New procedures of Metronidazole determination by the method of Gas-Liquid Chromatography

Lina Yu. Klimenko; Galyna L. Shkarlat; Zoia V. Shovkova; Sergii V. Kolisnyk; Olga I. Nazarko

doi:10.5958/0974-360X.2020.00213.9

Research Journal of Pharmacy and Technology

ISSN

0974-360X (Online)
0974-3618 (Print)

Submit Article

New procedures of Metronidazole determination by the method of Gas-Liquid Chromatography

Author(s): Lina Yu. Klimenko, Galyna L. Shkarlat, Zoia V. Shovkova, Sergii V. Kolisnyk, Olga I. Nazarko

Email(s): lina_klimenko@nuph.edu.ua

DOI: 10.5958/0974-360X.2020.00213.9

Address: Lina Yu. Klimenko1*, Galyna L. Shkarlat1, Zoia V. Shovkova2, Sergii V. Kolisnyk1, Olga I. Nazarko3
1Analytical Chemistry Department, National University of Pharmacy, Kharkiv, Ukraine.
2Drug and Analytical Toxicology Department, National University of Pharmacy, Kharkiv, Ukraine.
3Inorganic Chemistry Department, National University of Pharmacy, Kharkiv, Ukraine.
*Corresponding Author

Published In: Volume - 13, Issue - 3, Year - 2020

View HTML

View PDF

ABSTRACT:
Metronidazole is the most popular representative in the group of medicines of 5-nitroimidazole derivatives. Based on the information about metronidazole side effects and its interaction with alcohol it is a potential analyte in forensic toxicology. The purpose is to develop GLC-procedures of metronidazole quantification and carry out their step-by-step validation to choose the optimal variant for further application in analytical toxicology. The chromatographic conditions has been chosen for metronidazole determination by the method of gas-liquid chromatography in two variants of performance with flame-ionization and mass-spectrometry detection with temperature program changing during the analysis from 70°C to 250°C or 320°C respectively. The GLC/FID-analyses were performed using gas chromatograph HP 6890 Hewlett Packard; column – ??-1 ?0.32mm ? 30 m, 0.25µm, 100% dimethylpolysiloxane. The GLC/MSD-analyses were performed using Agilent 6890N Gas Chromatograph; columns – 1) ??-5MS ?0.25mm ? 30m, 0.25µm, 5% diphenylpolysiloxan/95% dimethylpolysiloxan; 2) DB-17MS ?0.25mm ? 30m, 0.15µm, 50% diphenylpolysiloxan/50% dimethylpolysiloxan; columns are connected sequentially through Deans switch. Under proposed conditions metronidazole and four other 5-nitroimidazole derivatives (tinidazole, ornidazole, secnidazole, nimorazole) are separated and detected without preliminary derivatization. In the method of GLC/FID the retention time for metronidazole is 9.08 min, in the method of GLC/MSD – 12.01 min. New GLC-procedures of metronidazole quantitative determination under proposed conditions have been developed. Their validation by such parameters as stability, linearity, accuracy and precision in the variants of the method of calibration curve, method of standard and method of additions has been carried out and acceptability for application has been shown.

Keywords:

Cite this article:
Lina Yu. Klimenko, Galyna L. Shkarlat, Zoia V. Shovkova, Sergii V. Kolisnyk, Olga I. Nazarko. New procedures of Metronidazole determination by the method of Gas-Liquid Chromatography. Research J. Pharm. and Tech 2020; 13(3): 1157-1166. doi: 10.5958/0974-360X.2020.00213.9

Cite(Electronic):
Lina Yu. Klimenko, Galyna L. Shkarlat, Zoia V. Shovkova, Sergii V. Kolisnyk, Olga I. Nazarko. New procedures of Metronidazole determination by the method of Gas-Liquid Chromatography. Research J. Pharm. and Tech 2020; 13(3): 1157-1166. doi: 10.5958/0974-360X.2020.00213.9 Available on: https://rjptonline.org/AbstractView.aspx?PID=2020-13-3-18

REFERENCES:

1. Brook I. Spectrum and treatment of anaerobic infections. Journal of Infection and Chemotherapy. 2016; 22(1): 1–13.

2. Abbas HA. Inhibition of virulence of Pseudomonas aeruginosa: a novel role of metronidazole against aerobic bacteria. Research Journal of Pharmacy and Technology. 2015; 8(12): 1640–1644.

3. Selvakumar S, Ravichandran S, Matsyagiri L. Development and validation of analytical method for simultaneous estimation of ornidazole and cefixime trihydrate tablet dosage forms by UV spectroscopy. Asian Journal of Pharmaceutical Analysis. 2016; 6(4): 246–252.

