Simultaneous Determination of Five Iridoids of Picrorhiza scrophulariiflora in Rat Plasma Using UHPLC-ESI-MS/MS
Abstract
:1. Introduction
2. Results and Discussion
2.1. Optimization of Chromatographic and Mass Spectrometric Conditions
2.2. Selection of Internal Standard
2.3. Optimization of Plasma Sample Processing Method
2.4. UHPLC-MS/MS Method Validation
2.4.1. Specificity
2.4.2. Linearity and Lowest Limit of Quantification (LLOQ)
2.4.3. Extraction Recovery and Matrix Effect
2.4.4. Intra-Day and Inter-Day Precision and Accuracy
2.4.5. Stability
2.5. Pharmacokinetic Characteristics
3. Materials and Methods
3.1. Chemicals and Reagents
3.2. Preparation of Standard Solutions
3.3. Processing of Plasma Samples
3.4. Instrumentation and LC–MS/MS Analytical Conditions
3.5. Validation of Analytical Methods for Plasma Samples
3.5.1. Specificity
3.5.2. Linearity and Lowest Limit of Quantification (LLOQ)
3.5.3. Extraction Recovery and Matrix Effects
3.5.4. Intra-Day and Inter-Day Precision and Accuracy
3.5.5. Stability
3.6. Pharmacokinetic and Data Analysis
3.6.1. Animals
3.6.2. Preparation of PS Gavage Solution
3.6.3. Dosing Regimen and Sample Collection and Processing
3.6.4. Plasma Sample Determination
3.6.5. Calculation of Pharmacokinetic Parameters
4. Conclusions
Author Contributions
Funding
Institutional Review Board Statement
Informed Consent Statement
Data Availability Statement
Acknowledgments
Conflicts of Interest
Sample Availability
References
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ID | Regression Equation | Linear Range (ng/mL) | r | LLOQ (ng/mL) |
---|---|---|---|---|
Picroside-I | Y = 1.32 × 10−3X + 2.7 × 10−3 | 6.876–764.0 | 0.9973 | 6.876 |
Picroside-II | Y = 8.51 × 10−3X + 6.2 × 10−2 | 5.193–577.0 | 0.9983 | 5.193 |
Picroside-III | Y = 0.82 × 10−3X + 0.6 × 10−3 | 5.040–560.0 | 0.9954 | 5.040 |
Minecoside | Y = 5.32 × 10−3X − 1.3 × 10−1 | 1.260–140.0 | 0.9911 | 1.260 |
Sweroside | Y = 2.20 × 10−2X + 0.4 × 10−2 | 4.527–503.0 | 0.9989 | 4.527 |
Compound | QC (ng/mL) | Recovery | Matrix Effect | ||
---|---|---|---|---|---|
Mean ± SD (%) | RSD (%) | Mean ± SD (%) | RSD (%) | ||
Picroside-I | 13.75 | 86.51 ± 4.2 | 4.9 | 96.17 ± 2.6 | 2.7 |
382.0 | 85.12 ± 3.6 | 4.2 | 101.9 ± 5.4 | 5.3 | |
573.0 | 91.34 ± 2.3 | 2.5 | 98.93 ± 6.4 | 6.5 | |
Picroside-II | 10.39 | 71.02 ± 8.2 | 11.5 | 101.7 ± 7.6 | 7.5 |
288.5 | 67.11 ± 4.0 | 6.0 | 99.71 ± 7.2 | 7.2 | |
