Determination of Toxic Pyrrolizidine Alkaloids in Traditional Chinese Herbal Medicines by UPLC-MS/MS and Accompanying Risk Assessment for Human Health
Abstract
:1. Introduction
2. Results
2.1. Pretreatment Method Development
2.1.1. Extraction Optimization
2.1.2. Purification Optimization
2.2. UPLC-MS/MS Method Development
2.3. Method Validation
2.3.1. Sensitivity, Linearity, Limits of Detection (LOD) and Limits of Quantification (LOQ)
2.3.2. Precision and Recovery
2.4. PA Concentrations in Chinese Herbal Medicines
2.5. Risk Assessment of Chinese Herbal Medicines Based on PAs Levels
2.5.1. Acute Exposure Scenario
2.5.2. Chronic Exposure Scenario
3. Discussion
4. Materials and Methods
4.1. Chemicals and Reagents
4.2. Collection and Preparation of Samples
4.3. PAs Extraction
4.4. LC-MS/MS Analysis
4.5. Estimated Daily Intake (EDI) of PAs Resulting from the Consumption of Herbal Medicines
4.6. Calculation of MOE
4.7. Actual Life Exposure of Chinese Herbal Medicines
5. Conclusions
Supplementary Materials
Author Contributions
Funding
Institutional Review Board Statement
Informed Consent Statement
Data Availability Statement
Conflicts of Interest
References
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PAs | P. frutescens | Average | R. rosea | Average | S. oblata | Average | C. sinensis | Average | ||||||||
---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|
Abbr. | 50 μg/kg | 100 μg/kg | 200 μg/kg | 50 μg/kg | 100 g/kg | 200 μg/kg | 50 μg/kg | 100 μg/kg | 200 μg/kg | 50 μg/kg | 100 μg/kg | 200 μg/kg | ||||
Ret | 52.96 | 50.23 | 44.33 | 49.17 | 34.05 | 31.48 | 28.58 | 31.37 | 33.80 | 32.45 | 28.92 | 31.73 | 28.29 | 25.93 | 22.58 | 25.60 |
Mc | 87.51 | 81.26 | 76.29 | 81.69 | 93.52 | 83.99 | 81.09 | 86.20 | 80.36 | 77.07 | 73.45 | 76.96 | 91.93 | 87.35 | 83.57 | 87.62 |
Er | 92.22 | 82.64 | 79.19 | 84.68 | 92.24 | 83.75 | 80.78 | 85.59 | 82.58 | 77.49 | 75.82 | 78.63 | 95.34 | 89.42 | 86.64 | 90.47 |
McNO | 93.11 | 87.48 | 84.56 | 88.39 | 99.22 | 92.92 | 93.90 | 95.35 | 91.41 | 88.53 | 85.60 | 88.51 | 95.78 | 92.95 | 90.91 | 93.21 |
ErNO | 93.30 | 88.68 | 81.93 | 87.97 | 99.11 | 94.69 | 91.74 | 95.18 | 92.86 | 88.15 | 84.76 | 88.59 | 97.35 | 93.44 | 91.38 | 94.06 |
Jb | 95.29 | 89.09 | 84.03 | 89.47 | 95.34 | 87.42 | 83.72 | 88.83 | 87.94 | 82.76 | 80.34 | 83.68 | 96.02 | 90.20 | 87.06 | 91.09 |
