Quantification of Oxidized and Unsaturated Bile Alcohols in Sea Lamprey Tissues by Ultra-High Performance Liquid Chromatography-Tandem Mass Spectrometry
Abstract
:1. Introduction
2. Results and Discussion
2.1. Method Development
2.2. Calibration and Method Validation
2.3. Matrix Effects
2.4. Quantitative Analysis of Sulfated BAs in Tissues
3. Experimental Section
3.1. Chemicals and Reagents
3.2. Preparation of Calibration Standards, Quality Control, and Internal Standard Solutions
3.3. Quantitative Conditions by UHPLC-MS/MS
3.4. Tissue Sample Preparation, Extraction, and Quantification
3.5. Method Validation
3.6. Data Analysis and Statistics
4. Conclusions
Acknowledgments
Author Contributions
Conflicts of Interest
References
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Compounds | [M − H]− m/z | MRM m/z | CV (V) | CE (eV) | RT (min) | LR | R2 | LOD (ng/g) | LOQ (ng/g) |
---|---|---|---|---|---|---|---|---|---|
1 | 465.2 | 465.2 > 96.7 | 49 | 40 | 0.89 | 0.1–1000 | 0.9918 | 0.10 | 0.33 |
2 | 467.3 | 467.3 > 96.7 | 23 | 40 | 1.08 | 0.1–1000 | 0.9924 | 0.10 | 0.33 |
3 | 469.3 | 469.3 > 96.7 | 36 | 40 | 2.90 | 0.2–1000 | 0.9973 | 0.20 | 0.66 |
4 | 469.3 | 469.3 > 96.7 | 23 | 40 | 3.16 | 0.2–1000 | 0.9952 | 0.20 | 0.66 |
[2H5]-3kPZS | 476.3 | 476.3 > 96.7 | 100 | 23 | 3.05 | 0.5–1000 | 0.9986 | 0.30 | 0.99 |
Analyte | NC (ng/g) | Intra-Day (n = 6) | Inter-Day (n = 6) | ||||
---|---|---|---|---|---|---|---|
MC (Mean ± SD, ng/mL) | Accuracy (DEV %) | Precision (RSD %) | MC (Mean ± SD, ng/mL) | Accuracy (DEV %) | Precision (RSD %) | ||
1 | 2.5 | 2.4 ± 0.03 | 96.9 | 1.24 | 2.4 ± 0.11 | 95.2 | 4.80 |
25 | 24.1 ± 0.50 | 96.5 | 2.07 | 24.1 ± 1.22 | 96.4 | 5.05 | |
250 | 248.2 ± 1.18 | 99.3 | 0.48 | 245.8 ± 5.84 | 98.3 | 2.38 | |
2 | 2.5 | 2.4 ± 0.03 | 95.5 | 1.22 | 2.5 ± 0.10 | 101.1 | 4.29 |
25 | 24.1 ± 0.72 | 96.3 | 2.99 | 25.0 ± 1.03 | 100.1 | 4.12 | |
250 | 243.6 ± 5.10 | 97.4 | 2.09 | 247.3 ± 3.77 | 98.9 | 1.52 | |
3 | 2.5 | 2.4 ± 0.05 | 97.1 | 1.96 | 2.4 ± 0.04 | 95.7 | 1.81 |
25 | 24.1 ± 0.89 | 96.4 | 3.70 | 25.2 ± 1.06 | 100.8 | 4.21 | |
250 | 248.3 ± 2.03 | 99.3 | 0.82 | 247.3 ± 4.25 | 98.9 | 1.72 | |
4 | 2.5 | 2.41 ± 0.04 | 96.3 | 1.67 | 2.4 ± 0.04 | 97.03 | 1.87 |
25 | 24.6 ± 0.99 | 98.3 | 4.03 | 25.2 ± 0.93 | 100.6 | 3.69 | |
250 | 247.5 ± 0.76 | 99.0 | 0.31 | 250.3 ± 13.21 | 100.1 | 5.28 |
