A simple and reliable high performance liquid chromatography tandem mass spectrometry (LC-MS/MS) assay for the determination of colistin A and colistin B in human plasma was developed and validated. Clarithromycin was used as an internal standard (IS). Plasma extraction was performed using C-18 cartridges and methanol containing 0.1% formic acid. Analysis was performed using Atlantis dC18 (2.1 × 100 mm, 3 μm) column at room temperature and a mobile phase of 0.2% formic acid in acetonitrile and water (50:50, v:v), delivered at a flow rate of 0.2 ml/minute. Eluent was detected in the positive ion mode using electrospray ionization at the following transitions of mass to charge (m/z): colistin A, 585.6 → 101.4; colistin B, 578.7 → 101.3; and IS, 748.6 → 158.4. No interference by components of blank plasma or commonly used drugs was observed. The relationship between colistin A colistin B concentrations and their corresponding peak height ratios to the IS was linear over the range of 0.05 - 10 μg/ml. Inter-day coefficient of variation and bias were, respectively, ≤11.5% and −3.0 to 6.0 for colistin A and ≤9.9 and −4.7 to 3.0 for colistin B. Mean extraction recovery of colistin A, colistin B, and the IS were 97%, 94%, and 97%, respectively. The method was applied to assess the stability of colistin A and colistin B in processed samples (24 hr. at room temperature, 48 hours at −20°C) and unprocessed samples (24 hr. at room temperature, 8 weeks at −20°C) and after three cycles of freeze and thaw found to be ≥87%.
References
[1]
Ahmed, M.A.E., Zhong, L.L., Shen, C., Yang, Y., Doi, Y. and Tian, G.B. (2020) Colistin and Its Role in the Era of Antibiotic Resistance: An Review (2000-2019). Emerging Microbes & Infections, 9, 868-885.
https://doi.org/10.1080/22221751.2020.1754133
[2]
Bergen, P.J., Li, J., Rayner, C.R. and Nation, R.L. (2006) Colistin Methanesulfonate Is an Inactive Prodrug of Colistin against Pseudomonas aeruginosa. Antimicrobial Agents and Chemotherapy, 50, 1953-1958.
https://pubmed.ncbi.nlm.nih.gov/16723551/
https://doi.org/10.1128/AAC.00035-06
[3]
Decolin, D., Leroy, P., Nicolas, A. and Archimbault, P. (1997) Hyphenated Liquid Chromatographic Method for the Determination of Colistin Residues in Bovine Tissues. Journal of Chromatographic Science, 35, 557-564.
https://pubmed.ncbi.nlm.nih.gov/9397540/
https://doi.org/10.1093/chromsci/35.12.557
[4]
Gregoire, N., Climent, V., Magreault, S., Marchand, S. and Couet, W. (2017) Clinical Pharmacokinetics and Pharmacodynamics of Colistin. Clinical Pharmacokinetics, 56, 1441-1460. https://link.springer.com/article/10.1007/s40262-017-0561-1
https://doi.org/10.1007/s40262-017-0561-1
[5]
Zheng, M., Wang, J., Gerber, J. and Milne, R. (2008) Determination of Colistin in Human Plasma, Urine and Other Biological Samples Using LC-MS/MS. Journal of Chromatography B, 862, 205-212.
https://www.sciencedirect.com/science/article/abs/pii/S1570023207008586
https://doi.org/10.1016/j.jchromb.2007.12.009
[6]
Thomas, A.H. and Holloway, I. (1978) Thin-Layer Chromatographic Method for the Identification of the Polymyxins. Journal of Chromatography A, 161, 417-420.
https://doi.org/10.1016/S0021-9673(01)85266-3
[7]
Holska, W. and Gwozdz, E. (1989) Determination of Colistin by Isotachophoresis. Journal of Liquid Chromatography, 12, 2761-2767.