Eu | 116.50 | 109.30 | 102.67 | 109.49 | 106.92 | 98.97 | 98.63 | 101.51 | 123.26 | 114.61 | 111.40 | 116.42 | 115.77 | 108.56 | 104.45 | 109.59 |
Im | 104.19 | 96.34 | 91.69 | 97.41 | 100.51 | 91.80 | 87.10 | 93.14 | 101.71 | 95.22 | 94.75 | 97.23 | 101.15 | 94.47 | 93.20 | 96.27 |
Ly | 112.08 | 99.29 | 91.32 | 100.90 | 118.46 | 102.36 | 97.05 | 105.96 | 119.29 | 108.72 | 107.15 | 111.72 | 117.58 | 105.60 | 104.14 | 109.11 |
JbNO | 92.05 | 86.68 | 83.15 | 87.29 | 95.84 | 91.72 | 93.77 | 93.77 | 90.24 | 87.77 | 86.67 | 88.23 | 99.58 | 93.67 | 93.10 | 95.45 |
EuNO | 113.80 | 106.74 | 102.79 | 107.77 | 112.71 | 103.62 | 106.20 | 107.51 | 111.69 | 108.06 | 106.05 | 108.60 | 111.70 | 103.73 | 105.91 | 107.11 |
ImNO | 136.31 | 125.89 | 120.85 | 127.68 | 127.33 | 115.07 | 119.21 | 120.54 | 133.24 | 122.01 | 123.50 | 126.25 | 129.96 | 116.92 | 120.13 | 122.34 |
LyNO | 114.13 | 106.84 | 103.62 | 108.20 | 111.30 | 105.04 | 108.91 | 108.41 | 112.67 | 106.88 | 106.47 | 108.67 | 114.17 | 106.61 | 107.32 | 109.37 |
Re | 88.24 | 85.83 | 81.80 | 85.29 | 98.16 | 92.80 | 87.90 | 92.95 | 96.13 | 94.37 | 91.86 | 94.12 | 99.43 | 96.15 | 93.41 | 96.33 |
ReNO | 97.58 | 92.65 | 88.85 | 93.03 | 101.48 | 96.09 | 98.72 | 98.76 | 101.12 | 93.88 | 94.61 | 96.53 | 103.04 | 97.81 | 97.75 | 99.53 |
Td | 98.47 | 93.47 | 87.79 | 93.25 | 99.88 | 92.35 | 92.91 | 95.05 | 96.87 | 93.51 | 92.58 | 94.32 | 98.56 | 94.97 | 94.82 | 96.12 |
Sp | 100.76 | 94.30 | 88.73 | 94.60 | 101.32 | 91.52 | 87.85 | 93.57 | 102.39 | 93.53 | 94.67 | 96.86 | 103.53 | 95.24 | 93.72 | 97.50 |
7-Im | 108.18 | 101.53 | 94.91 | 101.54 | 107.08 | 98.40 | 96.02 | 100.50 | 107.56 | 104.56 | 100.25 | 104.12 | 103.72 | 100.51 | 96.29 | 100.17 |
He | 109.93 | 102.09 | 97.39 | 103.14 | 107.59 | 98.34 | 96.99 | 100.97 | 108.75 | 103.93 | 100.47 | 104.39 | 106.52 | 101.40 | 98.85 | 102.26 |
7-Ly | 111.21 | 100.62 | 96.59 | 102.81 | 107.41 | 96.70 | 96.79 | 100.30 | 111.66 | 101.03 | 98.92 | 103.87 | 107.92 | 99.05 | 97.60 | 101.52 |
SpNO | 99.31 | 95.89 | 91.65 | 95.62 | 100.17 | 94.36 | 98.88 | 97.80 | 100.08 | 95.67 | 95.34 | 97.03 | 102.86 | 97.71 | 99.56 | 100.04 |
7ImNO | 80.81 | 77.37 | 75.52 | 77.90 | 89.81 | 86.90 | 88.52 | 88.41 | 83.31 | 81.43 | 79.87 | 81.54 | 88.80 | 87.43 | 85.12 | 87.12 |
HeNO | 105.60 | 97.82 | 95.78 | 99.74 | 106.34 | 96.47 | 102.04 | 101.62 | 104.15 | 99.02 | 99.01 | 100.73 | 104.00 | 98.86 | 98.52 | 100.46 |