432.8 | 72.53 ± 4.6 | 6.3 | 97.26 ± 5.1 | 5.2 | |
Picroside-III | 10.08 | 76.43 ± 6.1 | 8.0 | 95.77 ± 3.7 | 3.9 |
280.0 | 80.47 ± 3.3 | 4.1 | 99.32 ± 2.9 | 2.9 | |
420.0 | 83.84 ± 2.5 | 3.0 | 101.8 ± 4.8 | 4.7 | |
Minecoside | 2.520 | 77.62 ± 8.9 | 11.4 | 96.84 ± 5.4 | 5.6 |
70.00 | 83.16 ± 6.1 | 7.3 | 97.17 ± 2.6 | 2.7 | |
105.00 | 80.45 ± 3.7 | 4.6 | 97.47 ± 5.1 | 5.2 | |
Sweroside | 9.054 | 82.25 ± 6.8 | 8.3 | 98.61 ± 7.5 | 7.6 |
251.5 | 85.36 ± 5.6 | 6.6 | 98.65 ± 6.4 | 6.5 | |
377.2 | 79.57 ± 2.0 | 2.5 | 101.5 ± 3.7 | 3.6 |
ID | QC (ng/mL) | Inter-Day | Intra-Day | ||
---|---|---|---|---|---|
RSD (%) | RE (%) | RSD (%) | RE (%) | ||
Picroside-I | 6.876 | 5.5 | 1.3 | 7.7 | 6.1 |
13.75 | 6.8 | 1.2 | 7.9 | 5.8 | |
382.0 | 8.9 | 1.1 | 6.9 | 4.1 | |
573.0 | 5.6 | 2.6 | 6.6 | 3.1 | |
Picroside-II | 5.193 | 5.7 | 12.9 | 9.7 | 6.3 |
10.39 | 4.8 | −12.1 | 9.4 | −4.3 | |
288.5 | 8.5 | 13.2 | 10.1 | 7.1 | |
432.8 | 6.1 | 8.7 | 4.2 | 2.9 | |
Picroside-III | 5.040 | 6.2 | 11.5 | 8.1 | 6.8 |
10.08 | 5.8 | −11.3 | 7.6 | −3.4 | |
280.0 | 7.5 | 6.5 | 5.0 | 6.6 | |
420.0 | 5.9 | 2.0 | 5.8 | 6.3 | |
Minecoside | 1.260 | 10.2 | 12.8 | 7.0 | 12.9 |
2.520 | 9.7 | −12.3 | 4.1 | 13.2 | |
70.00 | 6.5 | 5.6 | 6.5 | 8.7 | |
105.00 | 11.1 | 2.2 | 6.7 | −10.3 | |
Sweroside | 4.527 | 9.1 | 10.8 | 9.4 | 10.7 |
9.054 | 7.6 | 11.2 | 7.8 | 6.3 | |
251.5 | 9.0 | −4.8 | 9.1 | 3.5 | |
377.2 | 6.8 | 8.8 | 8.8 | 11.3 |
ID | QC (ng/mL) | Short-Term Stability | Stability after Preparation | Freeze-Thaw | Long-Term Stability | ||||
---|---|---|---|---|---|---|---|---|---|
RSD (%) | RE (%) | RSD (%) | RE (%) | RSD (%) | RE (%) | RSD (%) | RE (%) | ||
Picroside-I | 13.75 | 5.1 | 8.93 | 5.8 | 6.80 | 7.1 | 6.43 | 10.9 | 5.60 |
382.0 | 2.9 | 3.83 | 6.8 | 9.73 | 5.0 | −2.74 | 8.1 | −5.69 | |
573.0 | 2.9 | 6.58 | 4.7 | 7.02 | 5.3 | −1.94 | 7.7 | 3.59 | |
Picroside-II | 10.39 | 4.4 | −4.99 | 4.4 | −3.26 | 4.2 | 7.08 | 7.6 | 8.69 |
288.5 | 3.6 | 8.53 | 5.0 | 6.66 | 5.9 | −7.21 | 6.6 | 1.37 | |
432.8 | 2.7 | 4.47 | 2.8 | −6.58 | 4.3 | −1.47 | 5.0 | −2.19 | |
Picroside-III | 10.08 | 4.5 | −2.91 | 3.0 | 9.08 | 6.3 | 2.75 | 11.1 | 5.66 |
280.0 | 3.2 | 6.82 | 5.5 | 7.95 | 5.1 | −5.33 | 6.3 | −1.92 | |
420.0 | 3.1 | 4.51 | 3.4 | −4.87 | 3.5 | −1.64 | 4.2 | −4.99 | |
Minecoside | 2.520 | 4.5 | 3.33 | 3.3 | 6.38 | 11.1 | −1.90 | 4.5 | 3.31 |
70.00 | 3.2 | 5.72 | 5.7 | 5.13 | 6.3 | 7.16 | 2.2 | 5.70 | |
