Screening and Identification of Mitragynine and 7-Hydroxymitragynine in Human Urine by LC-MS/MS
Abstract
:1. Introduction
2. Experimental Section
2.1. Chemicals and Materials
2.2. Instrumentation
2.3. Standard Solutions
3. Results and Discussion
3.1. HPLC Conditions
3.2. Mass Spectrometry Parameters
Ion Spray Voltage | 2500 V |
Temperature | 600 °C |
Collision Gas | Medium |
Ion Source Gas 1 | 50.0 |
Ion Source Gas 2 | 70.0 |
Compound | Precursor ion (m/z) | Product ion (m/z) | Collision energy (volts) |
---|---|---|---|
Mitragynine | 399.3 | 174.1/159.0 | 40/55 |
Mitragynine-D3 | 402.3 | 238.1 | 30 |
7-Hydroxymitragynine | 415.3 | 190.0/238.1 | 40/27 |
7-Hydroxymitragynine-D3 | 418.3 | 193.1 | 40 |
3.3. Method Validation
3.3.1. Linearity
3.3.2. Carryover
3.3.3. Sensitivity
3.3.4. Precision
3.3.5. Stability
3.3.5.1. Short-Term Stability (Autosampler Stability)
Mitragynine | 7-hydroxymitragynine | |||
---|---|---|---|---|
Low QC | High QC | Low QC | High QC | |
T0 | 0.1502 ng/mL | 1.0000 ng/mL | 0.7502 ng/mL | 4.9983 ng/mL |
Tx | 0.1498 ng/mL | 0.9997 ng/mL | 0.7502 ng/mL | 5.0000 ng/mL |
% Difference | 0.266% | 0.03% | 0% | −0.034% |
3.3.5.2. Long-Term Stability (Storage Stability)
Mitragynine | 7-hydroxymitragynine | |||
---|---|---|---|---|
Low QC | High QC | Low QC | High QC | |
T0 | 0.1500 ng/mL | 1.0017 ng/mL | 0.7500 ng/mL | 4.9967 ng/mL |
Tx | 0.1503 ng/mL | 0.9990 ng/mL | 0.7500 ng/mL | 5.0000 ng/mL |
% Difference | −0.20% | 0.27% | 0% | −0.066% |
3.3.6. Matrix Effect Study
3.4. Capability of the Established Method
Analyte Peak Name (MRM Transition) | Mean Calculated Concentration (ng/mL) | Std. Deviation (ng/mL) | %CV | Number of Values Used | Mean Accuracy (%) |
---|---|---|---|---|---|
Mitragynine1 (399.300/174.100 Da) | 3.594 | 0.004 | 0.12 | 2 | 95.84 |
Mitragynine 2 (399.300/159.000 Da) | 3.398 | 0.057 | 1.69 | 2 | 90.60 |
7-hydroxymitragynine 1 (415.300/190.000 Da) | 3.884 | 0.048 | 1.24 | 2 | 103.57 |
7-hydroxymitragynine 2 (415.300/238.100 Da) | 3.516 | 0.059 | 1.69 | 2 | 93.75 |
mitragynine 1 (399.300/174.100 Da) | 24.616 | 0.353 | 1.44 | 2 | 98.46 |
mitragynine 2 (399.300/159.000 Da) | 23.915 | 0.282 | 1.18 | 2 | 95.66 |
7-hydroxymitragynine 1 (415.300/190.000 Da) | 24.844 | 0.107 | 0.43 | 2 | 99.37 |
7-hydroxymitragynine 2 (415.300/238.100 Da) | 27.241 | 0.678 | 2.49 | 2 | 108.96 |
4. Conclusions
Acknowledgements
Author Contributions
Conflicts of Interest
References
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Fu, H.; Cid, F.X.; Dworkin, N.; Cocores, J.; Shore, G. Screening and Identification of Mitragynine and 7-Hydroxymitragynine in Human Urine by LC-MS/MS. Chromatography 2015, 2, 253-264. https://doi.org/10.3390/chromatography2020253
Fu H, Cid FX, Dworkin N, Cocores J, Shore G. Screening and Identification of Mitragynine and 7-Hydroxymitragynine in Human Urine by LC-MS/MS. Chromatography. 2015; 2(2):253-264. https://doi.org/10.3390/chromatography2020253
Chicago/Turabian StyleFu, Hanzhuo, Frank X. Cid, Nat Dworkin, James Cocores, and Gloria Shore. 2015. "Screening and Identification of Mitragynine and 7-Hydroxymitragynine in Human Urine by LC-MS/MS" Chromatography 2, no. 2: 253-264. https://doi.org/10.3390/chromatography2020253