An Inductively Coupled Plasma Optical Emission Spectrometric Method for the Determination of Toxic and Nutrient Metals in Spices after Pressure-Assisted Digestion
Abstract
:1. Introduction
2. Materials and Methods
2.1. Chemicals and Reagents
2.2. Instrumentation
2.3. Sample Collection
2.4. Sample Preparation
3. Results and Discussion
3.1. Selection of the Monitored Emission LInes
3.2. Figures of Merit
3.3. Real Samples Analysis and Discussion
4. Conclusions
Author Contributions
Funding
Institutional Review Board Statement
Informed Consent Statement
Data Availability Statement
Conflicts of Interest
References
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Element | Emission Line (nm) | Calibration Curve | R2 | LOD (mg kg−1) | LOQ (mg kg−1) | Upper Limit of Calibration Curve (mg kg−1) |
---|---|---|---|---|---|---|
Ag | 328.068 | y = 202.7x − 401.36 | 0.9999 | 0.18 | 0.61 | 1000 |
Al | 308.215 | y = 46.26x − 89.904 | 0.9999 | 2.34 | 7.81 | 1000 |
B | 249.772 | y = 31.24x − 192.07 | 0.9999 | 2.95 | 9.85 | 1000 |
Ba | 230.425 | y = 11.80x + 8.3761 | 0.9999 | 0.63 | 2.09 | 1000 |
Bi | 223.061 | y = 1.40x − 15.393 | 0.9999 | 3.41 | 11.38 | 1000 |
Ca | 317.933 | y = 34.88x + 678.32 | 0.9989 | 4.51 | 15.02 | 1000 |
Cd | 226.502 | y = 6.61x + 11.911 | 0.9999 | 1.57 | 5.24 | 1000 |
Co | 238.892 | y = 10.84x − 32.128 | 0.9999 | 0.67 | 2.22 | 1000 |
Cr | 357.869 | y = 380.5x − 2575.6 | 0.9999 | 0.43 | 1.45 | 1000 |
Cu | 324.752 | y = 600.0x − 1284.5 | 0.9999 | 0.15 | 0.52 | 1000 |
Fe | 238.204 | y = 18.81x + 46.632 | 0.9999 | 2.92 | 9.75 | 1000 |
Mg | 280.271 | y = 516.3x + 3009.4 | 0.9999 | 0.08 | 0.27 | 1000 |
Mn | 257.610 | y = 233.7x + 1176 | 0.9999 | 0.09 | 0.29 | 1000 |
Ni | 232.003 | y=2.76x − 13.599 | 0.9999 | 0.85 | 2.85 | 1000 |
Pb | 217.000 | y = 0.43x − 4.0975 | 0.9999 | 5.95 | 19.83 | 1000 |
Tl | 276.787 | y = 2.08x − 20.183 | 0.9998 | 4.98 | 16.60 | 1000 |
Zn | 213.857 | y = 6.86x + 23.944 | 0.9999 | 1.55 | 5.18 | 1000 |
Element | Clove_1 | Chilli_1 | |||||
---|---|---|---|---|---|---|---|
Added (mg kg−1) | Found (mg kg−1) | RR% | RSD% | Found (mg kg−1) | RR% | RSD% | |
Ag | 0 | <LOD | - | - | <LOD | - | - |
100 | 100.6 ± 0.3 | 100.6 | 0.3 | 104.8 ± 1.47 | 104.8 | 1.4 | |
