Monitoring of Polycyclic Aromatic Hydrocarbon Levels in Mussels (Mytilus galloprovincialis) from Aquaculture Farms in Central Macedonia Region, Greece, Using Gas Chromatography–Tandem Mass Spectrometry Method
Abstract
:1. Introduction
2. Results and Discussion
2.1. Extraction
2.2. Clean-Up
2.3. Optimization of Mass Spectrometry and Chromatography Parameters
2.4. Validation Parameters
2.5. Levels of PAHs in Mussels
2.5.1. Concentration Levels
2.5.2. Distribution Patterns and Diagnostic Ratios for PAH Origin
3. Materials and Methods
3.1. Collection of Mussels
3.2. Materials and Reagents
3.3. Preparation of Samples
3.3.1. Extraction of PAHs
3.3.2. Clean Up
3.4. Instrumental Analysis
Compound | Abbrev. | Rt | Precursor Ion | Quantifier Ion (m/z) | Qualifier Ion (m/z) | Collision Cell Energy (eV) |
---|---|---|---|---|---|---|
Naphthalene | Na | 2.75 | 127.89 | 128.00 | 102.00 | 15 |
Acenaphthylene | Acl | 3.98 | 151.88 | 152.00 | 126.00 | 22 |
Acenaphthene | Ac | 4.12 | 152.89 | 153.00 | 126.90 | 10 |
Fluorene | Fl | 4.91 | 164.88 | 165.00 | 163.00 | 10 |
Phenanthrene | Phe | 7.82 | 177.90 | 178.00 | 152.00 | 22 |
Anthracene a | An | 7.97 | 177.90 | 178.00 | 152.00 | 22 |
Fluoranthene | Fa | 13.72 | 201.90 | 202.00 | 200.00 | 10 |
Pyrene | Py | 15.37 | 201.90 | 202.00 | 200.00 | 10 |
Benzo[c]fluorene b | BcFl | 17.88 | 215.94 | 215.00 | 189.00 | 30 |
Benz(a)anthracene | BaA | 25.61 | 227.93 | 226.00 | 202.00 | 22 |
Chrysene | Chr | 26.30 | 227.90 | 226.00 | 202.00 | 22 |
Cyclopenta[c,d]pyrene c | Cpp | 25.99 | 225.90 | 226.00 | 224.00 | 22 |
5-methylchrysene c | 5MeChr | 28.19 | 241.93 | 242.00 | 240.00 | 10 |
Benzo[b]fluoranthene | BbFa | 30.91 | 251.90 | 252.00 | 226.00 | 22 |
Benzo[k]fluoranthene d | BkFa | 31.04 | 251.90 | 252.00 | 226.00 | 22 |
Benzo[j]fluoranthene d | BjFa | 31.12 | 251.90 | 252.00 | 226.00 | 22 |
Benzo[e]pyrene | BeP | 32.85 | 251.90 | 252.00 | 226.00 | 22 |
Benzo[a]pyrene | BaP | 33.20 | 251.90 | 252.00 | 226.00 | 22 |
Perylene | Per | 33.99 | 251.90 | 252.00 | 226.00 | 22 |
Indeno(1,2,3-c d)pyrene | IP | 40.17 | 275.86 | 276.00 | 274.00 | 22 |
Dibenzo[a,h]anthracene | DBahA | 40.21 | 277.88 | 278.00 | 252.00 | 22 |
Benzo[g,h,i]perylene | BghiP | 41.19 | 275.87 | 276.00 | 274.00 | 22 |
Dibenzo[a,l]pyrene e | DBalP | 43.90 | 301.85 | 302.00 | 300.00 | 5 |
Dibenzo[a,e]pyrene e | DBaeP | 44.84 | 301.85 | 302.00 | 300.00 | 5 |
Dibenzo[a,i]pyrene e | DBaiP | 45.39 | 301.85 | 302.00 | 300.00 | 5 |
Dibenzo[a,h]pyrene e | DBahP | 45.67 | 301.85 | 302.00 | 300.00 | 5 |
Naphthalene (D8) | Na (D8) | 2.73 | 135.96 | 136.00 | 107.96 | 22 |
