Determination of nikethamide by micellar electrokinetic chromatography.
MEKC
drugs
nikethamide
urine
Journal
Biomedical chromatography : BMC
ISSN: 1099-0801
Titre abrégé: Biomed Chromatogr
Pays: England
ID NLM: 8610241
Informations de publication
Date de publication:
Oct 2019
Oct 2019
Historique:
received:
11
11
2018
revised:
15
04
2019
accepted:
30
04
2019
pubmed:
8
5
2019
medline:
22
1
2020
entrez:
8
5
2019
Statut:
ppublish
Résumé
A simple, fast, sensitive and reproducible micellar electrokinetic chromatography (MEKC)-UV method for the determination of nikethamide (NKD) in human urine and pharmaceutical formulation has been developed and validated. The method exhibits high trueness, good precision, short analysis time and low reagent consumption. NKD is an organic compound belonging to the psychoactive stimulants used as an analeptic drugs. The proposed analytical procedure consists of few steps: dilution of urine or drug in distilled water, centrifugation for 2 min (12,000g), separation by MEKC and ultraviolet-absorbance detection of NKD at 260 nm. The background electrolyte used was 0.035 mol/L pH 9 borate buffer with the addition of 0.05 mol/L sodium dodecyl sulfate and 6.5% ACN. Effective separation was achieved within 5.5 min under a voltage of 21 kV (~90 μA) using a standard fused-silica capillary (effective length 51 cm, 75 μm i.d.). The determined limit of detection for NKD in urine was 1 μmol/L (0.18 μg/mL). The calibration curve obtained for NKD in urine showed linearity in the range 4-280 μmol/L (0.71-49.90 μg/mL), with R
Substances chimiques
Nikethamide
368IVD6M32
Types de publication
Journal Article
Langues
eng
Sous-ensembles de citation
IM
Pagination
e4571Informations de copyright
© 2019 John Wiley & Sons, Ltd.
Références
Belfroid, A. C., Van der Horst, A., Vethaak, A. D., Schafer, A. J., Rijs, G. B. J., Wegener, J., & Cofino, W. P. (1999). Analysis and occurrence of estrogenic hormones and their glucuronides in surface water and waste water in The Netherlands. Science of the Total Environment, 225, 101-108. https://doi.org/10.1016/S0048-9697(98)00336-2
Bessonneau, V., Boyaci, E., Maciazek-Jurczyk, M., & Pawliszyn, J. (2015). In vivo solid phase microextraction sampling of human saliva for non-invasive and on-site monitoring. Analytica Chimica Acta, 856, 35-45. https://doi.org/10.1016/j.aca.2014.11.029
Carmichael, W. M. (1971). The determination of nikethamide and other compounds in pharmaceutical dosage forms by thin-layer chromatography. Analyst, 96, 716-720. https://doi.org/10.1039/an9719600716
Chen, L., Liao, L., Zuo, Z., Yan, Y., Yang, L., Fu, Q., … Hou, J. (2007). Simultaneous determination of nikethamide and lidocaine in human blood and cerebrospinal fluid by high performance liquid chromatography. Journal of Pharmaceutical and Biomedical Analysis, 43, 1757-1762. https://doi.org/10.1016/j.jpba.2006.12.015
Delbeke, F. T., & Debackere, M. (1976). Excretion and metabolism of nikethamide in the horse. British Journal of Sports Medicine, 10, 116-123. https://doi.org/10.1136/bjsm.10.3.116
Hsu, K. F., Chien, K.-Y., Chang-Chien, G. P., Lin, S. F., Hsu, P. H., & Hsu, M.-C. (2011). Liquid chromatography-tandem mass spectrometry screening method for the simultaneous detection of stimulants and diuretics in urine. Journal of Analytical Toxicology, 35, 665-674. https://doi.org/10.1093/anatox/35.9.665
Kubalczyk, P., & Bald, E. (2013). Micellar electrokinetic chromatography. In B. Buszewski, E. Dziubakiewicz, & M. Szumski (Eds.), Electromigration techniques. Springer Series in Chemical Physics 105, 77-92. Berlin: Springer. https://doi.org/10.1007/978-3-642-35043-6_5
Leung, G. N. W., Tang, H. P. O., Tso, T. S. C., & Wan, T. S. M. (1996). Separation of basic drugs with non-aqueous capillary electrophoresis. Journal of Chromatography a, 738, 141-154. https://doi.org/10.1016/0021-9673(96)00061-1
Lewis, J. H. (1979). Determination of nikethamide and N-ethylnicotinamide in the blood and urine of greyhounds. Journal of Chromatography, 172, 295-302. https://doi.org/10.1016/S0021-9673(00)90965-8
Lide, D. R. (Ed.) (2009). Handbook of chemistry and physics (90th ed.). Boca Raton, FL: CRC Press.
Lu, J., Wang, S., Dong, Y., Wang, X., Yang, S., Zhang, J., … Ouyang, G. (2010). Simultaneous analysis of fourteen tertiary amine stimulants in human urine for doping control purposes by liquid chromatography-tandem mass spectrometry and gas chromatography-mass spectrometry. Anaytica Chimica Acta, 657, 45-52. https://doi.org/10.1016/j.aca.2009.10.016
Mirnaghi, F. S., Goryński, K., Rodriguez-Lafuente, A., Boyaci, E., Bojko, B., & Pawliszyn, J. (2013). Microextraction versus exhaustive extraction approaches for simultaneous analysis of compounds in wide range of polarity. Journal of Chromatography a, 1316, 37-43. https://doi.org/10.1016/j.chroma.2013.09.084
Pleuvry, B. J. (2006). CNS stimulants: Basic pharmacology and relevance to anaesthesia. Anaesthesia and Intensive Care Medicine, 7, 60-62. https://doi.org/10.1383/anes.2006.7.2.60
Terabe, S. (2004). Micellar electrokinetic chromatography. Analytical Chemistry, 76, 241-246.
Thomas, A., Geyer, H., Schänzer, W., Crone, C., Kellmann, M., Moehring, T., & Thevis, M. (2012). Sensitive determination of prohibited drugs in dried blood spots (DBS) for doping controls by means of a benchtop quadrupole/Orbitrap mass spectrometer. Analytical and Bioanalytical Chemistry, 403, 1279-1289. https://doi.org/10.1007/s00216-011-5655-2
US FDA (2018). Bioanalytical method validation. Guidance for industry. Rockville, MD: US Department of Health and Human Services Food and Drug Administration.
Wang, X.-Q., Xiang, Z., Yu, X.-M., Wu, J.-Z., Lin, D., & Ye, F.-Q. (2009). LC-MS-MS Determination of nikethamide in human plasma. Chromatographia, 69, 1067-1071. https://doi.org/10.1365/s10337-009-1041-z
World Anti-Doping Agency Prohibited List (January 2017). https://www.wada-ama.org/sites/default/files/resources/files/2016-09-29_-_wada_prohibited_list_2017_eng_final.pdf