LC-MS/MS METHOD DEVELOPMENT AND VALIDATION FOR THE DETERMINATION OF CARDIAZOL IN HUMAN PLASMA

IRYNA DRAPAK; BORYS ZIMENKOVSKY; LINA PEREKHODA; SERGIY KOVALENKO; Liliya Logoyda

doi:10.22159/ijap.2019v11i4.33482

Authors

IRYNA DRAPAK General, Bioinorganic, Physical and Colloidal Chemistry Department, Danylo Halytsky Lviv National Medical University, Lviv City, Ukraine
BORYS ZIMENKOVSKY Pharmaceutical, Organic and Bioorganic Chemistry Department, Danylo Halytsky Lviv National Medical University, Lviv City, Ukraine
LINA PEREKHODA Medicinal Chemistry Department, National University of Pharmacy, Kharkiv City, Ukraine
SERGIY KOVALENKO Organic and Bioorganic Chemistry Department, Zaporizhzhya State Medical University, Zaporizhzhya City, Ukraine
Liliya Logoyda Pharmaceutical Chemistry Department, Pharmaceutical Faculty, I. Horbachevsky Ternopil State Medical University, Ternopil City, Ukraine

DOI:

https://doi.org/10.22159/ijap.2019v11i4.33482

Keywords:

LC-MSMS, Cardiazol, Human plasma, Validation, Pharmacokinetic studies

Abstract

Objective: The main purpose of this study was to develop a simple, precise, rapid and accurate method for the quantification of cardiazol in human plasma.

Methods: Chromatography was achieved on Discovery C18, 50 × 2.1 mm, 5 μm column. Samples were chromatographed in a gradient mode (eluent A (acetonitrile-water–formic acid, 5: 95: 0.1 v/v), eluent B (acetonitrile–formic acid, 100: 0.1 v/v)). The initial content of the eluent B of 8%, which increases linearly to 1.0 min to 100%, is maintained up to 1.5 min and returned to the original 8% to 1.51 min. The mobile phase was delivered at a flow rate of 0.400 ml/min into the mass spectrometer ESI chamber. The sample volume was 300 μl.

Results: The total chromatographic run time was 2.5 min and the elution of cardiazol and IS (difenoconazole) occurred at ~2.15 and 1.98 min, respectively. A linear response function was established at 1-100 ng/ml for cardiazol and difenoconazole in human plasma. The % mean recovery for cardiazol in LQC, MQC and HQC was 102.8 %, 100.3 % and 95.9 %. The lowest concentration with the RSD<20% was taken as LLOQ and was found to be 1.10 ng/ml for cardiazol. The % accuracy of LLOQ samples prepared with the different biological matrix lots was found 109.7 %, which were found within the range of 80.00-120.00 % for the seven different plasma lots. % CV for LLOQ samples was observed as 11.9 %, which are within 20.00% of the acceptance criteria.

The within-run coefficients of variation ranged between 0.311 % and 0.601 % for cardiazol. The within-run percentages of nominal concentrations ranged between 99.80 % and 100.41 % for cardiazol. The between-run coefficients of variation ranged between 0.332 % and 0.615 % for cardiazol. The between-run percentages of nominal concentrations ranged between 98.18 % and 101.21 % for cardiazol.

Conclusion: A rapid method was developed for simultaneous determination of cardiazol in human plasma. The method was strictly validated according to the ICH guidelines. Acquired results demonstrate that the proposed strategy can be effortlessly and advantageously applied for routine examination of cardiazol in human plasma.

Downloads

Download data is not yet available.

References

https://www.omicsonline.org. [Last accessed on 01 May 2019]

Perekhoda LO, Drapak IV, Suleiman MM, Sych IA, Yaremenko VD. Synthesis and in silico research of derivatives of 3-allyl-4-(R-phenyl)-N-(R1-phenyl)thiazole-2-imine. Der Pharma Chemica 2017;9:95-8.

Guideline on Bioanalytical method validation: European Medicines Agencies; 2011.

Sonawane LV, Poul BN, Usnale SV. Bioanalytical method validation and its pharmaceutical application a review. Pharm Anal Acta 2014;5:1-7.

Pushpa Latha E, Sailaja B. Bioanalytical method development and validation by HPLC: a review. J Appl Pharm 2014;1:1-9.

Liliya Logoyda. Bioanalytical method development and validation from the simultaneous determination of verapamil and enalapril in the present of enalaprilat by HPLC MS/MS. Int J Appl Pharm 2018;10:19-27.

Liliya Logoyda. A HPLC-MS/MS method development and validation for the simultaneous determination of nifedipine and enalapril in human plasma. Int J Appl Pharm 2018;10:35-42.

Ghosh C, Jain I, Shinde CP, Chakraborty BS. Rapid and sensitive liquid chromatography/tandem mass spectrometry method for simultaneous determination of enalapril and its major metabolite enalaprilat, in human plasma: application to a bioequivalence study. Drug Testing Anal 2012;4:94–103.

Logoyda L, Kondratova Y, Korobko D, Susla O, Soroka Y, Tsytsiura R, et al. Youden's test of the chromatographic determination of captopril in pharmaceuticals. Int J Green Pharm 2017;11:188-91.

Liliya Logoyda, Dmytro Korobko, Oleksandra Oleshchuk, Taras Proniv, Mariya Dmutriv. A HPLC MS/MS method development and validation for the simultaneous determination of bisoprolol and enalapril in the present of enalaprilat in human plasma. Int J Appl Pharm 2018;10:31-40.

Bhardwaj SP, Singh S. Study of the forced degradation behavior of enalapril maleate by LC and LC-MS and development of a validated stability-indicating assay method. J Pharm Biomed Anal 2008;46:113–20.