Unique liquid chromatography technique for the determination of mirabegron in the presence of polymers; robustness by Design Expert in the light of Quality by Design

Abstract

The current study is designed to estimate mirabegron in the presence of high molecular weight polymers using a unique liquid chromatography method and sample preparation technique. The proposed method is significant because of the many analytical issues faced during the development studies. Based on the experimental results, we finally achieved the stability-indicating power of the method. The adequately prepared mobile phase was in the ratio of pH 2.0 buffer and acetonitrile (80:20) v/v, and the buffer pH 2.0 was prepared as follows: 8.7 ml of perchloric acid, 2 ml of triethylamine and 3.0 g sodium hydroxide into 1 L of water mixed well. The system suitability parameters were achieved using a Waters X-Bridge C 18 (4.6 Â 150 mm, 3.5 μm) column and mobile phase. The optimized chromatographic conditions included a column temperature of 45 C, a flow rate of 1.0 ml min À1 ; an injection volume of 5 μl, UV 247 nm, and 15 min runtime. The method was validated and transferred to quality control as per International Conference on Harmonization Q2(R1) and the Chinese Pharmacopoeia 2020 edition <9101> and <9100>. The recovery and linearity results were obtained between 99.0 and 101.0%; the value of r 2 was 0.9998. The method robustness study was established by utilizing the Design of Experiments part of the Quality by Design concept. The method's stability-indicating nature was proved by a forced degradation study; all of the conditions for analyte peak purity were passed, and mass balance was achieved. The method was used to determine mirabegron assay, as well as content uniformity, blend uniformity and cleaning samples. It is a user-friendly and cost-effective method.

Determination of Valbenazine related substances by liquid chromatography method complying with the current regulatory guidelines. Method robustness evaluation by Design of Experiments software

“…Experiments were performed using spiked sample solutions with specified levels of impurities and reference standard solutions to monitor the output response. The input parameters are changed from the actual process conditions as follows [22][23][24][25]. pH varied ± 0.2 units 1.…”

QbD‐based stability‐indicating liquid chromatography (RP‐HPLC) method for the determination of flurbiprofen in cataplasm

“…The quality by design (QbD) concept is newly, officially introduced by regulatory bodies and the International Conference on Harmonization (ICH) (Dandabattina et al, 2022; ICH, Q14, 2022; Reddy Saddala et al, 2022). The current proposed research considered the guidelines and suggestions from the regulatory bodies and utilized the QbD design of experiments (DoE) approach to study the method robustness (Katakam et al, 2021; Konduru, Gundla, et al, 2022; Konduru, Kowtharapu, & Gundla, 2022; Kowtharapu, Katari, Sandoval, Muchakayala, et al, 2022; Kowtharapu, Katari, Sandoval, Rekulapally, et al, 2022; Kowtharapu, Katari, Surekha, et al, 2022; Muchakayala et al, 2021; Subramanian et al, 2020, 2021).…”

Determination and quantification of related substances and degradation products in bictegravir by full factorial design evaluated HPLC and mass spectrometry

“…Hence, LC-MS methods have also been developed to identify and predict other unknown impurities, such as major degraded analytes in the product. Furthermore, to evaluate viable and robust method conditions such as buffer concentration, ow rate, column oven temperature [8][9][10][11][12][13][14][15][16] and chromatographic conditions with the requirement of current regulatory guidelines, multivariate Design of Experiments (DoEs) has been introduced in this study.…”