Acenaphthylene (D8) | Acl (D8) | 3.93 | 159.93 | 160.00 | 131.97 | 22 |
Acenaphthene (D10) | Ac (D10) | 4.07 | 163.96 | 164.00 | 162.00 | 22 |
Fluorene (D10) | Fl (D10) | 4.86 | 175.96 | 176.00 | 174.00 | 10 |
Phenanthrene (D10) | Phe (D10) | 7.71 | 187.97 | 188.00 | 159.99 | 22 |
Fluoranthene (D10) | Fa (D10) | 13.6 | 211.85 | 210.05 | 208.04 | 10 |
Pyrene (D10) | Py (D10) | 15.24 | 211.99 | 210.07 | 208.03 | 22 |
Benzo(a)anthracene (D12) | BaA (D12) | 25.29 | 240.00 | 236.00 | 212.00 | 22 |
Chrysene (D12) | Chr (D12) | 26.05 | 240.00 | 236.00 | 212.00 | 22 |
Benzo(b)fluoranthene (D12) | BbFa (D12) | 30.77 | 263.96 | 260.00 | 236.00 | 35 |
Benzo(k)fluoranthene (D12) | BkFa (D12) | 30.92 | 263.96 | 260.00 | 236.00 | 35 |
Benzo[a]pyrene (D12) | BaP (D12) | 33.03 | 263.96 | 260.00 | 236.00 | 35 |
Perylene (D12) | Per (D12) | 33.79 | 263.96 | 260.00 | 236.00 | 35 |
Indeno(1,2,3-cd)pyrene (D12) | IP (D12) | 40.06 | 287.93 | 288.07 | 284.00 | 35 |
Dibenz[a,h]anthracene (D14) | DBahA (D14) | 40.08 | 291.95 | 292.00 | 288.00 | 35 |
Benzo[g,h,i]perylene (D12) | BghiP (D12) | 41.1 | 287.93 | 288.07 | 284.00 | 35 |
3.5. Quantification and Quality Assurance
3.6. Statistical Analysis
4. Conclusions
Supplementary Materials
Author Contributions
Funding
Institutional Review Board Statement
Informed Consent Statement
Data Availability Statement
Acknowledgments
Conflicts of Interest
Sample Availability
References
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Target Value | Average | SD | %RSD | %Trueness | |
---|---|---|---|---|---|
Benz(a)anthracene | 2 | 2.37 | 0.17 | 7.23 | 18.67 |
5 | 5.41 | 0.29 | 5.35 | 8.20 | |
Chrysene | 5 | 2.16 | 0.08 | 3.65 | 8.00 |
5 | 4.97 | 0.15 | 3.03 | −0.67 | |
Benzo[b]fluoranthene | 2 | 2.19 | 0.22 | 9.86 | 9.61 |
5 | 5.53 | 0.26 | 4.79 | 10.67 | |
Benzo[a]pyrene | 2 | 2.21 | 0.12 | 5.52 | 10.50 |
5 | 5.58 | 0.13 | 2.26 | 11.69 | |
Σ4PAHs | 8 | 8.94 | 0.15 | 6.57 | 11.69 |
20 | 21.49 | 0.21 | 3.86 | 7.47 |
Sampling Period | Regional Unit of Thessaloniki | Regional Unit of Imathia and Pieria | Regional Unit of Chalkidiki and Serres |
---|---|---|---|
Spring: 21/05/2018–30/05/2018 | S1.spring 9 sampling stations | S2.spring 5 sampling stations | S3.spring 3 sampling stations |
Winter: 04/02/2019–20/05/2019 | S1.winter 9 sampling stations | S2.winter 5 sampling stations | S3.winter 3 sampling stations |
Summer: 08/07/2019–09/07/2019 | S1.summer 9 sampling stations | S2.summer 5 sampling stations | S3.summer 3 sampling stations |
S1 | S2 | S3 | |||||||||
---|---|---|---|---|---|---|---|---|---|---|---|
PAH | LOD | LOQ | Mean | Median | Range | Mean | Median | Range | Mean | Median | Range |
