Multidimensional Chromatographic Fingerprinting Combined with Chemometrics for the Identification of Regulated Plants in Suspicious Plant Food Supplements
Abstract
:1. Introduction
2. Results
2.1. Final Chromatographic Conditions
2.2. Correlation Analysis and Choice of Wavelengths
2.3. Chemometric Analysis
2.3.1. Partial Least Squares–Discriminant Analysis
Binary Models
Multiclass Models
2.3.2. Real Samples
2.3.3. Comparison of Results Obtained for 254 nm and for Selected Wavelengths
3. Materials and Methods
3.1. Samples and Reagents
3.2. Sample Preparation
3.2.1. Preparation of Reference Solutions
3.2.2. Preparation of Triturations
3.2.3. Preparation of Samples
3.3. Instrumentation and Conditions
3.3.1. Preparation of Reference Solutions
Method Development
3.4. Selection of Wavelengths
3.5. Data
3.5.1. Data Set Preparation and Multidimensional Fingerprints
3.5.2. Peak Alignment
3.5.3. Data Pretreatment
3.5.4. Test Set Selection
3.5.5. PLS-DA
3.5.6. Software
4. Discussion and Conclusions
Supplementary Materials
Author Contributions
Funding
Institutional Review Board Statement
Data Availability Statement
Conflicts of Interest
Sample Availability
References
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Aristolochia fanghi | Ilex paraguariensis | Hoodia gordonii | Garcinia cambogia |
---|---|---|---|
264 | 210 | 249 | 249 |
284 | 230 | 266 | 265 |
305 | 282 | 280 | 303 |
322 | 361 | 325 | 316 |
333 | 382 | 360 |
Type of Data Set | Class Assigned | Total Samples in the Data Set | No. of Samples in Training Set | No. of Samples in Test Set |
---|---|---|---|---|
Binary data set | 1, 2 | 67 | 50 | 17 |
Multiclass data set | 1, 2, 3, 4, 5 | 235 | 176 | 59 |
Slimming Plant | PLS Factors | Cross Validation (ccr%) with Misclassified Samples between Brackets () | Modelling (ccr%) | External Test Set Prediction (ccr%) with Misclassified Samples between Brackets () |
---|---|---|---|---|
Aristolochia fanghi | 23 | 94% (3/50) | 96% | 94% (1/17) |
Ilex paraguariensis | 14 | 96% (2/50) | 100% | 94% (1/17) |
Hoodia gordonii | 20 | 88% (6/50) | 96% | 94% (1/17) |
Garcinia cambogia | 22 | 96% (1/50) | 98% | 88% (2/17) |
Slimming Plant | True Positives Training Set Test Set (cv) | False Positives Training Set Test Set (cv) | True Negatives Training Set Test Set (cv) | False Negatives Training Set Test Set (cv) | ||||
---|---|---|---|---|---|---|---|---|
Aristolochia fanghi | 45 | 12 | 2 | 1 | 3 | 4 | 0 | 0 |
Ilex paraguariensis | 43 | 12 | 2 | 0 | 5 | 4 | 0 | 1 |
Hoodia gordonii | 42 | 14 | 6 | 1 | 2 | 2 | 0 | 0 |
Garcinia cambogia | 43 | 13 | 2 | 2 | 5 | 2 | 0 | 0 |
Slimming Plant | PLS Factors | Cross Validation (ccr%) with Misclassified Samples between Brackets () | Modelling (ccr%) | External Test Set Validation (ccr%) with Misclassified Samples between Brackets () |
---|---|---|---|---|
Aristolochia fanghi | 22 | 91% (15/176) | 93% | 90% (6/59) |
Ilex paraguariensis | 18 | 93% (12/176) | 97% | 88% (7/59) |
Hoodia gordonii | 23 | 87% (23/176) | 94% | 90% (6/59) |