250 | 250.6 ± 1.1 | 100.2 | 0.4 | 249.5 ± 4.62 | 99.8 | 1.9 | |
500 | 454.6 ± 7.9 | 90.9 | 1.7 | 490.2 ± 1.96 | 98.0 | 0.4 | |
Al | 0 | 312.2 ± 3.4 | - | 1.1 | 166.6 ± 2.4 | - | 1.4 |
100 | 405.1 ± 9.4 | 92.9 | 2.3 | 258.9 ± 12.1 | 92.3 | 4.7 | |
250 | 517.2 ± 2.7 | 82.0 | 0.5 | 448.5 ± 28.8 | 112.8 | 6.5 | |
500 | 784.7 ± 2.7 | 94.5 | 0.3 | 665.1 ± 6.1 | 99.7 | 0.9 | |
B | 0 | 39.4 ± 2.5 | - | 6.2 | 11.0 ± 0.9 | - | 8.2 |
100 | 131.9 ± 1.5 | 92.5 | 1.1 | 114.7 ± 0.9 | 103.7 | 0.8 | |
250 | 255.2 ± 0.8 | 86.3 | 0.3 | 232.7 ± 6.1 | 88.7 | 2.6 | |
500 | 542.6 ± 0.3 | 100.6 | 0.1 | 515.0 ± 2.9 | 100.8 | 0.6 | |
Ba | 0 | 34.1 ± 1.9 | - | 5.8 | 23.9 ±1.3 | - | 5.4 |
100 | 126.8 ± 0.3 | 92.7 | 0.2 | 135.8 ± 1.3 | 111.9 | 1.0 | |
250 | 255.1 ± 3.9 | 88.4 | 1.5 | 287.9 ± 25.7 | 105.6 | 8.9 | |
500 | 515.9 ± 2.0 | 96.4 | 0.4 | 525.3 ± 0.7 | 100.3 | 0.1 | |
Bi | 0 | <LOD | - | - | <LOD | - | - |
100 | 88.4 ± 5.1 | 88.4 | 5.8 | 104.5 ± 8.53 | 104.5 | 8.2 | |
250 | 224.8 ± 3.7 | 89.9 | 1.7 | 233.0 ± 21.4 | 93.2 | 9.2 | |
500 | 535.5 ± 6.6 | 107.1 | 1.2 | 533.5 ± 8.70 | 106.7 | 1.6 | |
Ca | 0 | 2245 ± 20.7 | - | 0.9 | 2449 ± 45.9 | - | 1.9 |
250 | 2498.3 ± 74.9 | 101.3 | 3.0 | 2710.5 ± 17.4 | 104.6 | 0.6 | |
500 | 2784.0 ± 12.5 | 107.8 | 0.5 | 2930.5 ± 31.7 | 96.3 | 1.1 | |
Cd | 0 | <LOD | - | - | <LOD | - | - |
100 | 98.7 ± 0.5 | 98.7 | 0.5 | 103.0 ± 0.7 | 103.0 | 0.7 | |
250 | 250.7 ± 1.6 | 100.3 | 0.6 | 253.0 ± 22.3 | 101.2 | 8.8 | |
500 | 491.5 ± 0.6 | 98.3 | 0.1 | 497.0 ± 2.0 | 99.4 | 0.4 | |
Co | 0 | <LOD | - | - | <LOD | - | - |
100 | 106.8 ± 0.7 | 106.8 | 0.7 | 107.5 ± 0.3 | 107.5 | 0.3 | |
250 | 263.7 ± 4.2 | 105.5 | 1.6 | 267.3 ± 11.6 | 106.9 | 4.3 | |
500 | 515.8 ± 1.7 | 103.2 | 0.3 | 514.7 ± 0.3 | 102.9 | 0.1 | |
Cr | 0 | <LOD | - | - | <LOD | - | - |
100 | 114.9 ± 1.1 | 114.9 | 1.0 | 117.5 ± 4.5 | 117.5 | 3.8 | |
250 | 244.8 ± 1.0 | 97.9 | 0.4 | 273.4 ± 7.9 | 109.4 | 2.9 | |
500 | 555.7 ± 10.0 | 111.1 | 1.8 | 537.4 ± 11.5 | 107.5 | 2.1 | |
Cu | 0 | 1.30 ±0.01 | - | 0.8 | 4.71 ±0.21 | - | 4.3 |
100 | 92.3 ± 0.8 | 91.0 | 0.9 | 97.5 ± 3.1 | 92.8 | 3.1 | |
250 | 236.1 ± 0.4 | 93.9 | 0.2 | 235.4 ± 15.8 | 92.3 | 6.7 | |
500 | 528.1 ± 8.7 | 105.4 | 1.7 | 520.0 ± 9.4 | 103.1 | 1.8 | |
Fe | 0 | 183.8 ± 3.2 | - | 1.7 | 137.4 ± 4.9 | - | 3.6 |
