New Method for Simultaneous Arsenic and Selenium Speciation Analysis in Seafood and Onion Samples
Abstract
:1. Introduction
2. Results and Discussion
2.1. Simultaneous Arsenic and Selenium Speciation Analysis
2.2. Speciation Analysis of Water-Soluble Arsenic and Selenium by HPLC–ICP–MS
3. Materials and Methods
3.1. Reagents and Standards
3.2. Analytical Instruments
3.3. Method Development for Simultaneous Speciation Analysis
Analytical Column and Mobile Phase Effect
- -
- PRP-X100 (250 mm × 4.1 mm, 10 μm), packing material type: PS-DVB/Trimethyl ammonium exchanger (Hamilton, Reno, NV, USA);
- -
- PRPX-200 PEEK (250 mm × 4.6 mm, 10 µm), packing material type: PSDVB/Sulfonic Acid (Hamilton, USA);
- -
- BioWAX (50 mm × 2.1 mm, 5 µm), packing material type: nonporous/dietyloamine (Agilent, Santa Clara, CA, USA);
- -
- Supelco SAX (250 mm × 4.6 mm, 5 µm), packing material type: silica gel, spherical particle platform/propyltrimethylammonium phase (Sigma–Aldrich, USA);
- -
- Waters SAX (250 mm × 4.6 mm, 5 µm), packing material type: silica-based quaternary ammonium bonded sorbent (Waters, Milford, MA, USA);
- -
- Dionex CS5A (250 mm × 4 mm, 9 µm), packing material type: latex, DVB/Cation: Sulfonic Acid/Anion: Quaternary Ammonium (Thermo, Waltham, MA, USA);
- -
- Dionex CG5A (50 mm × 4 mm, 9 µm), packing material type: latex, DVB/Cation: Sulfonic Acid/Anion: Quaternary Ammonium (Thermo, USA);
- -
- Dionex AS22 (250 mm × 4 mm, 6 µm), packing material type: DVB/Alkanol Quaternary Ammonium Ion (Thermo, USA);
- -
- Dionex AG22 (250 mm × 4 mm, 6 µm), packing material type: DVB/Alkanol Quaternary Ammonium Ion (Thermo, USA).
3.4. Oven Temperature Effect
3.5. Final Method
3.6. Samples and Sample Preparation
4. Conclusions
Author Contributions
Funding
Institutional Review Board Statement
Informed Consent Statement
Data Availability Statement
Conflicts of Interest
References
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Sample/Determined Form | As(III) | As(V) | MMA | DMA | As-Bet * | Water-Soluble as by ICP–MS | Column Recovery * |
---|---|---|---|---|---|---|---|
bio white onion | 166.1 ± 7.5 | <LOD | <LOD | <LOD | <LOD | 0.171 ± 0.002 | 97.7 ± 3.7 |
pink onion | 139.2 ± 5.6 | <LOD | <LOD | <LOD | <LOD | 0.153 ± 0.003 | 92.8 ± 4.7 |
sweet onion | 149.3 ± 5.9 | <LOD | <LOD | <LOD | <LOD | 0.164 ± 0.002 | 93.3 ± 4.8 |
bio red onion | 189.3 ± 7.9 | <LOD | <LOD | <LOD | <LOD | 0.206 ± 0.005 | 94.6 ± 4.7 |
