Abstract
A new analytical method for the simultaneous determination of eight synthetic musks compounds (SMs) including five polycyclic musks (PCMs) and three nitro musks (NMs) was validated for sediment samples based on a simple QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) sample preparation procedure followed by gas chromatography–mass spectrometry (GC–MS). Good analytical performances were obtained for all the target compounds. For the validation of the method, internal calibration (IC) and internal calibration with QuEChERS (ICQ) were compared. Good linearity was obtained for both calibration methods with determination coefficients (R2) ranging between 0.990 for Musk Xylene (MX) and 0.999 for Tonalide (AHTN) with IC and between 0.991 for Musk Ketone (MK) and 0.999 for Traseolide (ATII) with ICQ. The repeatability ranges were 0.1 %–1.9 % with the IC and 0.1 %–2.6 % with the ICQ. The apparent recoveries obtained for SMs in the standard reference sediment (SRM1944) varied in the range of 70 %–98 % and 75 %–103 % in the sediment from the Bizerte Lagoon (Tunisia). The absolute recoveries ranged between 61 % and 92 % for the SRM1944 and between 61 % and 89 % in the sediment from the Bizerte Lagoon. The limits of detection (LOD) calculated for the two main compounds, Galaxolide (HHCB) and Tonalide (AHTN) were 0.3 and 0.1 ng g−1 respectively. The LODs obtained for ADBI (Celestolide), AHMI (Phantolide), ATII (Traseolide), MM (Muks mosken), MK (Musk Ketone) and MX (Musk Xylene) were 0.08, 0.12, 0.03, 0.34, 0.11, 0.08, 0.10 and 0.15 ng g−1 respectively. The levels of ∑SMs in surface sediments from the Bizerte Lagoon ranged from 1.4 to 4.5 ng g−1, which are 1000 times lower that the predicted no effect concentration (PNEC) for marine organisms.
Similar content being viewed by others
References
Anastassiades M, Lehotay SJ, Stajnbaher D, Schenck FJ (2003) Fast and easy multiresidue method employing acetonitrile extraction/partitioning and “dispersive solid-phase extraction” for the determination of pesticide residues in produce. J AOAC Int 86:412–431
Barhoumi B, LeMenach K, Devier MH, Ben Ameur W, Etcheber H, Budzinski H, Driss MR (2013) Polycyclic aromatic hydrocarbons (PAHs) in surface sediments from the Bizerte Lagoon, Tunisia: levels, sources, and toxicological significance. Environ Monit Assess 186:2653–2669
Ben Ameur W, Trabelsi S, El Megdiche Y, Ben Hassine S, Barhoumi B, Hammami B, Eljarrat E, Barceló D, Driss MR (2013) Concentration of polychlorinated biphenyls and organochlorine pesticides in mullet (Mugil cephalus) and sea bass (Dicentrarchus labrax) from Bizerte Lagoon (Northern Tunisia). Chemosphere 90:2372–2380
Brausch JM, Rand GM (2011) A review of personal care products in the aquatic environment: environmental concentrations and toxicity. Chemosphere 82:1518–1532
Brondi SHG, de Macedo AN, Vicente GHL, Nogueira ARA (2011) Evaluation of the QuEChERS method and gas chromatography-mass spectrometry for the analysis pesticide residues in water and sediment. Bull Environ Contam Toxicol 86:18–22
Bruzzoniti MC, Checchini L, De Carlo RM, Orlandini S, Rivoira L, Del Bubba M (2014) QuEChERS sample preparation for the determination of pesticides and other organic residues in environmental matrices: a critical review. Anal Bioanal Chem 406:4089–4116
Burns C, Tripp K (2011) Concentrations of synthetic fragrance chemicals in aquatic systems. SURE Rep 1–11.