105.00 | 3.1 | 3.40 | 3.4 | 3.56 | 4.2 | −6.28 | 2.1 | 3.41 | |
Sweroside | 9.054 | 1.9 | 3.68 | 4.7 | 9.17 | 5.3 | −1.94 | 7.7 | 3.59 |
251.5 | 4.3 | −5.09 | 2.4 | 4.06 | 4.2 | 7.08 | 7.6 | 8.69 | |
377.2 | 1.6 | 9.62 | 5.0 | 6.66 | 5.9 | −7.21 | 6.6 | 1.37 |
ID | Cmax (ng/mL) | Tmax (h) | t1/2 (h) | AUC0–t (ng h/mL) | AUC0–∞ (ng h/mL) | MRT0–t (h) | Cl (L/h/kg) | Vd (L/kg) |
---|---|---|---|---|---|---|---|---|
Picroside-I | 114.2 ± 16.1 | 1.1 ± 0.2 | 2.4 ± 0.3 | 360.9 ± 25.6 | 381.8 ± 29.4 | 3.6 ± 0.2 | 36.43 ± 17.436 | 186.7 ± 17.436 |
Picroside-II | 335.9 ± 92.3 | 1.1 ± 0.1 | 2.3 ± 1.5 | 603.9 ± 239.4 | 610.8 ± 246.1 | 2.3 ± 0.5 | 172.40 ± 59.96 | 796 ± 503.5 |
Picroside-III | 148.2 ± 21.6 | 0.8 ± 0.1 | 17.5 ± 3.1 | 339.4 ± 56.1 | 597.6 ± 198.1 | 3.4 ± 0.1 | 90.07 ± 34.33 | 2747 ± 1642 |
Minecoside | 21.1 ± 7.8 | 1.0 ± 0.2 | 5.0 ± 2.3 | 78.9 ± 10.2 | 93.5 ± 22.6 | 4.1 ± 0.7 | 7.148 ± 2.382 | 19.26 ± 4.77 |
Sweroside | 63.7 ± 17.6 | 2.1 ± 0.1 | 1.2 ± 0.3 | 261.2 ± 65.3 | 267.9 ± 70.8 | 3.9 ± 0.3 | 120.9 ± 36.95 | 785.1 ± 130.6 |
ID | Parent Ion (m/z) | Daughter Ion (m/z) | DP (V) | CE (eV) |
---|---|---|---|---|
Picroside-I | 491.2 | 147.0 | −75.20 | −12.90 |
Picroside-II | 511.3 | 234.8 | −96.20 | −33.30 |
Picroside-III | 537.4 | 261.0 | −101.29 | −30.00 |
Minecoside | 537.5 | 281.4 | −84.92 | −13.46 |
Sweroside | 403.2 | 195.0 | −45.86 | −18.75 |
IS | 525.2 | 449.1 | −59.40 | −20.02 |
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Wang, Z.; Shi, X.; Jiang, S.; Sun, J.; Borjigin, G.; Li, Q.; Mu, Y.; Yang, C.; Wang, Z.; Kuang, H. Simultaneous Determination of Five Iridoids of Picrorhiza scrophulariiflora in Rat Plasma Using UHPLC-ESI-MS/MS. Molecules 2023, 28, 5925. https://doi.org/10.3390/molecules28155925
Wang Z, Shi X, Jiang S, Sun J, Borjigin G, Li Q, Mu Y, Yang C, Wang Z, Kuang H. Simultaneous Determination of Five Iridoids of Picrorhiza scrophulariiflora in Rat Plasma Using UHPLC-ESI-MS/MS. Molecules. 2023; 28(15):5925. https://doi.org/10.3390/molecules28155925
Chicago/Turabian StyleWang, Zhibin, Xuepeng Shi, Shuang Jiang, Jiahui Sun, Gilwa Borjigin, Qi Li, Yuanqiu Mu, Chunjuan Yang, Zhenyue Wang, and Haixue Kuang. 2023. "Simultaneous Determination of Five Iridoids of Picrorhiza scrophulariiflora in Rat Plasma Using UHPLC-ESI-MS/MS" Molecules 28, no. 15: 5925. https://doi.org/10.3390/molecules28155925