4. Rege PV, Sathe PA, Salvi VS. Simultaneous spectrophotometric estimation of norfloxacin and tinidazole from combined tablet dosage form. Asian Journal of Research in Chemistry. 2011; 4(5): 729–733.

5. Carolin Nimila I, Balan P, Sathiya Sundar R, Ashok Kumar J, Rajasekar S. Simultaneous RP-HPLC estimation of ciprofloxacin hydrochloride and ornidazole in tablet dosage form. Asian Journal of Research in Chemistry. 2011; 4(2): 227–230.

6. Kabra P, Kimbahune R. Validated liquid chromatographic method for simultaneous estimation of ofloxacin, ornidazole and its isomer in bulk and tablet dosage form. Asian Journal of Research in Chemistry. 2010; 3(3): 666–668.

7. Venkatachalam T, Narendiran S, Kalai Selvi P, Dheen Kumar P. RP-HPLC method for simultaneous determination of ofloxacin and satranidazole in tablet dosage form. Asian Journal of Research in Chemistry. 2009; 2(4): 469–471.

8. Aaraf TH, Raj HA, Jain VC, Sutariya V Development and validation of ratio derivative spectrophotometric method for estimation of metronidazole benzoate and related impurity in bulk and pharmaceutical formulation. Asian Journal of Pharmacy and Technology. 2015; 5(2): 66–70.

9. Lamp KC, Freeman CD, Klutman NE, Lacy MK. Pharmacokinetics and pharmacodynamics of the nitroimidazole antimicrobials. Clinical Pharmacokinetics. 1999; 36(5): 353–373.

10. Kuriyama A, Jackson JL, Doi A, Kamiya T. Metronidazole-induced central nervous system toxicity: a systematic review. Clinical Neuropharmacology. 2011; 34(6): 241–247.

11. Edwards DI. Mechanisms of selective toxicity of metronidazole and other nitroimidazole drugs. British Journal of Venereal Diseases. 1980; 56(5): 285–290.

12. Moreno SN, Docampo R. Mechanism of toxicity of nitrocompounds used in the chemotherapy of trichomoniasis. Environmental Health Perspectives. 1985; 64: 199–208.

13. Noureldin M, Krause J, Jin L, Ng V, Tran M. Drug-alcohol interactions: a review of three therapeutic classes. U.S. Pharmacist. 2010; 35(11): 29–40.

14. Fjeld H, Raknes G. [Is combining metronidazole and alcohol really hazardous?]. Tidsskrift for Den norske legeforening. 2014; 134(17): 1661–1663. [Article in Norwegian]

15. Cina SJ, Russell RA, Conradi SE. Sudden death due to metronidazole – ethanol interaction. American Journal of Forensic Medicine and Pathology. 1996; 17: 343–346.

16. Shkarlat GL, Zhuravel IO, Klimenko LYu, Shovkova ZV. Development and validation of UV-spectrophotometric methods of metronidazole quantitative determination for purposes of forensic and toxicological analysis. Ukrains’kyi medychnyi al’manakh. 2014; 17(1): 61–67 [in Russian].

17. Klimenko LYu, Shkarlat GL, Shovkova ZV, Yaremenko VD, Shpychak OS. Development and validation of HPLC/UV-spectrophotometric procedures for metronidazole quantitative determination. International Journal of Pharmaceutical Quality Assurance. 2018; 9(3): 291–299.

18. Shkarlat GL, Klimenko LYu, Shovkova ZV, Havrysh NВ, Lebedynets VO. Modelling the processes of sample preparation of biological objects for the subsequent determination of metronidazole. Journal of Pharmaceutical Sciences and Research. 2018; 10(3): 474–480.

19. Moffat AC, Osselton MD, Widdop B. Clarke’s analysis of drugs and poisons in pharmaceuticals, body fluids and postmortem material, Pharmaceutical Press, London. 2011, 4th ed.

20. Jickells S, Negrusz A. Clarke’s analytical forensic toxicology, Pharmaceutical Press, London, Chicago. 2008.

21. Ashour S., Kattan N. 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. 2010; 6(1): 13–18.

22. Wood NF. GLC analysis of metronidazole in human plasma. Journal of Pharmaceutical Sciences. 1975; 64(6): 1048–1049.

23. Midha KK, McGilveray IJ, Cooper JK. Determination of therapeutic levels of metronidazole in plasma by gas-liquid chromatography. Journal of Chromatography A. 1973; 87(2): 491–497.

24. Polzer J, Gowik P. Validation of a method for the detection and confirmation of nitroimidazoles and corresponding hydroxy metabolites in turkey and swine muscle by means of gas chromatography–negative ion chemical ionization mass spectrometry. Journal of Chromatography B: Biomedical Sciences and Applications. 2001; 761(1): 47–60.