Cavalheiro J, Prieto A, Monperrus M, Etxebarria N, Zuloaga O (2013) Determination of polycyclic and nitro musks in environmental water samples by means of microextraction by packed sorbents coupled to large volume injection-gas chromatography–mass spectrometry analysis. Anal Chim Acta 773:68–75
Derouiche A, Sanda YG, Driss MR (2004) Polychlorinated Biphenyls in Sediments from Bizerte Lagoon, Tunisia. Bull Environ Contam Toxicol 73:810–817
Dsikowitzky L, Schwarzbauer J, Littke R (2002) Distribution of polycyclic musks in water and particulate matter of the Lippe River (Germany). Org Geochem 33:1747–1758
Heberer T (2002) Occurrence, fate, and assessment of polycyclic musk residues in the aquatic environment of urban areas: a review. Acta hydrochim hydrobiol 30:227–243
HERA (2004) Human and environmental risk assessment on ingredients of household cleaning products polycyclic musks AHTN (CAS 1506-02-1) and HHCB (CAS 1222-05-05). Environ Sect 2:1–80
Hu X, Zhou Q (2011) Comparisons of microwave-assisted extraction, simultaneous distillation-solvent extraction, soxhlet extraction and ultrasound probe for polycyclic musks in sediments: recovery, repeatability, matrix effects and bioavailability. Chromatographia 74:489–495
Hu Z, Shi Y, Cai Y (2011) Concentrations, distribution, and bioaccumulation of synthetic musks in the Haihe River of China. Chemosphere 84:1630–1635
Kuster M, López de Alda MJ, Hernando MD, Petrovic M, Martín-Alonso J, Barceló D (2008) Analysis and occurrence of pharmaceuticals, estrogens, progestogens and polar pesticides in sewage treatment plant effluents, river water and drinking water in the Llobregat river basin (Barcelona, Spain). J Hydro 358:112–123
Lambropoulou DA, Albanis TD (2007) Methods of sample preparation for determination of pesticide residues in food matrices by chromatography–mass spectrometry-based techniques: a review. Anal Bioanal Chem 389:1663–1683
Lee IS, Kim UJ, Oh JE, Choi M, Hwang DW (2014) Comprehensive monitoring of synthetic musk compounds from freshwater to coastal environments in Korea: with consideration of ecological concerns and bioaccumulation. Sci Total Environ 470–471:1502–1508
Liu N, Shi Y, Li W, Xu L, Cai Y (2014) Concentrations and distribution of synthetic musks and siloxanes in sewage sludge of wastewater treatment plants in China. Sci Total Environ 476–477:65–72
Llompart M, García-Jares C, Salgado C, Polo M, Cela R (2003) Determination of musk compounds in sewage treatment plant sludge samples by solid-phase microextraction. J Chromatogr A 999:185–193
Mzoughi N, Stoichev T, Dachraoui M, El Abed A, Amouroux D, Donard OFX (2002) Inorganic mercury and methylmercury in surface sediments and mussel tissues from a microtidal lagoon (Bizerte, Tunisia). J Coast Conserv 8:141–145
Mzoughi N, Lespes G, Bravo M, Dachraoui M, Potin-Gautier M (2005) Organotin speciation in Bizerte lagoon (Tunisia). Sci Total Environ 349:211–222
Necibi M, Mzoughi N, Yahia MND, Pringault O (2015) Distributions of organochlorine pesticides and polychlorinated biphenyl in surface water from Bizerte Lagoon, Tunisia. Desalin Water Treat 56:1–9.
Peck AM, Linebaugh EK, Hornbuckle KC (2006) Synthetic musk fragrances in Lake Erie and Lake Ontario sediment cores. Environ Sci Technol 40:5629–5635
Picot Groz M, Martinez Bueno MJ, Rosain D, Fenet H, Casellas C, Pereira C, Gomez E (2014) Detection of emerging contaminants (UV filters, UV stabilizers and musks) in marine mussels from Portuguese coast by QuEChERS extraction and GC–MS/MS. Sci Total Environ 493:162–169
Pintado-Herrera MG, González-Mazo E, Lara-Martín PA (2012) Environmentally friendly analysis of emerging contaminants by pressurized hot water extraction–stir bar sorptive extraction–derivatization and gas chromatography–mass spectrometry. Anal Bioanal Chem 405:401–411
Pinto CG, Laespada MEF, Martin SH, Ferreira AMC, Pavón JLP, Cordero BM (2010) Simplified QuEChERS approach for the extraction of chlorinated compounds from soil samples. Talanta 81:385–391
Reiner JL, Kannan K (2011) Polycyclic Musks in water, sediment, and fishes from the Upper Hudson River, New York, USA. Water Air Soil Pollut 214:335–342
Rubinfeld SA, Luthy RG (2008) Nitromusk compounds in San Francisco Bay sediments. Chemosphere 73:873–879
Sumner NR, Guitart C, Fuentes G, Readman JW (2010) Inputs and distributions of synthetic musk fragrances in an estuarine and coastal environment; a case study. Environ Pollut 158:215–222
Vallecillos L, Pocurull E, Borrull F (2015) Influence of pre-treatment process on matrix effect for the determination of musk fragrances in fish and mussel. Talanta 134:690–698
Wu SF, Ding WH (2010) Fast determination of synthetic polycyclic musks in sewage sludge and sediments by microwave-assisted headspace solid-phase microextraction and gas chromatography–mass spectrometry. J Chromatogr A 1217:2776–2781
Zeng X, Mai B, Sheng G, Luo X, Shao W, An T, Fu J (2008) Distribution of polycyclic musks in surface sediments from the Pearl River Delta and Macao Coastal Region, South china. Environ Toxicol Chem 27:18–23
Zhang X, Yao Y, Zeng X, Qian G, Guo Y, Wu M, Fu J (2008) Synthetic musks in the aquatic environment and personal care products in Shanghai, China. Chemosphere 72:1553–1558
Acknowledgments
This work was supported by the Conseil Général des Pyrénées Atlantiques and the French INSU CNRS program. The authors have declared no conflict of interest.
Author information
Authors and Affiliations
Corresponding author
Rights and permissions
About this article
Cite this article
Necibi, M., Lanceleur, L., Mzoughi, N. et al. Determination of Synthetic Musks in Surface Sediment from the Bizerte Lagoon by QuEChERS Extraction Followed by GC-MS. Bull Environ Contam Toxicol 97, 659–669 (2016). https://doi.org/10.1007/s00128-016-1935-z
Received:
Accepted:
Published:
Issue Date:
DOI: https://doi.org/10.1007/s00128-016-1935-z