100 | 277.8 ± 1.6 | 94.0 | 0.6 | 232.6 ± 4.3 | 95.2 | 1.9 | |
250 | 402.8 ± 2.9 | 87.6 | 0.7 | 342.7 ± 15.1 | 82.1 | 4.4 | |
500 | 646.2 ± 2.5 | 92.5 | 0.4 | 623.5 ± 1.1 | 97.2 | 0.2 | |
Mg | 0 | 1230.0 ± 12.8 | - | 1.0 | 1542.0 ± 21.4 | - | 1.4 |
250 | 1456.0 ± 7.3 | 90.4 | 0.5 | 1770.5 ± 1.8 | 91.4 | 0.1 | |
500 | 1736.5 ± 1.4 | 101.3 | 0.1 | 2060.0 ± 3.7 | 103.6 | 0.2 | |
Mn | 0 | 159.2 ± 1.4 | - | 0.9 | 75.7 ± 4.9 | - | 6.5 |
100 | 241.2 ± 0.5 | 82.0 | 0.2 | 169.1± 2.4 | 93.4 | 1.4 | |
250 | 408.7 ± 2.0 | 99.8 | 0.5 | 308.1 ± 6.2 | 93.0 | 2.0 | |
500 | 590.9 ± 1.5 | 86.3 | 0.3 | 573.6 ± 1.7 | 99.6 | 0.3 | |
Ni | 0 | <LOD | - | - | <LOD | - | 8.0 |
100 | 82.2 ± 0.35 | 82.2 | 0.4 | 82.6 ± 1.2 | 82.6 | 1.5 | |
250 | 223.2 ± 3.3 | 89.3 | 1.5 | 242.8 ± 3.7 | 97.1 | 1.5 | |
500 | 522.2 ± 0.52 | 104.4 | 0.1 | 518.2 ± 0.4 | 103.6 | 0.1 | |
Pb | 0 | <LOD | - | - | <LOD | - | - |
100 | 97.2 ± 2.3 | 97.2 | 2.4 | 87.5 ± 7.7 | 87.5 | 8.8 | |
250 | 266.8 ± 5.2 | 106.7 | 2.0 | 285.3 ± 27.1 | 114.1 | 9.5 | |
500 | 562.1 ± 0.9 | 112.4 | 0.2 | 563.9 ± 3.9 | 112.8 | 0.7 | |
Tl | 0 | <LOD | - | - | <LOD | - | - |
100 | 87.6 ± 1.6 | 87.6 | 1.8 | 98.8 ± 0.5 | 98.8 | 0.5 | |
250 | 228.8 ± 5.5 | 91.5 | 2.4 | 270.2 ± 4.2 | 108.1 | 1.6 | |
500 | 550.9 ± 11.2 | 110.2 | 2.0 | 556.6 ± 10.2 | 111.3 | 1.8 | |
Zn | 0 | 46.0 ± 2.4 | - | 5.1 | 33.9 ± 1.3 | - | 3.8 |
100 | 136.5 ± 0.8 | 90.5 | 0.6 | 125.1 ± 0.2 | 91.2 | 0.2 | |
250 | 287.2 ± 4.8 | 96.5 | 1.7 | 286.9 ± 7.0 | 101.2 | 2.4 | |
500 | 538.8 ± 2.2 | 98.6 | 0.4 | 530.1 ± 1.5 | 99.2 | 0.3 |
Sample | Al | B | Ba | Ca | Cu | Cr | Fe | Mg | Mn | Ni | Zn |
---|---|---|---|---|---|---|---|---|---|---|---|
Asteroid anise (Illicium verum) | 142.9 | 40.0 | 51.3 | 931 | 7.98 | <LOD | 82.3 | 468 | 89.9 | <LOD | 61.4 |
Clove_1 (Syzygium aromaticum) | 312.2 | 39.4 | 34.1 | 2245 | 1.30 | <LOD | 183.8 | 1230 | 159.2 | <LOD | 46.0 |
Clove_2 (Syzygium aromaticum) | 156.9 | 39.9 | 52.4 | 1145 | <LOD 2 | <LOD | 87.6 | 498 | 88.8 | <LOD | 63.8 |
Cardamon (Elettaria cardamomum) | 136.1 | 11.4 | 26.1 | 4756 | 7.96 | 4.53 | 119.3 | 3847 | 387.8 | 8.02 | 51.9 |
Cinnamon (Cinnamomum verum) | 232.4 | <LOQ 1 | 100.7 | 7844 | 7.10 | 3.65 | 178.7 | 908 | 344.9 | <LOQ | 40.0 |