red shrimp | <LOD | <LOD | <LOD | <LOD | 15.48 ± 0.62 | 16.50 ± 0.09 | 93.9 ± 3.9 |
clam | <LOD | <LOD | 336.9 ± 12.4 | <LOD | 13.32 ± 0.58 | 13.91 ± 0.17 | 98.2 ± 4.8 |
octopus | <LOD | <LOD | <LOD | <LOD | 2.419 ± 0.112 | 2.511 ± 0.032 | 96.4 ± 3.8 |
squid | <LOD | <LOD | <LOD | <LOD | 4.691 ± 0.221 | 5.011 ± 0.061 | 93.7 ± 4.4 |
red big shrimp | <LOD | <LOD | <LOD | 119.8 ± 5.5 | 20.69 ± 0.782 | 21.30 ± 0.51 | 97.7 ± 3.7 |
white blanched shrimp Vannamei | <LOD | <LOD | <LOD | <LOD | 2.507 ± 0.100 | 2.652 ± 0.032 | 94.6 ± 2.7 |
white shrimp Vannamei | <LOD | <LOD | <LOD | <LOD | 2.221 ± 0.931 | 2.304 ± 0.027 | 96.6 ± 4.8 |
sample/determined form | Se(IV) | Se(VI) | Se-Met | Se-cystine | water-soluble Se by ICP–MS | Column recovery * | |
bio white onion | <LOD | 9.101 ± 0.302 | 609.7 ± 12.1 | <LOD | 0.671 ± 0.009 | 92.36 ± 4.41 | |
pink onion | 959.2 ± 45.8 | <LOD | <LOD | <LOD | 0.994 ± 0.021 | 96.89 ± 4.75 | |
sweet onion | <LOD | <LOD | 8788 ± 431.5 | <LOD | 8.921 ± 0.107 | 98.74 ± 3.85 | |
bio red onion | <LOD | <LOD | 5065 ± 217.8 | <LOD | 5.302 ± 0.153 | 95.57 ± 4.31 | |
red shrimp | <LOD | 47.53 ± 1.91 | 417.1 ± 16.9 | 987.2 ± 37.4 | 1.611 ± 0.032 | 90.17 ± 5.23 | |
clam | <LOD | 182.6 ± 7.6 | <LOD | <LOD | 0.203 ± 0.003 | 91.32 ± 4.75 | |
octopus | <LOD | 19.21 ± 0.92 | 435.5 ± 17.4 | <LOD | 0.502 ± 0.009 | 91.01 ± 4.55 | |
squid | <LOD | 67.41 ± 2.73 | <LOD | 202.2 ± 8.1 | 0.287 ± 0.006 | 96.31 ± 4.29 | |
red big shrimp | <LOD | 137.6 ± 5.7 | <LOD | <LOD | 0.152 ± 0.003 | 91.74 ± 3.89 | |
white blanched shrimp Vannamei | 94.5 ± 4.6 | <LOD | 760.3 ± 32.3 | <LOD | 0.879 ± 0.017 | 97.15 ± 3.79 | |
white shrimp Vannamei | <LOD | <LOD | 776.9 ± 36.4 | <LOD | 0.854 ± 0.011 | 91.41 ± 4.29 |
Column | Mobile Phase | As-Bet | As (III) | DMA | MMA | As (V) | Cr (III) | Cr (VI) | Se-Cystine | Se-Met | Se (IV) | Se (VI) | Sb (III) | Sb (V) |
---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|
PRPX-100 | HNO3 + CH3OH | ✕ | ✕ | ✕ | ✕ | ✕ | ✕ | ✕ | ✕ | ✕ | ✕ | ✕ | ✕ | ✕ |
PRPX-200 | HNO3 + CH3OH | ✕ | ✕ | ✕ | ✕ | ✕ | ✕ | ✕ | ✕ | ✕ | ✕ | ✕ | ✕ | ✕ |
NH4NO3 + CH3OH | ✕ | ✓ | ✓ | ✕ | ✕ | ✕ | ✕ | ✕ | ✕ | ✕ | ✕ | ✕ | ✕ | |
NH4NO3 + CH3OH + EDTA | ✕ | ✕ | ✕ | ✕ | ✕ | ✕ | ✕ | ✕ | ✕ | ✕ | ✕ | ✕ | ✕ | |
BIOWAX | NH4NO3 + CH3OH | ✕ | ✕ | ✕ | ✕ | ✕ | ✕ | ✕ | ✕ | ✕ | ✕ | ✕ | ✕ | ✕ |