25. Bhatia SC, Shanbhag VD. Electron-capture gas chromatographic assays of 5-nitroimidazole class of antimicrobials in blood. Journal of Chromatography B: Biomedical Sciences and Applications. 1984; 305: 325–334

26. Wang JH. Determination of three nitroimidazole residues in poultry meat by gas chromatography with nitrogen–phosphorus detection. Journal of Chromatography A. 2001; 918(2): 435–438.

27. Kadam AS, Pimpodkar NV, Gaikwad PS, Chavan SD. Bioanalytical method validation. Asian Journal of Pharmaceutical Analysis. 2015; 5(4): 219–225.

28. Saudagar RB, Thete PG. Bioanalytical method validation: a concise review. Asian Journal of Research in Pharmaceutical Sciences. 2018; 8(2): 107–114.

29. Mujoriya RZ. Analytical method development and validation of pharmaceutical technology: an overview. Research Journal of Pharmaceutical Dosage Forms and Technology. 2013; 5(4): 213–220.

30. Klimenko LYu, Petyunin GP. Development of approaches to validation of UV-spectrophotometric methods of quantitative determination in forensic and toxicological analysis: linearity and application range. Farmatsevtychnyi chasopys. 2014; 2(30): 46–51.

31. Klimenko LYu, Petyunin GP, Trut SM, Moroz VP. [Acceptability criteria for linear dependence when validating UV-spectrophotometric methods of quantitative determination in forensic and toxicological analysis]. Current issues in pharmacy and medicine: science and practice. 2014; 2(15): 15–22 [Article in Russian].

32. Klimenko LYu, Trut SM, Petyunin GP, Kostina TA. Determining accuracy in validation of UV-spectrophotometric methods of quantitative measurement in forensic toxicological analysis. Ukrainian Biopharmaceutical Journal. 2014; 2(31): 55–67.

33. Klimenko LYu, Trut SM, Mykytenko OYe. Approaches to determination of precision for UV-spectrophotometric methods of quantitative determination in forensic and toxicological analysis. Farmatsyia Kazakhstana. 2014; 3(154): 44–48.

34. Klimenko LYu. [Development of approaches to determination of linearity, accuracy and precision of UV-spectrophotometric methods of quantitative determination by the method of standard in forensic and toxicological analysis]. Farmatsyia Kazakhstana. 2014; 4(155): 31–35 [Article in Russian].

35. Klimenko LYu. 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. 2014; 7(158): 51–58.

36. Shovkova OV, Klimenko LYu, Kovalenko SM, Zhukova TV. Development and validation of UV-spectrophotometric procedures for secnidazole quantitative determination. Journal of Pharmaceutical Sciences and Research. 2017; 9(4): 338–348.

37. Shovkova OV, Klimenko LYu, Shovkova ZV, Lebedynets VO, Bohomol NP. Study of secnidazole extraction from aqueous solutions. Journal of Pharmaceutical Sciences and Research. 2018; 10(8): 2056–2064.

38. Shovkova OV, Klimenko LYu, Shovkova ZV, Kostina TA. Development and validation of HPLC/UV-procedure of secnidazole determination. Journal of Organic and Pharmaceutical Chemistry. 2018; 16(63): 30–38.

39. Shovkova OV, Klimenko LYu, Shovkova ZV, Savchenko MO. Development and validation of GLC/FID- and GLC/MS-procedures of secnidazole determination by the method of additions. Journal of Organic and Pharmaceutical Chemistry. 2018; 16(64): 40–47.

40. Shovkova OV, Klimenko LYu, Shovkova ZV, Ulanova VA, Shpychak OS. Application of thin layer chromatography in analysis of secnidazole, ornidazole, tinidazole and nimorazole. Journal of Pharmaceutical Sciences and Research. 2018; 10(12): 3411–3416.

41. Slabiak OI, Ivanchuk IM, Klimenko LYu, Lebedynets VO, Yaremenko VD. Development and validation of HPLC/UV-procedure for efavirenz quantitative determination. Journal of Pharmaceutical Sciences and Research. 2018; 10(11): 2829–2835.

42. Gryzodub OI. Standardized validation procedures for methods of medicines quality control, SE «Ukrainian Scientific Pharmacopoeial Center for Quality of Medicines», Kharkiv. 2016.

43. Guidance for the validation of analytical methodology and calibration of equipment used for testing of illicit drugs in seized materials and biological specimens, United Nations Office on Drugs and Crime, Laboratory and Scientific Section, New York. 2009.