Validation of a Simple HPLC-Based Method for Lysine Quantification for Ruminant Nutrition
Abstract
:1. Introduction
2. Results and Discussion
2.1. Method Optimization
2.2. Method Validation
3. Materials and Methods
3.1. Materials
3.2. Preparation of the Matrices Samples
3.3. Derivatization
3.4. Chromatographic Conditions
3.5. Method Validation
3.6. Sample Stability
3.7. Application of the Method towards Lys Quantification
4. Conclusions
Supplementary Materials
Author Contributions
Funding
Institutional Review Board Statement
Informed Consent Statement
Data Availability Statement
Acknowledgments
Conflicts of Interest
Sample Availability
References
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Compound | tR (min; Mean (RSD)) | k | N | α | Rs |
---|---|---|---|---|---|
Lysine | 13.5 (0.2) | 6.9 | 2037 | 1.2 | 1.9 |
IS | 15.7 (0.1) | 8.2 | 3275 |
Matrix | Range (µM) | Slope | Correlation Coefficient | LOD (µM) | LOQ (µM) |
---|---|---|---|---|---|
Li2CO3 | 1–225 | 0.011265 | 0.9999 | 0.12 | 0.41 |
PBS | 1–225 | 0.009982 | 0.9998 | 0.16 | 0.53 |
Rumen | 5–225 | 0.031104 | 0.9996 | 1.24 | 4.14 |
Matrix | Concentration (µM) | Accuracy (%) | Precision (%) | |
---|---|---|---|---|
Intra-Day | Inter-Day | |||
Li2CO3 | 25 | 94 ± 3 | 2 ± 1 | 13 ± 7 |
PBS | 25 | 92 ± 2 | 2 ± 3 | 22 ± 10 |
Rumen | 25 | 92 ± 9 | 9 ± 5 | 9 ± 5 |
Matrix | 24 h | 48 h | 96 h | ||||||
---|---|---|---|---|---|---|---|---|---|
A | B | C | A | B | C | A | B | C | |
Recovery (%) when stored at RT | |||||||||
Li2CO3 | 99 ± 2 | 286 ± 83 | 102 ± 1 | 75 ± 4 | 343 ± 67 | 109 ± 1 | 76 ± 4 | 151 ± 762 | 83 ± 1 |
PBS | 100 ± 1 | 211 ± 7 | 100 ± 1 | 101 ± 1 | 588 ± 17 | 105 ± 1 | 100 ± 1 | 1976 ± 62 | 85 ± 1 |
Rumen | 100 ± 3 | 8414 ± 1472 | 99 ± 1 | 107 ± 14 | 5375 ± 4227 | 100 ± 1 | 106 ± 13 | 2105 ± 2917 | 95 ± 1 |
Recovery (%) when stored at 4 °C | |||||||||
Li2CO3 | 101 ± 1 | 167 ± 5 | 103 ± 1 | 115 ± 70 | 111 ± 3 | 108 ± 1 | 344 ± 377 | 155 ± 6 | 83 ± 1 |
PBS | 100 ± 1 | 115 ± 5 | 100 ± 1 | 101 ± 1 | 168 ± 5 | 105 ± 1 | 100 ± 1 | 189 ± 7 | 85 ± 1 |
Rumen | 99 ± 3 | 69 ± 2 | 99 ± 1 | 101 ± 9 | 83 ± 21 | 101 ± 1 | 99 ± 9 | 4891 ± 2198 | 96 ± 1 |
Recovery (%) when stored at −20 °C | |||||||||
Li2CO3 | 338 ± 111 | 134 ± 7 | 102 ± 1 | 400 ± 98 | 85 ± 15 | 108 ± 1 | 368 ± 96 | 91 ± 7 | 83 ± 1 |
PBS | 105 ± 9 | 105 ± 10 | 100 ± 1 | 524 ± 264 | 122 ± 6 | 106 ± 1 | 410 ± 178 | 110 ± 7 | 85 ± 1 |
Rumen | 474 ± 91 | 147 ± 19 | 99 ± 1 | 287 ± 62 | 140 ± 11 | 101 ± 1 | 522 ± 422 | 167 ± 27 | 96 ± 1 |
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Albuquerque, J.; Casal, S.; Cruz, R.; Van Dorpe, I.; Maia, M.R.G.; Fonseca, A.J.M.; Cabrita, A.R.J.; Neves, A.R.; Reis, S. Validation of a Simple HPLC-Based Method for Lysine Quantification for Ruminant Nutrition. Molecules 2021, 26, 4173. https://doi.org/10.3390/molecules26144173
Albuquerque J, Casal S, Cruz R, Van Dorpe I, Maia MRG, Fonseca AJM, Cabrita ARJ, Neves AR, Reis S. Validation of a Simple HPLC-Based Method for Lysine Quantification for Ruminant Nutrition. Molecules. 2021; 26(14):4173. https://doi.org/10.3390/molecules26144173
Chicago/Turabian StyleAlbuquerque, João, Susana Casal, Rebeca Cruz, Ingrid Van Dorpe, Margarida Rosa Garcez Maia, António José Mira Fonseca, Ana Rita Jordão Cabrita, Ana Rute Neves, and Salette Reis. 2021. "Validation of a Simple HPLC-Based Method for Lysine Quantification for Ruminant Nutrition" Molecules 26, no. 14: 4173. https://doi.org/10.3390/molecules26144173