Na | 0.016 | 0.05 | 0.10 | 0.05 | <LOQ–0.85 | 0.08 | 0.05 | <LOQ–0.54 | 0.24 | 0.05 | <LOQ–1.72 |
Acl | 0.006 | 0.02 | 0.31 | 0.18 | <LOQ–2.11 | 0.20 | 0.09 | <LOQ–1.42 | 0.19 | 0.18 | <LOQ–0.48 |
Ac | 0.006 | 0.02 | 0.07 | 0.02 | <LOQ–0.51 | 0.06 | 0.04 | <LOQ–0.28 | 0.11 | 0.11 | <LOQ–0.29 |
Fl | 0.006 | 0.02 | 0.82 | 0.63 | 0.08–2.99 | 0.36 | 0.37 | 0.08–0.81 | 0.56 | 0.58 | 0.13–0.98 |
Phe | 0.006 | 0.02 | 1.78 | 0.74 | 0.28–7.62 | 0.62 | 0.45 | 0.28–2.13 | 0.95 | 0.53 | 0.35–2.43 |
An | 0.006 | 0.02 | 0.07 | 0.06 | <LOQ–0.29 | 0.04 | 0.04 | <LOQ–0.07 | 0.09 | 0.06 | <LOQ–0.46 |
Fa | 0.006 | 0.02 | 0.91 | 0.20 | 0.06–3.75 | 0.31 | 0.16 | 0.06–1.39 | 0.94 | 0.11 | 0.04–5.07 |
Py | 0.006 | 0.02 | 0.27 | 0.09 | 0.02–1.24 | 0.82 | 0.10 | 0.02–9.29 | 0.41 | 0.13 | 0.02–2.56 |
BcFl | 0.006 | 0.02 | 0.07 | 0.02 | <LOQ–0.45 | 0.04 | 0.02 | <LOQ–0.16 | 0.10 | 0.04 | <LOQ–0.47 |
BaA | 0.006 | 0.02 | 0.05 | 0.02 | <LOQ–0.24 | 0.04 | 0.02 | <LOQ–0.23 | 0.06 | 0.03 | <LOQ–0.24 |
Chr | 0.006 | 0.02 | 0.24 | 0.09 | <LOQ–1.44 | 0.29 | 0.07 | <LOQ–1.57 | 0.42 | 0.07 | <LOQ–2.01 |
Cpp | 0.006 | 0.02 | 0.04 | 0.02 | <LOQ–0.14 | 0.10 | 0.03 | <LOQ–0.48 | 0.05 | 0.02 | <LOQ–0.27 |
5MeChr | 0.006 | 0.02 | 0.09 | 0.08 | <LOQ–0.54 | 0.10 | 0.06 | <LOQ–0.46 | 0.13 | 0.06 | <LOQ–0.76 |
BbFa | 0.006 | 0.02 | 0.07 | 0.05 | <LOQ–0.29 | 0.10 | 0.05 | <LOQ–0.45 | 0.21 | 0.05 | <LOQ–1.41 |
BkFa | 0.006 | 0.02 | 0.06 | 0.02 | <LOQ–0.36 | 0.06 | 0.02 | <LOQ–0.24 | 0.25 | 0.03 | <LOQ–1.88 |
BjFa | 0.006 | 0.02 | 0.06 | 0.03 | <LOQ–0.32 | 0.06 | 0.03 | <LOQ–0.23 | 0.24 | 0.03 | <LOQ–1.69 |
BaP | 0.006 | 0.02 | 0.09 | 0.02 | <LOQ–0.47 | 0.09 | 0.02 | <LOQ–0.34 | 0.29 | 0.02 | <LOQ–2.11 |
BeP | 0.006 | 0.02 | 0.10 | 0.06 | <LOQ–0.40 | 0.14 | 0.06 | <LOQ–0.66 | 0.27 | 0.04 | <LOQ–1.87 |
Per | 0.006 | 0.02 | 0.22 | 0.09 | <LOQ–1.20 | 0.22 | 0.14 | <LOQ–0.94 | 0.14 | 0.05 | <LOQ–0.71 |
IP | 0.006 | 0.02 | 0.03 | 0.02 | <LOQ–0.10 | 0.04 | 0.02 | <LOQ–0.12 | 0.06 | 0.02 | <LOQ–0.25 |
DBahA | 0.016 | 0.05 | 0.05 | 0.05 | <LOQ | 0.05 | 0.05 | <LOQ | 0.05 | 0.05 | <LOQ |
BghiP | 0.016 | 0.05 | 0.05 | 0.05 | <LOQ | 0.05 | 0.05 | <LOQ | 0.05 | 0.05 | <LOQ |
DBalP | 0.033 | 0.10 | 0.10 | 0.10 | <LOQ | 0.10 | 0.10 | <LOQ | 0.10 | 0.10 | <LOQ |
DBaeP | 0.033 | 0.10 | 0.10 | 0.10 | <LOQ | 0.10 | 0.10 | <LOQ | 0.10 | 0.10 | <LOQ |
DBaiP | 0.033 | 0.10 | 0.10 | 0.10 | <LOQ | 0.10 | 0.10 | <LOQ | 0.10 | 0.10 | <LOQ |
DBahP | 0.033 | 0.10 | 0.10 | 0.10 | <LOQ | 0.08 | 0.10 | <LOQ | 0.24 | 0.10 | <LOQ |
Σ26PAHs | 5.96 | 3.59 | 1.92–16.03 | 4.27 | 5.28 | 1.37–12.33 | 6.21 | 2.82 | 2.03–25.59 | ||
