid-phase microextraction (HS-SPME) followed by GC¿MS. Five different fibres (PDMS 7 µm, PDMS 30 µm, PDMS 100 µm, PDMS/DVB 65 µm and PA 85 µm) were tested. The best conditions were achieved when a PDMS/DVB 65 µm fibre was exposed for 45 min in the headspace of 10 mL water samples at 100ºC. Method detection limits were found in the low ng L-1 range between 0.75 ng L-1 and 5 ng L-1 depending on the target analytes. Moreover, under optimized conditions, the method gave good levels of intra-day and inter-day repeatabilities in wastewater samples with relative standard deviations (n=3, 1000 ng L-1) less than 9% and 14%, respectively. The applicability of the method was tested with influent and effluent urban wastewater samples from different wastewater treatment plants (WWTPs). The analysis of influent urban wastewater revealed the presence of most of the target macrocyclic musks with, most notably, the maximum concentration of ambrettolide being obtained in WWTP A (4.36 µg L-1) and WWTP B (12.29 µg L-1) respectively. The analysis of effluent urban wastewater showed a decrease in target analyte concentrations, with exaltone and ambrettolide being the most abundant compounds with concentrations varying between below method quantification limit

Fully Automated ionic liquid-based headspace single drop microextraction followed by GC-MS/MS to determine musks fragances in environmental water samples

10.1016/j.talanta.2012.07.036A fully automated ionic liquid-based headspace single drop microextraction (IL-HS-SDME) procedure has been developed for the first time to preconcentrate trace amounts of ten musk fragrances extensively used in personal care products (six polycyclic musks, three nitro musks and one polycyclic musk degradation product) from wastewater samples prior to analysis by gas chromatography and ion trap tandem mass spectrometry (GC¿IT-MS/MS). Due to the low volatility of the ILs, a large internal diameter liner (3.4 mm i.d.) was used to improve the ILs evaporation. Furthermore, a piece of glass wool was introduced into the liner to avoid the entrance of the ILs in the GC column and a guard column was used to prevent analytical column damages. The main factors influencing the IL-HS-SDME were optimized. For all species, the highest enrichments factors were achieved using 1 µL of 1-octyl-3-methylimidazolium hexafluorophosphate ([OMIM][PF6]) ionic liquid exposed in the headspace of 10 mL water samples containing 300 g L-1 of NaCl and stirred at 750 rpm and 60 °C for 45 min. All compounds were determined by direct injection GC¿IT-MS/MS with a chromatographic time of 19 min. Method detection limits were found in the low ng mL-1 range between 0.010 ng mL-1 and 0.030 ng mL-1 depending on the target analytes. Also, under optimized conditions, the method gave good levels of intra-day and inter-day repeatabilities in wastewater samples with relative standard deviations varying between 3% and 6% and 5% and 11%, respectively (n=3, 1 ng mL-1). The applicability of the method was tested with different wastewater samples from influent and effluent urban wastewater treatment plants (WWTPs) and one potable treatment plant (PTP). The analysis of influent urban wastewater revealed the presence of g

Fully automated determination of macrocyclic musk fragrances in wastewater by microextraction by packed sorbents and large volume injection gas chromatography-mass spectrometry

10.1016/j.chroma.2012.09.049A fully automated method has been developed for the determination of eight macrocyclic musk fragrances in urban wastewater. The procedure includes the enrichment of the analytes by microextraction by packed sorbent (MEPS) followed by large volume injection¿gas chromatography¿mass spectrometry (LVI¿GC¿MS). The main factors in the MEPS technique were optimized. For all of the analytes, the highest enrichment factors were achieved when 4 mL samples were extracted by using C18 MEPS-sorbent and 50 µL of ethyl acetate were used for desorption. The eluate was directly analysed by GC¿MS. Detection limits were found to be between 5 ng L-1 and 10 ng L-1, depending on the target analytes. In addition, under optimized conditions, the method gave good levels of intra-day and inter-day repeatability in wastewater samples with relative standard deviation (RSD) (n = 3, 1000 ng L-1) less than 5% and 9%, respectively. The applicability of the method was tested with wastewater samples from two influent and effluent urban wastewater treatment plants (WWTPs). The analysis of influent urban wastewater revealed the presence of most of the macrocylic musks at concentrations higher than the method quantification limits (MQLs), being the most abundant analyte ambrettolide at 9.29 µg L-1. In addition, the analyses of effluent urban wastewater showed a decrease in the concentrations with macrocyclic musk concentrations of between not detected (n.d.) and 2.26 µg L-1 being detected

Co-occurrence of musk fragrances and UV-filters in seafood and macroalgae collected in European hotspots

In the last decades, awareness regarding personal care products (PCP), i.e. synthetic organic chemicals frequently used in cosmetic and hygienic products, has become a forward-looking issue, due to their persistency in the environment and their potential multi-organ toxicity in both human and wildlife. Seafood is one of the most significant food commodities in the world and, certainly, one of the most prone to bioaccumulation of PCP, what can consequently lead to human exposure, especially for coastal population, where its consumption is more marked. The aim of this work was to evaluate the co-occurrence of musk fragrances and UV-filters in both seafood and macroalgae collected in different European hotspots (areas with high levels of pollution, highly populated and near wastewater treatment plants). Despite the fact that UV-filters were detected in three different kind of samples (mussel, mullet, and clam), in all cases they were below the limit of quantification. Galaxolide (HHCB) and tonalide (AHTN) were the musk fragrances most frequently detected and quantified in samples from the European hotspots. Cashmeran (DPMI) was also detected in most samples but only quantified in two of them (flounder/herring and mullet). The highest levels of HHCB and AHTN were found in mussels from Po estuar

Headspace stir bar sorptive extraction followed by thermal desorption and gas chromatography with mass spectrometry to determine musk fragrances in sludge samples without sample pretreatment

10.1002/jssc.20140004

Sorbent-packed needle microextraction trap for synthetic musks determination in wastewater samples

10.1016/j.talanta.2014.08.016A needle trap (NT) device filled with HF Bondesil-C18 as a sorbent material was evaluated for the dynamic headspace analysis of a family of nine synthetic musks compounds that include two nitro musks, six polycyclic musks (with galaxolide and tonalide as the most widespread used polycyclic musks) and the degradation product of galaxolide (galaxolidone) in wastewater samples. Different parameters affecting the adsorption capacity of the sorbent were studied (e.g. extraction mode, extraction temperature, salt concentration, preincubation time fill and ejection speed or fill volume). Furthermore, injection parameters used with the NT device (e.g. desorption mode, desorption temperature and time) were evaluated to optimize the desorption and transfer of the target compounds into the GC column. Method detection limits obtained with gas chromatography-tandem mass spectrometry (GC-MS/MS) detection were found in the low ng L-1 range, between 2.5 and 10 ng L-1, depending on the target compounds. Moreover, under optimized conditions, the method gave good levels of intra-day and inter-day repeatabilities in wastewater samples with relative standard deviations (n=5, 100 ng L-1) less than 11 and 17%, respectively. The developed method was satisfactorily applied to the analysis of aqueous samples obtained from three wastewater treatment plants. All the polycyclic musks studied were detected in influent samples with cashmeran, galaxolide and tonalide as the most representative compounds. The analysis of effluent wastewater showed a decrease in the concentrations of all of the polycyclic musk detected in influent samples and an increase in the concentration of galaxolidone until a maximum value of 820 ng L-1