Analysis of Cyclic Imines in Mussels (Mytilus galloprovincialis) from Galicia (NW Spain) by LC-MS/MS
Abstract
:1. Introduction
2. Materials and Methods
2.1. Reagents and Standards
2.2. Sampling
2.3. Extraction
2.4. Hydrolysis
2.5. Solid Phase Extraction (SPE) Step for the Concentration of CIs and Clean-Up of Sample Extracts
2.6. LC-MS/MS Analysis
3. Results and Discussion
3.1. Adjustment of LC-MS/MS to the Analysis of CIs
3.2. Quality Control in LC-MS/MS Analysis
3.3. Quantification of SPX-1 and PnTX-G in Samples
3.4. LC-MS/MS Screening of CIs after the Concentration of Sample Extracts Using an SPE Step
4. Conclusions
Supplementary Materials
Author Contributions
Funding
Acknowledgments
Conflicts of Interest
References
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Analyte | Precursor Ion, m/z | Product Ion, m/z | Fragmentor, V | Collision Energy, V | Cell Accelerator | Retention Time, min |
---|---|---|---|---|---|---|
GYM-A | 508.3 | 392.3 | 220 | 40 | 3 | 2.60 |
GYM-A | 508.3 | 136.1 | 220 | 42 | 3 | 2.60 |
desmethylSPX-1 | 678.5 | 430.3 | 240 | 40 | 2 | 3.11 |
desmethylSPX-1 | 678.5 | 164.1 | 240 | 54 | 2 | 3.11 |
SPX-1 | 692.5 | 444.3 | 240 | 40 | 2 | 3.68 |
SPX-1 | 692.5 | 164.1 | 240 | 54 | 2 | 3.68 |
PnTX-A | 712.4 | 458.3 | 240 | 50 | 2 | 2.87 |
PnTX-A | 712.4 | 164.1 | 240 | 60 | 2 | 2.87 |
PnTX-G | 694.5 | 458.3 | 240 | 50 | 2 | 4.55 |
PnTX-G | 694.5 | 164.1 | 240 | 60 | 2 | 4.55 |
Methanol | MMS | ||||
---|---|---|---|---|---|
Analyte | Slope | RSD, % * | Slope | RSD, % * | Signal Suppression, % |
PnTX-G | 135,853 | 2.2 | 98,659 | 2.9 | 27.4 |
SPX-1 | 226,904 | 0.8 | 225,225 | 2.6 | 0.7 |
GYM-A | 40,854 | 1.4 | 36,309 | 2.6 | 11.1 |
Sampling Zone | Sample Code | SPX-1 (µg/kg) | PnTX-G (µg/kg) | |
---|---|---|---|---|
Before Hydrolysis | After Hydrolysis | |||
Ría de Sada A (1) | RS1.1 | 2.7 | 1.8 | 2.2 |
RS1.2 | 1.9 | 1.8 | 2.2 | |
RS1.3 | 3.1 | 1.8 | 2.2 | |
RS1.4 | 2.2 | 1.8 | 2.2 | |
RS1.5 | 3.3 | 1.8 | 2.2 | |
RS1.6 | 3.5 | 1.8 | 2.2 | |
RS1.7 | 4.0 | 1.8 | 2.2 | |
RS1.8 | 1.8 | 1.8 | 2.2 | |
RS1.9 | 6.9 | 1.8 | 2.2 | |
RS1.10 | 4.2 | 1.8 | 2.2 | |
RS1.11 | 4.2 | 1.8 | 2.2 | |
RS1.12 | 3.5 | 1.8 | 2.2 | |
Ría de Arousa (2) | RA2.1 | <LoQ | 2.9 | 3.2 |
RA2.2 | <LoQ | 3.1 | 3.2 | |
Ría de Arousa (3) | RA3.1 | 1.2 | 2.3 | 2.7 |
RA3.2 | 1.6 | 2.8 | 3.1 | |
RA3.3 | <LoQ | 2.3 | 2.7 | |
RA3.4 | 2.2 | 2.9 | 3.2 |
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Moreiras, G.; Leão, J.M.; Gago-Martínez, A. Analysis of Cyclic Imines in Mussels (Mytilus galloprovincialis) from Galicia (NW Spain) by LC-MS/MS. Int. J. Environ. Res. Public Health 2020, 17, 281. https://0-doi-org.brum.beds.ac.uk/10.3390/ijerph17010281
Moreiras G, Leão JM, Gago-Martínez A. Analysis of Cyclic Imines in Mussels (Mytilus galloprovincialis) from Galicia (NW Spain) by LC-MS/MS. International Journal of Environmental Research and Public Health. 2020; 17(1):281. https://0-doi-org.brum.beds.ac.uk/10.3390/ijerph17010281
Chicago/Turabian StyleMoreiras, Guillermo, José Manuel Leão, and Ana Gago-Martínez. 2020. "Analysis of Cyclic Imines in Mussels (Mytilus galloprovincialis) from Galicia (NW Spain) by LC-MS/MS" International Journal of Environmental Research and Public Health 17, no. 1: 281. https://0-doi-org.brum.beds.ac.uk/10.3390/ijerph17010281