[8]
Kristensen, H.K. and Hansen, S.H. (1993) Separation of Polymyxins by Micellar Electrokinetic Capillary Chromatography. Journal of Chromatography A, 628, 309-315.
https://www.sciencedirect.com/science/article/abs/pii/002196739380013X
https://doi.org/10.1016/0021-9673(93)80013-X
[9]
Orwa, J.A., Van Gerven, A., Roets, E. and Hoogmartens, J. (2000) Development and Validation of a Liquid Chromatography Method for Analysis of Colistin Sulphate. Chromatographia, 51, 433-436.
https://link.springer.com/article/10.1007/BF02490480
https://doi.org/10.1007/BF02490480
[10]
Li, J., Milne, R.W., Nation, R.L., Turnidge, J.T., Coulthard, K. and Johnson, D.W. (2001) A Simple Method for the Assay of Colistin in Human Plasma, Using Pre-Column Derivatization with 9-Fluorenylmethyl Chloroformate in Solid-Phase Extraction Cartridges and Reversed-Phase High-Performance Liquid Chromatography. Journal of Chromatography B: Biomedical Sciences and Applications, 761, 167-175.
https://pubmed.ncbi.nlm.nih.gov/11587346/
https://doi.org/10.1016/S0378-4347(01)00326-7
[11]
Chepyala, D., Tsai, I.L., Sun, H.Y., Lin, S.W. and Kuo, C.H. (2015) Development and Validation of a High-Performance Liquid Chromatography-Fluorescence Detection Method for the Accurate Quantification of Colistin in Human Plasma. Journal of Chromatography B: Analytical Technologies in the Biomedical and Life Sciences, 980, 48-54. https://europepmc.org/article/med/25589254
https://doi.org/10.1016/j.jchromb.2014.12.015
[12]
Hanai, Y., Matsuo, K., Kosugi, T., Kusano, A., Ohashi, H., Kimura, I., Hirayama, S., Nanjo, Y., Ishii, Y., Sato, T., Miyazaki, T., Nishizawa, K. and Yoshio, T. (2018) Rapid, Simple, and Clinically Applicable High-Performance Liquid Chromatography Method for Clinical Determination of Plasma Colistin Concentrations. Journal of Pharmaceutical Health Care and Sciences, 4, Article No. 22.
https://link.springer.com/article/10.1186/s40780-018-0119-x
https://doi.org/10.1186/s40780-018-0119-x
[13]
Pinho, A.R., Rocha, M., Alves, G., Falcao, A.C. and Fortuna, A.C. (2018) Development and Validation of an HPLC-FLD Technique for Colistin Quantification and Its Plasma Monitoring in Hospitalized Patients. Analytical Methods, 10, 389-396.
https://pubs.rsc.org/en/content/articlelanding/2018/ay/c7ay02585h#!divAbstract
https://doi.org/10.1039/C7AY02585H
[14]
Gobin, P., Lemaitre, F., Marchand, S., Couet, W. and Olivier, J. (2010) Assay of Colistin and Colistin Methanesulfonate in Plasma and Urine by Liquid Chromatography-Tandem Mass Spectrometry. Antimicrobial Agents and Chemotherapy, 54, 1741-1748. https://pubmed.ncbi.nlm.nih.gov/20176909/
https://doi.org/10.1128/AAC.01367-09
[15]
Dorsikas, Y., Markopoulou, C., Koundourellis, J. and Loukas, Y. (2010) Validation of a Novel LC-MS/MS Methods for the Quantification of Colistin A and B in Human Plasma. Journal of Separation Science, 34, 37-45.
https://pubmed.ncbi.nlm.nih.gov/21171174/
https://doi.org/10.1002/jssc.201000680
[16]
Bihan, K., Lu, Q., Enjalbert, M., Apparuit, M., Langeron, O., Rouby, J., Brentano, C. and Zahr, N. (2016) Determination of Colistin and Colistimethate Levels in Humanplasma and Urine by High Performance Liquid Chromatography-Tandem Mass Spectrometry. Therapeutic Drug Monitoring, 38, 796-803.
https://pubmed.ncbi.nlm.nih.gov/27684296/
https://doi.org/10.1097/FTD.0000000000000345
[17]
Leporati, M., Bua, R., Matiano, F., Carignano, P., Stella, M., Biancone, L. and Vincent, M. (2014) Determination by LC-MS/MS of Colistin A and B in Plasma and Ultrafiltrate from Critically Ill Patients Undergoing Continuous Venovenous Hemodiafiltration. Therapeutic Drug Monitoring, 36, 182-191.
https://pubmed.ncbi.nlm.nih.gov/24216535/
https://doi.org/10.1097/FTD.0b013e3182a8997c
[18]
Food and Drug Administration, Centre for Drug Evaluation and Research (CDER) (2018) Bioanalytical Method Validation: Guidance for Industry.
https://www.fda.gov/files/drugs/published/Bioanalytical-Method-Validation-Guidance-for-Industry.pdf
