Research Article


DOI :10.26650/IstanbulJPharm.2022.877867   IUP :10.26650/IstanbulJPharm.2022.877867    Full Text (PDF)

Determination of diazepam in human plasma by developed and validated a high-performance liquid chromatographic ultraviolet method

Emrah DuralBeyza Nur Kaya

Background and Aims: Diazepam is accepted as a safer drug to medicate in many serious cases, acting as an anticonvulsant, an anxiolytic and a treatment for many types of poisoning. Monitoring it is important in achieving successful treatment and reducing the risk of toxic effects. In this study, it is aimed to develop and validate a sensitive, repeatable, and reliable method based on high-performance liquid chromatographic analysis for the determination in human plasma. Methods: Separation was carried out using a reverse-phase C18 column (4.0 mm x 150 mm, 3 μm) at 30 °C. The solution was prepared with a 10 mM phosphate buffer and acetonitrile (1:1, v/v) was employed as a mobile phase at the isocratic flow with 0.5 mL/min rate. Quantification was applied at 230 nm. A solid-phase extraction method was established and optimized, which was then used in the preparation of the plasma (0.5 mL) samples to the analysis. Results: The method was found to be linear (r2 = 0.9805) between 100 and 1200 ng/mL. The analysis run was ≤12 min. Intraday and inter-day accuracy were found between -5.78 and 5.93 and precision was ≤1.82%. The limit of detection and quantification were calculated as 20.42 and 61.86 ng/mL, respectively. Recovery was found between the range of 95.12% and 106.83%. The method was determined to be robust according to changes in UV, mobile phase organic solvent content, mobile phase pH, column temperature, and operator. Conclusion: This simple, sensitive and reliable method is suggested for accredited-reference laboratories working on the therapeutic drug monitorization and/or overdose-toxicological quantified analysis of diazepam in human plasma.


