Analytical eco‐scale and quality by design‐oriented liquid chromatography method for simultaneous quantification of metoprolol succinate, telmisartan, and cilnidipine in their fixed‐dose combination

Abstract

A new combination of metoprolol succinate, telmisartan, and cilnidipine is recently approved to treat hypertension effectively. A reversed‐phase liquid chromatography method was developed to quantify the said compounds, combining analytical eco‐scale and quality‐by‐design approach. The former one revealed an excellent green score for the present method. Later, method variables were assessed for risks and optimized using the quality‐by‐design‐oriented method development. The optimization process included using a Box‐Behnken design, and the obtained response surfaces for resolution amongst target peaks were mapped systematically. The optimal separation conditions employed a mobile phase of methanol: 0.01 M KH2PO4 buffer of pH 3.0 (70:30, %v/v) flowing at a rate of 1.0 mL/min on a C18 column with diode array detection at 240 nm. All three analyte peaks were well separated from each other with a resolution greater than 2.0. The analytical method was linear (2.5‐80 μg/mL) for target compounds with accuracy (>99%), and precision (<1%) results complying with regulatory requirements. The results of detection and quantitation limits, solution stability, and system suitability limit were good and acceptable. The current method selectively quantified the analytes from commercial dosage forms. Overall a green analytical method is developed and suitable for estimating metoprolol, telmisartan, and cilnidipine simultaneously in their combined pharmaceutical formulations.

Dispersive Membrane Microextraction of Substituted Phenols from Honey Samples and a Brief Outlook on Its Sustainability Using Analytical Eco-Scale and Analytical GREEnness Metric Approach

“…Galuszka et al (2012) proposed the categorization of the analytical eco-scale into four main segments with 100 being ideal, above 75 being excellent, 74–50 being acceptable, and anything below 50 being inadequate. Table 4 summarizes the penalty point calculations for the proposed DMME–HPLC method with reference to the AES [ 24 , 45 ]. By virtue of this, the AES value of our method fell under the excellent category with a score of 94.…”

Experimental design in HPLC separation of pharmaceuticals

“…Literature survey revealed tremendous number of HPLC methods that were developed using DoE-based AQbD approach in recent years (23,62,69,(71)(72)(73). In most studies, CCD and D-optimal designs were favorably used to optimize HPLC systems with 2 critical method parameters (CMPs) and BBD in case of 3 or 4 CMPs.…”

Design of Experimental Approach for Development of Rapid High Performance Liquid Chromatographic Process for Simultaneous Estimation of Metoprolol, Telmisartan, and Amlodipine from Formulation: Greenness and Whiteness Evaluation

“…This decreases the work pressure of the heart and reduces pain in the chest [ 5 ]. Analytical procedures are well documented in the literature for the analysis of MET, TEL, and AML alone and along with other drugs [ 6 , 7 , 8 , 9 , 10 , 11 , 12 , 13 ]. The literature documented the implementation of the HPLC technique [ 14 ] for the quantification of AML along with its impurities in formulation.…”