Curry (Commercial powder) | 256.0 | <LOQ | 4.38 | 3298 | 7.80 | 3.94 | 338.0 | 1793 | 73.0 | <LOQ | 13.8 |
Coriander (Coriandrum sativum) | 237.3 | 21.2 | 27.2 | 2816 | 10.6 | <LOD | 177.8 | 1666 | 103.3 | <LOD | 42.5 |
Turmeric_1 (Curcuma longa) | 291.3 | 28.6 | 34.5 | 2520 | 0.98 | <LOD | 213.4 | 1507 | 130.2 | <LOD | 44.2 |
Turmeric_1 (Curcuma longa) | 80.5 | 22.7 | 9.8 | 2335 | <LOD | 3.02 | 49.1 | 748 | 28.2 | <LOQ | 10.6 |
Cumin (Cuminum cyminum) | 438.8 | 34.6 | 17.2 | 10921 | 13.1 | 3.50 | 359.3 | 3065 | 28.6 | 8.94 | 37.1 |
White pepper (Piper nigrum) | 73.5 | <LOQ | 20.6 | 2369 | 15.9 | 1.80 | 93.2 | 842 | 123.7 | <LOQ | 5.3 |
Black pepper _1 (Piper nigrum) | 350.6 | 23.1 | 59.1 | 4481 | 15.4 | 3.34 | 357.4 | 1991 | 289.5 | 8.97 | 5.9 |
Black pepper_2 (Piper nigrum) | 67.2 | 22.1 | 12.3 | 2691 | <LOD | 2.60 | 50.1 | 749 | 29.7 | 6.25 | 10.9 |
Nutmeg (Myristica fragrans) | 68.2 | 10.2 | 14.8 | 1642 | 15.2 | 4.93 | 70.7 | 1709 | 43.9 | 14.7 | 20.5 |
Allspice (Pimenta dioica) | 34.1 | 23.4 | 11.3 | 9239 | 19.9 | 3.04 | 31.2 | 1256 | 6.51 | 5.82 | 17.8 |
Chilli_1 (Capsicum frutescens) | 166.6 | 11.0 | 23.9 | 2449 | 4.71 | <LOD | 137.4 | 1542 | 75.7 | <LOD | 33.9 |
Chilli_2 (Capsicum frutescens) | 88.4 | 12.9 | 8.31 | 2054 | <LOD | 2.60 | 51.6 | 770 | 29.3 | 3.63 | 11.9 |
Paprika_1 (Capsicum annuum) | 316.4 | 12.6 | 5.17 | 3976 | 14.8 | 3.97 | 450.3 | 2957 | 24.5 | 3.79 | 12.4 |
Paprika_2 (Capsicum annuum) | 82.3 | 11.7 | 11.2 | 2945 | <LOD | 3.36 | 56.1 | 880 | 33.1 | <LOQ | 13.2 |
Ginger (Zingiber officinale) | 566.0 | <LOQ | 19.8 | 2863 | 13.9 | 2.37 | 736.3 | 2369 | 501.0 | 7.84 | 26.7 |
Green pepper (Capsicum annuum) | 57.0 | <LOD | 10.9 | 2452 | <LOD | 2.83 | 46.4 | 671 | 25.7 | <LOQ | 11.2 |
Pink pepper (Schinus molle) | 248.8 | 23.9 | 31.7 | 2674 | 5.68 | <LOD | 202.7 | 1503 | 119.5 | <LOD | 40.1 |
Element | This work | [7] | [16] | [17] | [18] | [19] | [20] | [21] | [12] 1 |
---|---|---|---|---|---|---|---|---|---|
Ag | <LOD 2 | - | - | - | - | - | - | - | - |
Al | 34.1–566.0 | - | 40–700 | - | - | - | - | - | - |
B | <LOD–40.0 | - | - | 3.65–31.7 | - | - | - | - | - |
Ba | 4.38–100.7 | 2.02–39.22 | - | 0.63–77.34 | - | - | - | - | - |
Bi | <LOD | - | - | 0.46 × 10−3–14.96 × 10−3 | - | - | - | - | - |