Sv | 100.08 | 93.29 | 87.62 | 93.66 | 99.35 | 89.16 | 85.48 | 91.33 | 99.25 | 93.91 | 92.12 | 95.09 | 99.89 | 91.94 | 91.49 | 94.44 |
Sn | 101.29 | 96.03 | 90.98 | 96.10 | 101.42 | 92.35 | 87.74 | 93.84 | 100.07 | 94.97 | 93.77 | 96.27 | 100.19 | 95.83 | 95.42 | 97.15 |
SvNO | 104.14 | 97.65 | 94.73 | 98.84 | 105.24 | 99.60 | 102.36 | 102.40 | 104.85 | 99.38 | 96.48 | 100.24 | 107.33 | 99.20 | 99.17 | 101.90 |
SnNO | 103.66 | 96.53 | 94.35 | 98.18 | 105.18 | 99.56 | 101.74 | 102.16 | 103.00 | 95.50 | 95.41 | 97.97 | 101.84 | 99.27 | 99.26 | 100.12 |
Em | 107.55 | 101.47 | 99.18 | 102.73 | 105.32 | 99.30 | 98.47 | 101.03 | 106.05 | 102.22 | 100.38 | 102.88 | 105.90 | 100.02 | 98.84 | 101.59 |
EmNO | 108.87 | 107.19 | 113.70 | 109.92 | 111.86 | 113.25 | 129.58 | 118.23 | 112.14 | 111.47 | 116.28 | 113.29 | 113.34 | 113.89 | 125.30 | 117.51 |
Sk | 105.56 | 100.38 | 95.60 | 100.51 | 105.89 | 100.33 | 104.05 | 103.42 | 105.62 | 101.63 | 99.82 | 102.36 | 106.31 | 101.57 | 101.08 | 102.99 |
Lc | 92.85 | 88.45 | 90.21 | 90.50 | 94.69 | 89.25 | 93.62 | 92.52 | 89.74 | 87.28 | 91.01 | 89.34 | 97.76 | 93.19 | 95.74 | 95.56 |
LcNO | 90.74 | 85.54 | 81.06 | 85.78 | 94.34 | 88.08 | 90.09 | 90.84 | 85.59 | 81.88 | 81.63 | 83.03 | 96.76 | 90.92 | 92.21 | 93.30 |
Ret | 52.96 | 50.23 | 44.33 | 49.17 | 34.05 | 31.48 | 28.58 | 31.37 | 33.80 | 32.45 | 28.92 | 31.73 | 28.29 | 25.93 | 22.58 | 25.60 |
Mc | 87.51 | 81.26 | 76.29 | 81.69 | 93.52 | 83.99 | 81.09 | 86.20 | 80.36 | 77.07 | 73.45 | 76.96 | 91.93 | 87.35 | 83.57 | 87.62 |
Sample ID | Herbal Samples | Numbers of PAs Detected and Top Three | Total PAs Content (μg/kg) | Recommended Maximum Daily Use (g) | PAs Maximum Daily Consumption (g) | EDI (μg/kg bw/ Day) | MOE Values (Life Long Time) | MOE Values (Shorter Exposure) |
---|---|---|---|---|---|---|---|---|
HM-1 | Arnebia euchroma | 7 (LyNO, ImNO, EmNO) | 25567.4 | 10 | 255.6 | 3.652 | 64.8 | 1687.0 |
HM-2 | Tussilago farfara | 10 (Sk, SnNO, Sn) | 17600.2 | 10 | 176.0 | 2.514 | 94.2 | 2450.7 |
HM-3 | Eupatorium fortunei | 5 (Im, Ly, LyNO) | 16943.6 | 10 | 169.4 | 2.420 | 97.9 | 2545.7 |
HM-4 | Eupatorium lindleyanum | 5 (LyNO, Im, Ly) | 1863.6 | 60 | 111.8 | 1.597 | 148.3 | 3857.4 |
HM-5 | Senecio scandens | 12 (Sk, SnNO, SpNO) | 229.0 | 30 | 6.8 | 0.098 | 2414.5 | 62,777.8 |
HM-6 | Laggera pterodonta | 9 (Im, ImNO, JbNO) | 198.5 | 15 | 2.9 | 0.042 | 5569.5 | 144,808.1 |
