Colistimethate Acidic Hydrolysis Revisited: Arrhenius Equation Modeling Using UPLC-QToF MS
Abstract
:1. Introduction
2. Results and Discussion
2.1. LC-MS
2.2. Method Validation
2.2.1. Quantitation of the Ratio of CSA and CSB in Reference Sample
2.2.2. Standard Curves
2.2.3. Accuracy and Precision
2.2.4. Stability
2.2.5. Robustness
2.2.6. Limit of Detection and Limit of Quantitation
2.2.7. Carry-Over
2.3. Acidic Hydrolysis of CMS
2.4. Application in Plasma Samples
3. Materials and Methods
3.1. Chemical and Reagents
3.2. Liquid Chromatography
3.3. Mass Spectrometry
3.4. Preparation of Standard Solutions
3.5. Assay Validation
3.6. Acidic Hydrolysis of CMS
3.7. Application to Plasma Samples
4. Conclusions
Supplementary Materials
Author Contributions
Funding
Data Availability Statement
Conflicts of Interest
Sample Availability
References
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Authors | Acid | Concentration (M) | Reaction Time (min) | Temp (°C) |
---|---|---|---|---|
Li et al. [19] | sulfuric | 0.08–0.1 | 10 | room |
Jansson et al. [20] | sulfuric | 1 | 15–20 | room |
Gobin et al. [21] | sulfuric | 0.5 | 60 | room |
Gikas et al. [18] | sulfuric | 0.5 | 60 | room |
Mercier et al. [22] | sulfuric | 1 | 30 | room |
Zhao et al. [15] | sulfuric | 0.5 | 15 | room |
Bihan et al. [16] | sulfuric | 1 | 60 | room |
Analyte (μg mL−1) | Accuracy * (n = 3, %Error) | Repeatability * (n = 3, %RSD) | Intermediate Precision (%RSD) | Autosampler Stability (n = 3, %RSD) | Benchtop Stability (n = 3, %RSD) | Robustness (n = 3, %RSD) |
---|---|---|---|---|---|---|
CSA | ||||||
1.81 | <6.15 | <3.71 | 1.86 | 2.78 | 3.45 | <4.45 |
2.41 | <1.41 | <2.55 | 1.28 | |||
3.61 | <11.05 | <5.61 | 9.07 | 1.15 | 3.12 | <3.12 |
4.82 | <4.71 | <1.73 | 4.23 | |||
6.02 | <2.26 | <5.14 | 3.44 | |||
6.62 | <3.21 | <5.42 | 3.58 | 1.96 | 2.95 | <2.14 |
CSB | ||||||
4.19 | <1.71 | <5.71 | 5.16 | 2.53 | 3.56 | <4.27 |
5.59 | <1.68 | <3.80 | 2.48 | |||
8.39 | <2.02 | <4.39 | 5.59 | 1.84 | 3.78 | <2.95 |
11.18 | <5.33 | <2.55 | 2.13 | |||
13.98 | <5.07 | <3.82 | 2.93 | |||
15.38 | <4.61 | <4.85 | 3.71 | 1.69 | 3.17 | <1.97 |
CMS | ||||||
2 | <11.01 | <5.41 | 5.96 | |||
6 | <13.21 | <5.71 | 5.74 | 2.35 | 7.54 | <4.12 |
8 | <7.91 | <4.27 | 5.06 | |||
12 | <4.79 | <4.54 | 5.98 | 1.87 | 5.58 | <4.05 |
16 | <4.71 | <3.84 | 2.30 | |||
20 | <1.53 | <1.85 | 1.29 | |||
22 | <0.40 | <0.53 | 0.37 | 2.56 | 5.87 | <3.94 |
LOD (μg mL−1) | LOQ (μg mL−1) | |||||
CSA | 0.29 | 0.88 | ||||
CSB | 1.38 | 4.18 | ||||
CMS | 1.92 | 5.83 |
Temp (°C) | kt (min−1) | t1/2 (0.693/K) (min) |
---|---|---|
20 * | 0.0003 | 2310.00 |
40 ** | 0.0146 | 47.47 |
50 ** | 0.0709 | 9.78 |
60 ** | 0.4485 | 1.55 |
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Dagla, I.; Tsarbopoulos, A.; Gikas, E. Colistimethate Acidic Hydrolysis Revisited: Arrhenius Equation Modeling Using UPLC-QToF MS. Molecules 2021, 26, 447. https://doi.org/10.3390/molecules26020447
Dagla I, Tsarbopoulos A, Gikas E. Colistimethate Acidic Hydrolysis Revisited: Arrhenius Equation Modeling Using UPLC-QToF MS. Molecules. 2021; 26(2):447. https://doi.org/10.3390/molecules26020447
Chicago/Turabian StyleDagla, Ioanna, Anthony Tsarbopoulos, and Evagelos Gikas. 2021. "Colistimethate Acidic Hydrolysis Revisited: Arrhenius Equation Modeling Using UPLC-QToF MS" Molecules 26, no. 2: 447. https://doi.org/10.3390/molecules26020447