Garcinia cambogia | 22 | 84% (28/176) | 93% | 90% (6/59) |
Slimming Plant | True Positives Training Set Test Set (cv) | False Positives Training Set Test Set (cv) | ||
---|---|---|---|---|
A multiclass model with wavelengths of Aristolochia fanghi | ||||
Aristolochia fanghi | 43 | 13 | 6 | 0 |
Hoodia gordonii | 49 | 6 | 6 | 4 |
Ilex paraguariensis | 29 | 20 | 2 | 0 |
Garcinia cambogia | 39 | 14 | 1 | 2 |
Blank | 0 | 0 | 0 | 0 |
A multiclass model with wavelengths of Ilex paraguariensis | ||||
Aristolochia fanghi | 46 | 10 | 1 | 4 |
Hoodia gordonii | 44 | 9 | 5 | 2 |
Ilex paraguariensis | 34 | 21 | 1 | 0 |
Garcinia cambogia | 40 | 12 | 5 | 0 |
Blank | 0 | 0 | 0 | 1 |
A multiclass model with wavelengths of Hoodia gordonii | ||||
Aristolochia fanghi | 43 | 11 | 8 | 0 |
Hoodia gordonii | 46 | 10 | 10 | 6 |
Ilex paraguariensis | 26 | 23 | 1 | 0 |
Garcinia cambogia | 38 | 8 | 4 | 0 |
Blank | 0 | 1 | 0 | 0 |
A multiclass model with wavelengths of Garcinia cambogia | ||||
Aristolochia fanghi | 40 | 12 | 10 | 2 |
Hoodia gordonii | 35 | 10 | 2 | 2 |
Ilex paraguariensis | 27 | 23 | 1 | 0 |
Garcinia cambogia | 45 | 8 | 13 | 1 |
Blank | 0 | 0 | 2 | 1 |
Samples | Plants Classified According to Binary Modelling (Comparative) | Plants Classified with the Multiclass Model |
---|---|---|
Sample 1 | Ilex paraguariensis, Garcinia cambogia | Garcinia cambogia |
Sample 2 | -- | Garcinia cambogia |
Sample 3 | Aristolochia fanghi, Hoodia gordonii, Garcinia cambogia | Hoodia gordonii |
Sample 4 | Hoodia gordonii, Ilex paraguariensis | Aristolochia fanghi |
Sample 5 | Hoodia gordonii, | Aristolochia fanghi |
Sample 6 | Garcinia cambogia, Ilex paraguariensis | Ilex paraguariensis |
Sample 7 | Aristolochia fanghi, Hoodia gordonii, Garcinia cambogia | Hoodia gordonii |
Sample 8 | -- | -- |
Sample 9 | Aristolochia fanghi, Hoodia gordonii, Garcinia cambogia | Garcinia cambogia |
Sample 10 | Garcinia cambogia, Ilex paraguariensis | Garcinia cambogia |
Sample 11 | Aristolochia fanghi, Hoodia gordonii | Aristolochia fanghi |
Sample 12 | Garcinia cambogia | Aristolochia fanghi |
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Ranjan, S.; Adams, E.; Deconinck, E. Multidimensional Chromatographic Fingerprinting Combined with Chemometrics for the Identification of Regulated Plants in Suspicious Plant Food Supplements. Molecules 2023, 28, 3632. https://doi.org/10.3390/molecules28083632
Ranjan S, Adams E, Deconinck E. Multidimensional Chromatographic Fingerprinting Combined with Chemometrics for the Identification of Regulated Plants in Suspicious Plant Food Supplements. Molecules. 2023; 28(8):3632. https://doi.org/10.3390/molecules28083632
Chicago/Turabian StyleRanjan, Surbhi, Erwin Adams, and Eric Deconinck. 2023. "Multidimensional Chromatographic Fingerprinting Combined with Chemometrics for the Identification of Regulated Plants in Suspicious Plant Food Supplements" Molecules 28, no. 8: 3632. https://doi.org/10.3390/molecules28083632