HM-7 | Artemisia scoparia | 6 (Im, Ly, LyNO) | 233.6 | 10 | 3.5 | 0.033 | 7100.9 | 184,625.2 |
HM-8 | Cassia angustifolia | 9 (Mc, McNO, Td) | 220.6 | 6 | 1.3 | 0.018 | 12,528.8 | 325,751.0 |
HM-9 | Euphorbia hirta | 6 (Im, ImNO, LyNO) | 121.9 | 9 | 1.0 | 0.015 | 15,121.6 | 393,163.7 |
HM-10 | Gynura japonica | 6 (SnNO, SpNO, Sk) | 531.0 | 6 | 3.1 | 0.045 | 5206.7 | 135,375.7 |
HM-11 | Scutellaria barbata | 5 (LyNO, Ly, ImNO) | 61.7 | 30 | 1.8 | 0.026 | 8958.3 | 232,917.5 |
HM-12 | Euphorbia humifusa | 6 (LyNO, Ly, ImNO) | 45.0 | 20 | 0.9 | 0.012 | 18,421.0 | 478,947.3 |
HM-13 | Picria fel-terrae | 6 (LyNO, Ly, Im) | 58.2 | 15 | 0.8 | 0.012 | 18,983.8 | 493,580.5 |
HM-14 | Cirsium japonicum | 7 (Im, Sk, LyNO) | 44.6 | 15 | 0.6 | 0.009 | 24,798.2 | 644,753.3 |
HM-15 | Abrus cantoniensis | 6 (LyNO, Ly, ImNO) | 22.1 | 30 | 0.6 | 0.009 | 25,067.9 | 651,767.9 |
HM-16 | Equisetum hyemale | 6 (LyNO, Ly, ImNO) | 66.6 | 9 | 0.5 | 0.008 | 27,677.6 | 719,619.6 |
HM-17 | Apocynum venetum | 5(LyNO, Ly, ImNO) | 49.3 | 12 | 0.5 | 0.008 | 28,071.0 | 729,847.7 |
HM-18 | Siphonostegia chinensis | 13 (Im, ImNO, LyNO) | 51.8 | 9 | 0.4 | 0.006 | 35,530.7 | 923,798.5 |
HM-19 | Achillea alpina | 4 (Sk, Im, Ly) | 51.9 | 45 | 2.3 | 0.033 | 7103.4 | 184,688.5 |
HM-20 | Phryma leptostachya | 6 (LyNO, Ly, ImNO) | 45.7 | 15 | 0.6 | 0.009 | 24,179.6 | 628,671.4 |
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Wang, J.; Zhang, M.; Chen, L.; Qiao, Y.; Ma, S.; Sun, D.; Si, J.; Liao, Y. Determination of Toxic Pyrrolizidine Alkaloids in Traditional Chinese Herbal Medicines by UPLC-MS/MS and Accompanying Risk Assessment for Human Health. Molecules 2021, 26, 1648. https://doi.org/10.3390/molecules26061648
Wang J, Zhang M, Chen L, Qiao Y, Ma S, Sun D, Si J, Liao Y. Determination of Toxic Pyrrolizidine Alkaloids in Traditional Chinese Herbal Medicines by UPLC-MS/MS and Accompanying Risk Assessment for Human Health. Molecules. 2021; 26(6):1648. https://doi.org/10.3390/molecules26061648
Chicago/Turabian StyleWang, Junchi, Meng Zhang, Lihua Chen, Yue Qiao, Siqi Ma, Dian Sun, Jianyong Si, and Yonghong Liao. 2021. "Determination of Toxic Pyrrolizidine Alkaloids in Traditional Chinese Herbal Medicines by UPLC-MS/MS and Accompanying Risk Assessment for Human Health" Molecules 26, no. 6: 1648. https://doi.org/10.3390/molecules26061648