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References

  • Abou-Donia, M. B., Siracuse, B., Gupta, N., & Sobel Sokol, A. (2016). Sarin (GB, O-isopropyl methylphosphonofluoridate) neurotoxic-ity: critical review. Critical Reviews in Toxicology, 46(10), 845-875. https://doi.org/10.1080/10408444.2016.1220916 google scholar
  • Bakavoli, M., & Kaykhaii, M. (2003). Quantitative determination of diazepam, nitrazepam and flunitrazepam in tablets using thin-layer chromatography-densitometry technique. Journal of Phar-maceutical and Biomedical Analysis, 31(6), 1185-1189. https://doi. org/10.1016/S0731-7085(03)00027-X google scholar
  • Bialer, M. (2007). Clinical pharmacology of parenteral use of antiepileptic drugs. 48, 46-48. https://doi.org/10.1111/j.1528-1167.2007.01348.x google scholar
  • Borges, K. B., Freire, E. F., Martins, I., & de Siqueira, M. E. P. B. (2009). Simultaneous determination of multibenzodiazepines by HPLC/ UV: Investigation of liquid-liquid and solid-phase extractions in human plasma. Talanta, 78(1), 233-241. https://doi.org/10.1016/j. talanta.2008.11.003 google scholar
  • Brieudes, V., Lardy-Fontan, S., Lalere, B., Vaslin-Reimann, S., & Budzinski, H. (2016). Validation and uncertainties evaluation of an isotope dilution-SPE-LC-MS/MS for the quantification of drug residues in surface waters. Talanta, 146, 138-147. https://doi. org/10.1016/j.talanta.2015.06.073 google scholar
  • Calcaterra, N. E., & Barrow, J. C. (2014). Classics in chemical neu-roscience: diazepam (valium). ACS Chemical Neuroscience, 5(4), 253-260. https://doi.org/10.1021/cn5000056 google scholar
  • Chamberlain, J. M., Okada, P., Holsti, M., Mahajan, P., Brown, K. M., Vance, C.,... Baren, J. (2014). Lorazepam vs diazepam for pediat-ric status epilepticus: a randomized clinical trial. JAMA, 311(16), 1652-1660. https://doi.org/10.1001/jama.2014.2625 google scholar
  • Cook, P. J., Flanagan, R., & James, I. M. (1984). Diazepam toler-ance: effect of age, regular sedation, and alcohol. British Medical Journal (Clinical Research Ed.), 289(6441), 351-353. https://doi. org/10.1136/bmj.289.6441.351 google scholar
  • de Araujo, F. G., Bauerfeldt, G. F., Marques, M., & Martins, E. M. (2019). Development and validation of an analytical method for the detection and quantification of bromazepam, clonaz-epam and diazepam by UPLC-MS/MS in surface water. Bulletin of Environmental Contamination and Toxicology, 103(2), 362-366. https://doi.org/10.1007/s00128-019-02631-z google scholar
  • Faye, C., Hen, R., Guiard, B. P., Denny, C. A., Gardier, A. M., Mendez-David, I., & David, D. J. (2020). Rapid anxiolytic effects of RS67333, a serotonin type 4 receptor agonist, and diazepam, a benzodi-azepine, are mediated by projections from the prefrontal cortex to the dorsal raphe nucleus. Biological Psychiatry, 87(6), 514-525. https://doi.org/10.1016/j.biopsych.2019.08.009 google scholar
  • Friedman, H., Greenblatt, D. J., Peters, G. R., Metzler, C. M., Charlton, M. D., Harmatz, J. S., ... Francom, S. F. (1992). Pharmacokinetics and pharmacodynamics of oral diazepam: effect of dose, plasma concentration, and time. Clinical Pharmacology and Therapeutics, 52(2), 139-150. https://doi.org/10.1038/clpt.1992.123 google scholar
  • Ghosh, P., Reddy, M. M. K., Ramteke, V. B., & Rao, B. S. (2004). Analysis and quantitation of diazepam in cream biscuits by high-performance thin-layer chromatography and its confirmation by mass spectrometry. Analytica Chimica Acta, 508(1), 31-35. https:// doi.org/10.1016/j.aca.2003.11.058 google scholar
  • Gong, W., Liu, S., Xu, P., Fan, M., & Xue, M. (2015). Simultaneous Quantification of Diazepam and Dexamethasone in Plasma by High-Performance Liquid Chromatography with Tandem Mass Spectrometry and Its Application to a Pharmacokinetic Compari-son between Normoxic and Hypoxic Rats. 6901-6912. https://doi. org/10.3390/molecules20046901 google scholar
  • Herman, R. J., Van Pham, J. D., & Szakacs, C. B. (1989). Disposition of lorazepam in human beings: enterohepatic recirculation and first-pass effect. Clinical Pharmacology and Therapeutics, 46(1), 18-25. https://doi.org/10.1038/clpt.1989.101 google scholar
  • Henney, H. R., 3rd, Sperling, M. R., Rabinowicz, A. L., Bream, G., & Carrazana, E. J. (2014). Assessment of pharmacokinetics and tolerability of intranasal diazepam relative to rectal gel in healthy adults. Epilepsy research, 108(7), 1204-1211. https://doi. org/10.1016/j.eplepsyres.2014.04.007 google scholar
  • Hughes, D. A. (2020). Acute chloroquine poisoning: A compre-hensive experimental toxicology assessment of the role of diaze-pam. British Journal of Pharmacology, 177(21), 4975-4989. https:// doi.org/10.1111/bph.15101 google scholar
  • ICH, I. (2005). Q2 (R1): Validation of analytical procedures: text and methodology. International Conference on Harmonization, Geneva. google scholar
  • Kim, D. H., Cho, J. Y., Chae, S. I., Kang, B. K., An, T. G., Shim, W. S., . Lee, K. T. (2017). Development of a simple and sensitive HPLC-MS/MS method for determination of diazepam in human plasma and its application to a bioequivalence study. Translational and Clinical Pharmacology, 25(4), 173-178. https://doi.org/10.12793/ tcp.2017.25.4.173 google scholar
  • McGrath, M., Hoyt, H., Pence, A., Jayakar, S. S., Zhou, X., Forman, S. A., . Raines, D. E. (2020). Competitive Antagonism of Etomidate Action by Diazepam. Anesthesiology, 133(3), 583-594. https://doi. org/10.1097/ALN.0000000000003403 google scholar
  • Mercolini, L., Mandrioli, R., Amore, M., & Raggi, M. A. (2008). Sepa-ration and HPLC analysis of 15 benzodiazepines in human plas-ma. Journal of Separation Science, 31(14), 2619-2626. https://doi. org/10.1002/jssc.200800212 google scholar
