Rapid Evaluation of Spermidine from 12 Bean Cultivars by Direct Real-Time Mass Spectrometry Analysis
Abstract
:1. Introduction
2. Results and Discussion
2.1. Comparison of MS and MS/MS Spectra of SPD Fragments
2.2. Optimization of the DART-MS Conditions
2.2.1. Effect of Gas Heating Temperature of DART Ion Source
2.2.2. Effect of Grid Voltage
2.2.3. Effect of Sample Presentation Speed
2.2.4. Effect of Collision Energy (CE)
2.2.5. Method Validation
2.3. Matrix Effect
2.4. Qualitative Analysis of SPD in Beans by DART-MS
3. Materials and Methods
3.1. Sample and Reagents
3.2. Preparation of Standard and Sample Solution
3.3. DART-MS Analysis
3.4. UHPLC-QTOF-MS Analysis
3.5. Method Validation
3.6. Data Analysis
4. Conclusions
Supplementary Materials
Author Contributions
Funding
Acknowledgments
Conflicts of Interest
References
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Sample Availability: Samples of the 12 bean cultivars are available from the authors. |
Method | Linear | R2 | LOD (mg/kg) | LOQ (mg/kg) | Precision | |
---|---|---|---|---|---|---|
Intra-Day | Inter-Day | |||||
DART-MS | y = 292923x − 45007 | 0.990 | 0.025 | 0.078 | 3.6% | 7.50% |
UHPLC-ESI-QTOF | y = 89517x − 8931 | 0.999 | 0.036 | 0.131 | 2.15% | 5.30% |
Variety | Sample Measurement (mg/L) | Spiked (mg/L) | DART-MS Recovery (%) | UHPLC-ESI-MS Recovery (%) |
---|---|---|---|---|
NO.12 | 1.20 ± 0.03 | 0.625 | 102.79 ± 3.13 | 95.64 ± 1.44 |
1.25 | 115.70 ± 4.01 | 93.31 ± 1.91 | ||
2.5 | 148.44 ± 3.83 | 103.60 ± 1.75 |
Matrix | Method | Equation of Calibration Curve | Matrix Effect (%) |
---|---|---|---|
Blank | DART-MS | y = 292923x − 45007 | - |
UHPLC-ESI-QTOF | y = 89517x − 8931 | - | |
NO. 12 | DART-MS | y = 331591x + 26566 | 13.20% |
UHPLC-ESI-QTOF | y = 107561x + 528890 | 20.16% |
Number | DART-MS (mg/kg) | UHPLC-ESI-QTOF (mg/kg) |
---|---|---|
1 | 3.42 ± 0.05 | 3.38 ± 0.06 |
2 | 3.87 ± 0.17 * | 3.19 ± 0.08 |
3 | 9.62 ± 0.15 * | 9.16 ± 0.10 |
4 | 10.44 ± 0.26 * | 9.55 ± 0.14 |
5 | 5.28 ± 0.28 | 4.90 ± 0.10 |
6 | 3.58 ± 0.23 * | 5.22 ± 0.08 |
7 | 2.96 ± 0.10 * | 2.15 ± 0.07 |
8 | 3.63 ± 0.14 * | 1.95 ± 0.03 |
9 | 2.01 ± 0.06 * | 1.84 ± 0.01 |
10 | 5.11 ± 0.31 * | 3.34 ± 0.20 |
11 | 4.55 ± 0.22 * | 3.64 ± 0.10 |
12 | 12.08 ± 0.35 * | 13.45 ± 0.19 |
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Wu, T.; Wu, X.; Yuan, X.; Wang, Y.; Zhou, W.; Li, W. Rapid Evaluation of Spermidine from 12 Bean Cultivars by Direct Real-Time Mass Spectrometry Analysis. Molecules 2018, 23, 2138. https://doi.org/10.3390/molecules23092138
Wu T, Wu X, Yuan X, Wang Y, Zhou W, Li W. Rapid Evaluation of Spermidine from 12 Bean Cultivars by Direct Real-Time Mass Spectrometry Analysis. Molecules. 2018; 23(9):2138. https://doi.org/10.3390/molecules23092138
Chicago/Turabian StyleWu, Tao, Xiaoyu Wu, Xv Yuan, Yi Wang, Wenhua Zhou, and Weili Li. 2018. "Rapid Evaluation of Spermidine from 12 Bean Cultivars by Direct Real-Time Mass Spectrometry Analysis" Molecules 23, no. 9: 2138. https://doi.org/10.3390/molecules23092138