Matrix | Analyte | Mean Extraction Recovery (%) | Matrix Effect (%) | ||||
---|---|---|---|---|---|---|---|
Low | Medium | High | Low | Medium | High | ||
Liver | 1 | 96.3 (2.3) | 95.6 (3.1) | 92.9 (1.5) | 97.3 (4.1) | 99.3 (3.2) | 96.3 (2.9) |
2 | 92.3 (1.8) | 95.2 (2.0) | 91.3 (3.2) | 90.3 (3.2) | 92.3 (2.9) | 92.6 (2.1) | |
3 | 87.9 (3.1) | 89.6 (2.7) | 88.6 (3.4) | 89.6 (3.5) | 87.9 (3.2) | 88.6 (2.8) | |
4 | 92.3 (2.6) | 86.3 (2.5) | 84.3 (2.7) | 85.9 (1.6) | 95.6 (2.7) | 89.6 (2.2) | |
Kidney | 1 | 96.3 (2.5) | 95.8 (1.4) | 95.6 (3.2) | 98.6 (2.3) | 96.3 (4.2) | 95.8 (4.9) |
2 | 95.3 (2.4) | 95.6 (2.5) | 94.3 (4.5) | 88.9 (3.1) | 87.6 (2.2) | 89.6 (1.8) | |
3 | 86.9 (3.0) | 89.6 (1.9) | 92.3 (3.1) | 87.9 (3.8) | 86.9 (2.7) | 89.6 (3.6) | |
4 | 91.2 (2.0) | 89.6 (1.7) | 93.2 (2.9) | 92.3 (1.1) | 85.6 (1.9) | 86.9 (1.7) | |
Intestine | 1 | 96.3 (3.3) | 95.3 (2.7) | 94.2 (2.5) | 95.3 (3.6) | 94.3 (2.8) | 95.6 (1.9) |
2 | 94.2 (2.9) | 95.3 (3.1) | 92.3 (2.9) | 93.6 (4.0) | 92.7 (3.8) | 93.5 (2.5) | |
3 | 86.3 (3.2) | 87.5 (4.1) | 89.6 (1.9) | 87.9 (3.5) | 85.9 (1.8) | 89.6 (1.7) | |
4 | 92.5 (3.4) | 95.6 (2.9) | 91.5 (3.2) | 95.2 (1.3) | 93.2 (2.7) | 94.3 (1.6) |
Sample | Concentration (ng/g) | |||
---|---|---|---|---|
1 | 2 | 3 | 4 | |
Kidney | N.D | N.D | N.D | N.D |
Intestine | N.D | N.D | 0.85 | 0.74 |
Liver extract | N.D | N.D | 0.81 | 0.92 |
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Li, K.; Scott, A.M.; Chung-Davidson, Y.-W.; Bussy, U.; Patel, T.; Middleton, Z.E.; Li, W. Quantification of Oxidized and Unsaturated Bile Alcohols in Sea Lamprey Tissues by Ultra-High Performance Liquid Chromatography-Tandem Mass Spectrometry. Molecules 2016, 21, 1119. https://doi.org/10.3390/molecules21091119
Li K, Scott AM, Chung-Davidson Y-W, Bussy U, Patel T, Middleton ZE, Li W. Quantification of Oxidized and Unsaturated Bile Alcohols in Sea Lamprey Tissues by Ultra-High Performance Liquid Chromatography-Tandem Mass Spectrometry. Molecules. 2016; 21(9):1119. https://doi.org/10.3390/molecules21091119
Chicago/Turabian StyleLi, Ke, Anne M. Scott, Yu-Wen Chung-Davidson, Ugo Bussy, Trinkal Patel, Zoe E. Middleton, and Weiming Li. 2016. "Quantification of Oxidized and Unsaturated Bile Alcohols in Sea Lamprey Tissues by Ultra-High Performance Liquid Chromatography-Tandem Mass Spectrometry" Molecules 21, no. 9: 1119. https://doi.org/10.3390/molecules21091119