Ca | 931–10,921 | 2510–9600 | 6560–13,700 | - | - | - | 2282–15,579 | 4300–24,500 | 11,032 |
Cd | <LOD | <LOD–8.0 × 10−3 | - | 3.56 × 10−3–94.3 × 10−3 | 13 × 10−3–315 × 10−3 | 0.10–0.93 | - | ≤0.0966 | 0.066 |
Co | <LOD | 0.006–0.522 | <LOD–4.12 | 50.99 × 10−3–432.7 × 10−3 | - | - | - | - | |
Cr | <LOD–4.93 | 0.44–1.79 | <LOD–3.99 | 0.38–3.33 | - | 0.67–7.15 | - | - | - |
Cu | <LOD–19.9 | 2.78–11.70 | 2.5–19.03 | 2.35–77.68 | - | 4.1–28.7 | - | ≤100 | 8.55 |
Fe | 31.2–736.3 | 53–409 | 70–950 | - | - | 88.9–376.3 | 46.12–1002 | ≤592 | 587 |
Mg | 468–3847 | 400–2590 | 1790–4250 | - | - | - | 492.2–3870 | 640–7160 | - |
Mn | 6.51–501.0 | 14.2–164.7 | 26.17–79.73 | 18.99–879.8 | - | 11.9–211.3 | - | ≤307 | - |
Ni | <LOD–14.7 | 0.32–6.50 | <LOD–7.71 | 0.94–3.19 | - | 0.65–8.69 | - | ≥0.165 | 0.486 |
Pb | <LOD | - | <LOD–5.80 | 121.3 × 10−3–451.1 × 10−3 | 3.9 × 10−3–972 × 10−3 | 0.47–1.89 | - | 0.0631–2.053 | 0.282 |
Tl | <LOD | - | - | 0.387 × 10−3–28.50 × 10−3 | - | - | - | - | - |
Zn | 5.3–63.8 | 16.5–45.7 | 6.35–77.5 | 12.64–84.95 | - | 7.84–47.6 | - | ≤100 |
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Manousi, N.; Isaakidou, E.; Zachariadis, G.A. An Inductively Coupled Plasma Optical Emission Spectrometric Method for the Determination of Toxic and Nutrient Metals in Spices after Pressure-Assisted Digestion. Appl. Sci. 2022, 12, 534. https://doi.org/10.3390/app12020534
Manousi N, Isaakidou E, Zachariadis GA. An Inductively Coupled Plasma Optical Emission Spectrometric Method for the Determination of Toxic and Nutrient Metals in Spices after Pressure-Assisted Digestion. Applied Sciences. 2022; 12(2):534. https://doi.org/10.3390/app12020534
Chicago/Turabian StyleManousi, Natalia, Eleni Isaakidou, and George A. Zachariadis. 2022. "An Inductively Coupled Plasma Optical Emission Spectrometric Method for the Determination of Toxic and Nutrient Metals in Spices after Pressure-Assisted Digestion" Applied Sciences 12, no. 2: 534. https://doi.org/10.3390/app12020534
APA StyleManousi, N., Isaakidou, E., & Zachariadis, G. A. (2022). An Inductively Coupled Plasma Optical Emission Spectrometric Method for the Determination of Toxic and Nutrient Metals in Spices after Pressure-Assisted Digestion. Applied Sciences, 12(2), 534. https://doi.org/10.3390/app12020534