Σ16PAHs (EPA) | 4.98 | 2.96 | 1.07–15.36 | 3.21 | 1.96 | 0.76–11.18 | 4.88 | 2.67 | 1.25–19.42 | ||
Σ15+1PAHs (EU) | 1.29 | 0.94 | 0.70–3.75 | 1.42 | 0.87 | 0.72–4.16 | 2.32 | 0.97 | 0.71–11.47 | ||
Σ4PAHs | 0.45 | 0.21 | 0.08–2.42 | 0.53 | 0.16 | 0.09–2.35 | 0.98 | 0.16 | 0.09–5.77 |
Spring | Winter | Summer | ||||||||
---|---|---|---|---|---|---|---|---|---|---|
Mean | Total Seasonal Mean | Total Range | Mean | Total Seasonal Mean | Total Range | Mean | Total Seasonal Mean | Total Range | ||
BaP | S1 | 0.03 | 0.02 | <LOQ–0.06 | 0.18 | 0.28 | <LOQ–2.11 | 0.07 | 0.08 | <LOQ–0.34 |
S2 | 0.02 | 0.15 | 0.12 | |||||||
S3 | 0.02 | 0.83 | 0.02 | |||||||
Σ26PAHs | S1 | 2.70 | 2.45 | 1.37–4.50 | 11.60 | 10.12 | 2.28–25.59 | 3.59 | 3.95 | 1.97–12.33 |
S2 | 1.81 | 5.71 | 5.28 | |||||||
S3 | 2.77 | 13.05 | 2.82 | |||||||
Σ16PAHs (EPA) | S1 | 1.83 | 1.66 | 0.76–3.40 | 10.51 | 8.70 | 0.13–19.42 | 2.61 | 2.97 | 1.28–11.18 |
S2 | 1.12 | 4.44 | 4.09 | |||||||
S3 | 2.06 | 10.36 | 2.21 | |||||||
Σ15+1PAHs (EU) | S1 | 0.96 | 0.89 | 0.72–2.04 | 2.01 | 2.67 | 0.83–11.47 | 0.90 | 0.97 | 0.70–2.17 |
S2 | 0.78 | 2.29 | 1.18 | |||||||
S3 | 0.89 | 5.24 | 0.84 | |||||||
Σ4PAHs | S1 | 0.16 | 0.15 | 0.08–0.26 | 0.99 | 1.34 | 0.13–5.77 | 0.20 | 0.21 | 0.08–0.74 |
S2 | 0.14 | 1.16 | 0.28 | |||||||
S3 | 0.16 | 2.66 | 0.13 |
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Grigoriou, C.; Costopoulou, D.; Vassiliadou, I.; Chrysafidis, D.; Tzamtzis, V.; Bakeas, E.; Leondiadis, L. Monitoring of Polycyclic Aromatic Hydrocarbon Levels in Mussels (Mytilus galloprovincialis) from Aquaculture Farms in Central Macedonia Region, Greece, Using Gas Chromatography–Tandem Mass Spectrometry Method. Molecules 2021, 26, 5953. https://doi.org/10.3390/molecules26195953
Grigoriou C, Costopoulou D, Vassiliadou I, Chrysafidis D, Tzamtzis V, Bakeas E, Leondiadis L. Monitoring of Polycyclic Aromatic Hydrocarbon Levels in Mussels (Mytilus galloprovincialis) from Aquaculture Farms in Central Macedonia Region, Greece, Using Gas Chromatography–Tandem Mass Spectrometry Method. Molecules. 2021; 26(19):5953. https://doi.org/10.3390/molecules26195953
Chicago/Turabian StyleGrigoriou, Constantina, Danae Costopoulou, Irene Vassiliadou, Dimitrios Chrysafidis, Vassilios Tzamtzis, Evangelos Bakeas, and Leondios Leondiadis. 2021. "Monitoring of Polycyclic Aromatic Hydrocarbon Levels in Mussels (Mytilus galloprovincialis) from Aquaculture Farms in Central Macedonia Region, Greece, Using Gas Chromatography–Tandem Mass Spectrometry Method" Molecules 26, no. 19: 5953. https://doi.org/10.3390/molecules26195953