An analytical multi-residue approach for the determination of semi-volatile organic pollutants in pine needles

Abstract

Vegetation (and pine needles in particular) has been widely used as an alternative to other conventional sampling devices to assess the atmospheric presence of semi-volatile organic contaminants (SVOCs). While most analytical procedures developed focus only on one or two chemical classes, this this work intends to establish a multi-component protocol to quantify brominated flameretardants (BFRs), polychlorinated biphenyls (PCBs), organochlorine pesticides (OCPs), polynuclear aromatic hydrocarbons (PAHs) and one class of contaminant of emerging concern, the synthetic musks fragrances (SMCs). Pine needles extracts were obtained by ultrasonic solvents extraction (USE), and different cleanup approaches using solid-phase extraction (SPE) employing combinations of sorbents and solvents as well as gel permeation chromatography (GPC) were tested. SPE with alumina followed by GCP yielded the best results, with average recoveries over 80%. The application of the method under field conditions was proven by the analysis of naturally contaminated samples from 3 sites of different potential exposure (remote, rural and urban). The total detected concentrations ranged from 0.45 to 0.87 ng g -1 dry weight (dw) for BFRs, 0.35 to 1.01 ng g -1 (dw) for PCBs, 0.36 to 12.2 ng g -1 (dw) for HCB, 245.7 to 967.8 ng g -1 (dw) for PAHs and 20.7 to 277.5 ng g -1 (dw) for SMCs.This methodology is a viable approach for the simultaneous analysis of five different classes of atmospheric pollutants employing less analytical efforts. Moreover, to the author's best knowledge, this is also the first time vegetation 2 is employed in the detection of SMCs.

Method development for gas chromatography‐tandem mass spectrometry analysis of trace level polycyclicaromatic hydrocarbons, alkyl polycyclicaromatic hydrocarbons, polychlorinated biphenyls, and organochlorinepesticides in pine needle specimen

“…Total PAHs were detected in a concentration range of 135.18-411.39 μg/kg. Overall, the total concentrations in the most samples were similar or below the values presented in literature for pine needles, 13,14,[17][18][19][20][21][22]24,25,32 but was higher than those presented in certain literature, 15,23 when no source specific data were compared. Table 1 compares the concentration of total PAHs detected in pine needles in this study with the results of other previous studies.…”

“…The GC method has been widely used to measure PCBs and OCPs in pine needles, [25][26][27][28][29][30][31][32][33] mainly using ECD, 25,28,30,31 but it is not an appropriate measurement method because it is difficult to confirm qualitatively. The analysis of PCB or/and OCP has also been conducted using GC-MS, 27,32 but this method has a high detection limit and requires a large amount of sample. In another study, high resolution (HR) GC-HRMS was used for simultaneous analysis of PCB and PCN, 29 but this equipment is very expensive and difficult to use routinely.…”

“…The GC method has been widely used to measure PCBs and OCPs in pine needles, 25–33 mainly using ECD, 25,28,30,31 but it is not an appropriate measurement method because it is difficult to confirm qualitatively. The analysis of PCB or/and OCP has also been conducted using GC–MS, 27,32 but this method has a high detection limit and requires a large amount of sample. In another study, high resolution (HR) GC–HRMS was used for simultaneous analysis of PCB and PCN, 29 but this equipment is very expensive and difficult to use routinely.…”

Estimation of urban POP and emerging SVOC levels employing Ligustrum lucidum leaves

“…The injection volume was 1 μL in splitless mode and the temperatures of the injector, transfer line, manifold, and ion trap were 300°C, 250°C, 50°C and 250°C, respectively. The identification and quantification of the target compounds was based on the retention times and the relative abundance of the monitored ions (for more details, see Silva et al, 2015) using the selected ion storage (SIS) system of Varian MS workstation v. 6.9.3 software.…”

Solvent-saving approaches for the extraction of siloxanes from pine needles, soils and passive air samplers

“…As a rst attempt, the adaptation of a previously developed protocol 26 based on ultrasonic assisted extraction (USE) followed by cleanup with solid phase extraction (SPE) and gel permeation chromatography (GPC) was tested for pine needles, as this was one of the three matrices in study for which, to our knowledge, there were no reports of VMS analysis and quanti-cation. To set-up the appropriate amount of elution solvent for the SPE cleanup, elution prole assays were established following the SPE protocol described above, extracting pine needles with a total of 100 mL of two solvent mixes that were tested separately (DCM/Hex (1 : 1) and Acet : Hex (1 : 1)), and collecting 10 mL fractions of the eluate.…”