SUPELCO | NH4NO3 + CH3OH | ✕ | ✓ | ✓ | ✕ | ✕ | ✕ | ✕ | ✕ | ✕ | ✕ | ✕ | ✕ | ✕ |
WATERS | NH4NO3 + CH3OH | ✕ | ✓ | ✓ | ✕ | ✕ | ✕ | ✕ | ✕ | ✕ | ✕ | ✕ | ✕ | ✕ |
DIONEX CG5A | NH4NO3 + CH3OH | ✕ | ✕ | ✕ | ✕ | ✕ | ✕ | ✕ | ✕ | ✕ | ✓ | ✓ | ✕ | ✕ |
DIONEX CS5A | NH4NO3 + CH3OH | ✕ | ✕ | ✓ | ✓ | ✓ | ✕ | ✕ | ✕ | ✕ | ✕ | ✕ | ✕ | ✕ |
DIONEX AG22 + AS22 | NH4NO3 + CH3OH | ✕ | ✕ | ✓ | ✓ | ✓ | ✕ | ✕ | ✓ | ✓ | ✓ | ✓ | ✕ | ✕ |
DIONEX AS22 + CG5A | NH4NO3 + CH3OH alkaline pH | ✓ | ✓ | ✓ | ✓ | ✓ | ✕ | ✕ | ✓ | ✓ | ✓ | ✓ | ✕ | ✕ |
NH4NO3 + CH3OH acidic pH | ✕ | ✕ | ✕ | ✓ | ✓ | ✕ | ✕ | ✓ | ✓ | ✓ | ✓ | ✕ | ✕ | |
(NH4)2CO3 alkaline pH | ✕ | ✓ | ✓ | ✓ | ✓ | ✕ | ✕ | ✕ | ✕ | ✓ | ✓ | ✕ | ✕ | |
NH4NO3 + NH4HCO3 | ✕ | ✕ | ✓ | ✓ | ✓ | ✕ | ✕ | ✓ | ✓ | ✓ | ✓ | ✕ | ✕ | |
NH4HCO3alkaline pH | ✕ | ✓ | ✓ | ✓ | ✓ | ✕ | ✕ | ✓ | ✓ | ✓ | ✓ | ✕ | ✕ | |
(NH4)2CO3 + NH4HCO3 | ✕ | ✕ | ✓ | ✓ | ✓ | ✕ | ✕ | ✓ | ✓ | ✓ | ✓ | ✕ | ✕ |
As(III) | As(V) | MMA | DMA | AsB | Se(IV) | Se(VI) | SeMet | Secystine | |
---|---|---|---|---|---|---|---|---|---|
Conc. Range | Up to 100 µg·L−1 * | ||||||||
Slope | 9.004 | 21.08 | 8.863 | 0.495 | 7.749 | 3.407 | 6.405 | 4.087 | 4.086 |
R2 | 0.9999 | 0.9999 | 0.9999 | 0.9995 | 0.9993 | 0.9999 | 0.9999 | 0.9997 | 0.9993 |
Limit of detection | 1.257 | 1.027 | 0.229 | 1.133 | 1.659 | 0.359 | 1.116 | 1.987 | 2.307 |
Generator power [W] | 1200 |
Argon flow—plasma [L/min] | 8.0 |
Argon flow—nebulizer [L/min] | 1.1 |
Argon flow—auxiliary [L/min] | 0.7 |
Nebulizer | Concentric type “micro” |
Torch | Concentric type “mini” |
Spray chamber temperature [°C] | 5.0 |
Collision gas—He [mL/min] | 6.0 |
Voltage on octapole rods [V] | −21 |
Energy filter [V] | 7.0 |
Sampling deep [mm] | 5.0 |
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Karaś, K.; Zioła-Frankowska, A.; Frankowski, M. New Method for Simultaneous Arsenic and Selenium Speciation Analysis in Seafood and Onion Samples. Molecules 2021, 26, 6223. https://doi.org/10.3390/molecules26206223
Karaś K, Zioła-Frankowska A, Frankowski M. New Method for Simultaneous Arsenic and Selenium Speciation Analysis in Seafood and Onion Samples. Molecules. 2021; 26(20):6223. https://doi.org/10.3390/molecules26206223
Chicago/Turabian StyleKaraś, Katarzyna, Anetta Zioła-Frankowska, and Marcin Frankowski. 2021. "New Method for Simultaneous Arsenic and Selenium Speciation Analysis in Seafood and Onion Samples" Molecules 26, no. 20: 6223. https://doi.org/10.3390/molecules26206223