Development and validation of GLC/FID- and GLC/MS-procedures of secnidazole determination by the methods of additions

Authors

  • O. V. Shovkova National University of Pharmacy, Ukraine
  • L. Yu. Klimenko National University of Pharmacy, Ukraine
  • Z. V. Shovkova National University of Pharmacy, Ukraine
  • M. O. Savchenko National University of Pharmacy, Ukraine

DOI:

https://doi.org/10.24959/ophcj.18.954

Keywords:

secnidazole, gas-liquid chromatography, validation

Abstract

Gas-liquid chromatography is widely used in the process of forensic toxicological examinations, but data about application of GLC with flame-ionization and mass-spectrometry detection for secnidazole determination in analytical toxicology are absent.

Aim. To develop GLC/FID- and GLC/MS-procedures for the quantitative determination of secnidazole and carry out step-by-step validation of the procedures developed in the variant of the method of additions.

Results and discussion. The chromatographic conditions has been chosen for secnidazole determination by the method of GLC in two variants of performance with flame-ionization and mass-spectrometry detection with the temperature program changing during the analysis from 70 °C to 250 °C or 320 °C. Retention times for secnidazole are 8.97 min and 11.74 min. To prove the possibility of application of the procedures proposed in further analysis their validation has been carried out in the variant of the method of additions. Such validation parameters as in-process stability, linearity, accuracy and precision have been estimated by model solutions.

Experimental part. The GLC/FID-analysis: HP 6890 Hewlett Packard; НР-1 ø0.32 mm × 30 m, 0.25 μm; thermostat – 70 ºС (3 min), 40 ºС/min to 180 ºС (2 min), 40 ºС/min to 250 ºС (3 min); injector – 280 ºС; detector – 280 ºС; volume rate of a carrier gas (helium) – 1.5 ml/min; split mode – 1 : 2. The GLC/MS-analysis: Agilent 6890N/5973N/7683; НР-5MS ø0.25 mm × 30 m, 0.25 μm; DB-17MS ø0.25 mm × 30 m, 0.15 μm; columns are connected sequentially through Deans switch; thermostat – 70 ºС (2 min), 45 ºС/min. to 210 ºС, 6 ºС/min to 320 ºС (12.56 min); transfer line – 280 ºС; ion source – 230 ºС; quadrupole – 150 ºС; electron impact – 70eV; 40-750 m/z; injector – 250 ºС; splitless mode; inlet carrier gas (helium) pressure: 1st column – 26.06 psi, 2nd column – 19.30 psi.

Conclusions. New procedures for the quantitative determination of secnidazole by the method of GLC/FID and GLC/MS have been developed. Their validation has been carried out, and acceptability for application has been shown.

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References

  1. Moffat, A. C., Osselton, M. D., Widdop, B. (2011). Clarke’s analysis of drugs and poisons in pharmaceuticals, body fluids and postmortem material. Pharmaceutical Press,London, 4th ed.
  2. Jickells, S., Negrusz, A. (2008). Clarke’s Analytical Forensic Toxicology. Pharmaceutical Press,London,Chicago.
  3. Ashour, S., Kattan, N. (2010). Simultaneous Determination of Miconazole Nitrate and Metronidazole in Different Pharmaceutical Dosage Forms by Gas Chromatography and Flame Ionization Detector (GC-FID). International Journal of Biomedical Science, 6 (1), 13–18.
  4. Wood, N. F. (1975). GLC Analysis of Metronidazole in Human Plasma. Journal of Pharmaceutical Sciences, 64 (6), 1048–1049. https://doi.org/10.1002/jps.2600640642
  5. Midha, K. K., McGilveray, I.J., & Cooper, J. K. (1973). Determination of therapeutic levels of metronidazole in plasma by gas-liquid chromatography. Journal of Chromatography A, 87 (2), 491–497. https://doi.org/10.1016/s0021-9673(01)91751-0
  6. Videau, D., Niel, G., Siboulet, A., Catalan, F. (1978). Secnidazole. A 5-nitroimidazole derivative with a long half-life. British Journal of Venereal Diseases, 54 (2), 77–80. https://doi.org/10.1136/sti.54.2.77
  7. Symonds, J. (1979). Secnidazole – a nitroimidazole with a prolonged serum half-life. Journal of Antimicrobial Chemotherapy, 5 (4), 484–486. https://doi.org/10.1093/jac/5.4.484
  8. Pasupuleti, V., Escobedo, A. A., Deshpande, A., Thota, P., Roman, Y., & Hernandez, A. V. (2014). Efficacy of 5-Nitroimidazoles for the Treatment of Giardiasis: A Systematic Review of Randomized Controlled Trials. PLoS Neglected Tropical Diseases, 8 (3), 2733. https://doi.org/10.1371/journal.pntd.0002733
  9. Thulkar, J., Kriplani, A., & Agarwal, N. (2012). A comparative study of oral single dose of metronidazole, tinidazole, secnidazole and ornidazole in bacterial vaginosis. Indian Journal of Pharmacology, 44 (2), 243. https://doi.org/10.4103/0253-7613.93859
  10. Klymenko, L. Yu. (2015). Kompleksnyi pidkhid do rozrobky ta validatsii metodyk kilkisnoho vyznachennia analitiv u biolohichnykh ridynakh v khimiko-toksykolohichnomu analizi. Doctor’s thesis. Kharkiv: NpaU, 816.
  11. Klimenko, L. Yu. (2014). Determination of linearity, accuracy and precision of UV-spec­trophotometric methods of quantitative determination in forensic and toxicological analysis in the variant of the method of additions. Farmatsyia Kazakhstana, 7 (158), 51–58.
  12. Derzhavne pidpryiemstvo «Ukrainskyi naukovyi ekspertnyi farmakopeinyi tsentr yakosti likarskykh zasobiv». (2015). Derzhavna farmakopeia Ukrainy (Vols 1–3. Vol.1). (2-e ed.) Kharkiv, 1128.
  13. Grizodub, A. I. (2016). Standartizovannye protcedury validatcii metodik kontrolia kachestva lekarstvennykh sredstv. Kharkiv: DP “Ukrainskyi naukovyi farmakopeinyi tsentr yakosti likarskykh zasobiv” 396.
  14. 14. U.S. Department of Health and Human Services, Food and Drug Administration (FDA), Center for Drug Evolution and Research (CDER), Center for Veterinary Medicine (CVM). (2001). Guidance for Industry: Bioanalytical Method Validation.Washington,DC:U.S. Government Printing Office, 22.
  15. Danzer, K., Otto, M., Currie, L. A. (2004). Guidelines for calibration in analytical chemistry. Part 2. Multispecies calibration. Pure and Applied Chemistry, 76 (6), 1215–1225.

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Published

2018-12-14

How to Cite

(1)
Shovkova, O. V.; Klimenko, L. Y.; Shovkova, Z. V.; Savchenko, M. O. Development and Validation of GLC/FID- and GLC/MS-Procedures of Secnidazole Determination by the Methods of Additions. J. Org. Pharm. Chem. 2018, 16, 40-47.

Issue

Vol. 16 No. 4(64) (2018)

Section

Original Researches

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