  • Mercolini, L., Mandrioli, R., Iannello, C., Matrisciano, F., Nicoletti, F., & Raggi, M. A. (2009). Simultaneous analysis of diazepam and its metabolites in rat plasma and brain tissue by HPLC-UV and SPE. Ta-lanta, 80(1), 279-285. https://doi.org/10.1016/j.talanta.2009.06.074 google scholar
  • Miller, E. I., Wylie, F. M., & Oliver, J. S. (2008). Simultaneous detec-tion and quantification of amphetamines, diazepam and its me-tabolites, cocaine and its metabolites, and opiates in hair by LC-ESI-MS-MS using a single extraction method. Journal of Analytical Toxicology, 32(7), 457-469. https://doi.org/10.1093/jat/32.7.457 google scholar
  • Montoro, J., Bartra, J., Sastre, J., Davila, I., Ferrer, M., Mullol, J.,... Vale-ro, A. (2013). H-1 antihistamines and benzodiazepines. Pharmaco-logical interaction and their impact on cerebral function. Journal of Investigational Allergology & Clinical Immunology: Official Organ of the International Association of Asthmology (INTERASMA) and Socie-dad Latinoamericana de Alergia e Inmunologia, 23, 17-26. google scholar
  • Morelli, B. (1997). Determination of diazepam and otilonium bromide in pharmaceuticals by ratio-spectra derivative spec-trophotometry. Fresenius’ Journal of Analytical Chemistry, 357(8), 1179-1184. https://doi.org/10.1007/s002160050327 google scholar
  • Muchohi, S. N., Ogutu, B. R., Newton, C. R. J. C., & Kokwaro, G. O. (2001). High-performance liquid chromatographic determination of diazepam in plasma of children with severe malaria. Jour-nal of Chromatography B: Biomedical Sciences and Applications, 761(2), 255-259. https://doi.org/10.1016/S0378-4347(01)00284-5 Perry, P. J., Stambaugh, R. L., Tsuang, M. T., & Smith, R. E. (1981). Sed-ative-hypnotic tolerance testing and withdrawal comparing diaz-epam to barbiturates. Journal of Clinical Psychopharmacology, 1(5), 289-296. https://doi.org/10.1097/00004714-198109000-00004 Pilli, N., Narayanasamy, S., Xu, L., Chockalingam, A., Shea, K., Stew-art, S., . Matta, M. (2020). A high-throughput bioanalytical as-say to support pharmacokinetic interaction study of oxycodone and diazepam in Sprague Dawley rats. RSC Advances, 10, 886-896. https://doi.org/10.1039/C9RA05785D google scholar
  • Qin, X., Xie, H., Wang, W., He, N., Huang, S., Xu, Z., . Zhou, H. (1999). Effect of the gene dosage of on diazepam metabolism in Chinese subjects. Clinical Pharmacology & Therapeutics, 66(6), 642-646. https://doi.org/10.1053/cp.1999.v66.103379001">https://doi.org/10.1053/cp.1999.v66.103379001 Richards, B. L., Whittle, S. L., & Buchbinder, R. (2012). Muscle re-laxants for pain management in rheumatoid arthritis. The Co-chrane Database of Systematic Reviews, 1, CD008922. https://doi. org/10.1002/14651858.CD008922.pub2 google scholar
  • Rogers, J. J., Stanford, C., & Dart, R. C. (2006, March). The use of visual analog pain scales in black widow spider envenomation. Journal of Medical Toxicology, 2(1), 46-47. https://doi.org/10.1007/BF03161013 Taysse, L., Cal, J., Bue, J., Christin, D., Delamanche, S., & Breton, P. (2003). Comparative efficacy of diazepam and avizafone against sarin-induced neuropathology and respiratory failure in guinea pigs : influence of atropine dose. Toxicology, 188(2-3), 197-209. https://doi.org/10.1016/S0300-483X(03)00086-6 google scholar
  • Tran, N. H., Hu, J., & Ong, S. L. (2013). Simultaneous determination of PPCPs, EDCs, and artificial sweeteners in environmental water samples using a single-step SPE coupled with HPLC-MS/MS and isotope dilution. Talanta, 113, 82-92. https://doi.org/10.1016/j. talanta.2013.03.072 google scholar
  • Uddin, M. N., Samanidou, V. F., & Papadoyannis, I. N. (2008). Validation of SPE-HPLC determination of 1,4-benzodiazepines and metabolites in blood plasma, urine, and saliva. Journal of Separation Science, 31(21), 3704-3717. https://doi.org/10.1002/ jssc.200800342 google scholar
  • Weintraub, S. J. (2017). Diazepam in the treatment of moderate to severe alcohol withdrawal. CNS Drugs, 31(2), 87-95. https://doi. org/10.1007/s40263-016-0403-y google scholar
  • Wexler, P., Peyster, A. De, Hakkinen, P. J., & Pope, C. (2005). Encyclo-pedia of toxicology. 2944,(783-784). google scholar
  • Yasui, M., Kato, A., Kanemasa, T., Murata, S., Nishitomi, K., Koike, . Abe, K. (2005). Pharmacological profiles of benzodiazepiner-gic hypnotics and correlations with receptor subtypes. Japanese Journal of Psychopharmacology, 25(3), 143-151. google scholar
  • Yuan, H., & Pawliszyn, J. (2001). Application of solid-phase micro-extraction in the determination of diazepam binding to human serum albumin. Analytical Chemistry, 73(18), 4410-4416. https:// doi.org/10.1021/ac010227s google scholar
  • Zanette, G., Manani, G., Favero, L., Stellini, E., Mazzoleni, S., Co-cilovo, F., . Facco, E. (2013). Conscious sedation with diazepam and midazolam for dental patient: priority to diazepam. Minerva Stomatologica, 62(10), 355-374. google scholar
  • Zendelovska, D., Pavlovska, K., Atanasovska, E., Gjorgjievska, K., & Petrusevska, M. (2018). High performance liquid chromatograph-ic method for direct determination of diazepam in whole blood and serum - optimization of solid-phase extraction method. Prilozi, 38(3), 89-96. https://doi.org/10.2478/prilozi-2018-0009. google scholar
  • Zhang, Y., Ouyang, K., Lipina, T. V, Wang, H., & Zhou, Q. (2019). Con-ditioned stimulus presentations alter anxiety level in fear-condi-tioned mice. Molecular Brain, 12(1), 28. https://doi.org/10.1186/ s13041-019-0445-4. google scholar

