Lc-MS/MS Method Development and Validation for the Determination of Cardiazol in Human Plasma

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.

Spectrophotometric methods for the determination of lisinopril in medicines

“…Analytical methods of analysis such as HPLC (El Gindy et al 2001;Beasley et al 2005;Ivanovic et al 2007;Chauhan et al 2011;Sultana et al 2011;Naveed et al 2012;Arayne et al 2013;Peleshok et al 2021a;Shulyak et al 2021), LC/MS (Andreas et al 2003;Huang et al 2006;Drapak et al 2019a, b), gas chromatography with mass detection (Leis et al 1998(Leis et al , 1999, spectrophotometry (El-Emam et al 2004;Rahman et al 2005a, b;Basavaiah et al 2009;Jamakhandi et al 2011;Sbârcea et al 2014) have been developed for the determination of lisinopril in medicines and biological liquids. Spectrophotometry as a quantitative analytical methodology belongs to the foremost oftused analytical techniques in pharmaceutical analysis.…”