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APA

Dural, E., & Kaya, B.N. (2022). Determination of diazepam in human plasma by developed and validated a high-performance liquid chromatographic ultraviolet method. İstanbul Journal of Pharmacy, 52(1), 37-46. https://doi.org/10.26650/IstanbulJPharm.2022.877867


AMA

Dural E, Kaya B N. Determination of diazepam in human plasma by developed and validated a high-performance liquid chromatographic ultraviolet method. İstanbul Journal of Pharmacy. 2022;52(1):37-46. https://doi.org/10.26650/IstanbulJPharm.2022.877867


ABNT

Dural, E.; Kaya, B.N. Determination of diazepam in human plasma by developed and validated a high-performance liquid chromatographic ultraviolet method. İstanbul Journal of Pharmacy, [Publisher Location], v. 52, n. 1, p. 37-46, 2022.


Chicago: Author-Date Style

Dural, Emrah, and Beyza Nur Kaya. 2022. “Determination of diazepam in human plasma by developed and validated a high-performance liquid chromatographic ultraviolet method.” İstanbul Journal of Pharmacy 52, no. 1: 37-46. https://doi.org/10.26650/IstanbulJPharm.2022.877867


Chicago: Humanities Style

Dural, Emrah, and Beyza Nur Kaya. Determination of diazepam in human plasma by developed and validated a high-performance liquid chromatographic ultraviolet method.” İstanbul Journal of Pharmacy 52, no. 1 (Sep. 2022): 37-46. https://doi.org/10.26650/IstanbulJPharm.2022.877867


Harvard: Australian Style

Dural, E & Kaya, BN 2022, 'Determination of diazepam in human plasma by developed and validated a high-performance liquid chromatographic ultraviolet method', İstanbul Journal of Pharmacy, vol. 52, no. 1, pp. 37-46, viewed 26 Sep. 2022, https://doi.org/10.26650/IstanbulJPharm.2022.877867


Harvard: Author-Date Style

Dural, E. and Kaya, B.N. (2022) ‘Determination of diazepam in human plasma by developed and validated a high-performance liquid chromatographic ultraviolet method’, İstanbul Journal of Pharmacy, 52(1), pp. 37-46. https://doi.org/10.26650/IstanbulJPharm.2022.877867 (26 Sep. 2022).


MLA

Dural, Emrah, and Beyza Nur Kaya. Determination of diazepam in human plasma by developed and validated a high-performance liquid chromatographic ultraviolet method.” İstanbul Journal of Pharmacy, vol. 52, no. 1, 2022, pp. 37-46. [Database Container], https://doi.org/10.26650/IstanbulJPharm.2022.877867


Vancouver

Dural E, Kaya BN. Determination of diazepam in human plasma by developed and validated a high-performance liquid chromatographic ultraviolet method. İstanbul Journal of Pharmacy [Internet]. 26 Sep. 2022 [cited 26 Sep. 2022];52(1):37-46. Available from: https://doi.org/10.26650/IstanbulJPharm.2022.877867 doi: 10.26650/IstanbulJPharm.2022.877867


ISNAD

Dural, Emrah - Kaya, BeyzaNur. Determination of diazepam in human plasma by developed and validated a high-performance liquid chromatographic ultraviolet method”. İstanbul Journal of Pharmacy 52/1 (Sep. 2022): 37-46. https://doi.org/10.26650/IstanbulJPharm.2022.877867



TIMELINE


Submitted10.02.2021
Accepted17.02.2022
Published Online28.04.2022

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