Implementation of analytical quality by design and green chemistry principles to develop an ultra-high performance liquid chromatography method for the determination of Fluocinolone Acetonide impurities from its drug substance and topical oil formulations

Muchakayala, Siva Krishna; Katari, Naresh Kumar; Saripella, Kalyan Kumar; Schaaf, Henele; Marisetti, Vishnu Murthy; Ettaboina, Santhosh Kumar; Rekulapally, Vijay Kumar

doi:10.1016/j.chroma.2022.463380

Cited by 63 publications

(32 citation statements)

References 32 publications

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“…Its shows the stability‐indicating power of the method. All the results of degradation studies are shown in Figure 5(a–f) and Table 5 (Cholleti et al, 2022; Muchakayala et al, 2021; Muchakayala et al, 2022; Nakkala et al, 2022; Pydimarry, Cholleti, & Vangala, 2014; Pydimarry, Cholleti, & Venagala, 2014).…”

Section: Resultsmentioning

confidence: 99%

Development and validation of a stability‐indicating, single HPLC method for sacubitril–valsartan and their stereoisomers and identification of forced degradation products using LC–MS/MS

Vijaykumar

Yalavarti²,

Aparna

2022

Biomedical Chromatography

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The aim of this research work was to develop and validate a stability-indicating, single reversed-phase HPLC method for the separation of five impurities, including enantiomers, diastereomers, and degradation products in sacubitril-valsartan tablets.The method was developed using a Chiralcel OJ-RH column (150 Â 4.6 mm, 5 μm) at 45 C with a gradient program of (T/%B) 0.01/25, 10.0/25, 25/38, 37.0/45, 39.0/25, and 45.0/25 at a flow rate of 0.8 ml/min. Mobile phase A consisted of 1 ml of trifluoroacetic acid in 1000 ml of Milli-Q water. Mobile phase B consisted of 1 ml of trifluoroacetic acid in a mixture of acetonitrile and methanol in the ratio of 950:50 (v/v). Sacubitril, valsartan, and their five impurities were monitored at 254 nm. Degradation was not observed when sacubitril-valsartan was subjected to heat, light, hydrolytic, and oxidation conditions. In acid degradation study (1 N HCl/60 C/2 h) impurity 1 (m/z 383.44) was formed, and in base degradation study (0.1 N NaOH/40 C/1 h) impurities 1 and 5 (m/z 265.35) were formed; both impurities were confirmed using LC-MS. The degradation products, enantiomers, and diastereomers were well separated from sacubitril and valsartan, proving the stability-indicating power of the method. The developed method was validated per the International Council for Harmonisation of Technical Requirements for Pharmaceuticals for Human Use guidelines. The inter-and intra-day percentage relative standard deviation for sacubitril, valsartan, and their five impurities was less than 5.2%, recovery of the five impurities was between 93 and 105%, and linearity was ≥0.999. The limit of detection was 0.030-0.048 μg/ml, and the limit of quantification was 0.100-0.160 μg/ml.

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Section: Resultsmentioning

confidence: 99%

Development and validation of a stability‐indicating, single HPLC method for sacubitril–valsartan and their stereoisomers and identification of forced degradation products using LC–MS/MS

Vijaykumar

Yalavarti²,

Aparna

2022

Biomedical Chromatography

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“…In the process of developing new drugs, the AQbD approaches have been applied in several stages, such as raw material control [ 94 ], bioassay [ 95 , 96 ], stability test [ 96 , 97 ], impurity test [ 98 , 99 , 100 ], efficacy and safety test [ 101 ]. However, there are several limits to apply the AQbD approach in developing new drugs based on medicinal plants, and this is closely related to the limitations of botanical resources as a raw material for drug development [ 1 ].…”

Section: Perspectives : Challenges and Prospectsmentioning

confidence: 99%

Analytical Quality by Design (AQbD) Approach to the Development of Analytical Procedures for Medicinal Plants

Park

Kim

et al. 2022

Plants

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Scientific regulatory systems with suitable analytical methods for monitoring quality, safety, and efficacy are essential in medicinal plant drug discovery. There have been only few attempts to adopt the analytical quality by design (AQbD) strategy in medicinal plants analysis over the last few years. AQbD is a holistic method and development approach that understands analytical procedure, from risk assessment to lifecycle management. The enhanced AQbD approach reduces the time and effort necessary to develop reliable analytical methods, leads to flexible change control through the method operable design region (MODR), and lowers the out-of-specification (OOS) results. However, it is difficult to follow all the AQbD workflow steps in the field of medicinal plants analysis, such as defining the analytical target profiles (ATPs), identifying critical analytical procedure parameters (CAPPs), among others, because the complexity of chemical and biological properties in medicinal plants acts as a barrier. In this review, various applications of AQbD to medicinal plant analytical procedures are discussed. Unlike the analysis of a single compound, medicinal plant analysis is characterized by analyzing multiple components contained in biological materials, so it will be summarized by focusing on the following points: Analytical methods showing correlations within analysis parameters for the specific medicinal plant analysis, plant raw material diversity, one or more analysis targets defined for multiple phytochemicals, key analysis attributes, and analysis control strategies. In addition, the opportunities available through the use of design-based quality management techniques and the challenges that coexist are also discussed.

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“…A traditional one-factor-at-a-time (OFAT) method development process is a time-consuming, trial and error approach 29 – 38 . The QbD-based method development process is a systematic approach that involves identifying probable risks that cause failures.…”

Section: Introductionmentioning

confidence: 99%

AQbD based green UPLC method to determine mycophenolate mofetil impurities and Identification of degradation products by QToF LCMS

Muchakayala

Katari

Saripella

et al. 2022

Sci Rep

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We report an ideal method for quantifying impurities in mycophenolate mofetil drug substances and their oral suspension preparations. We developed a systematic and eco-friendly analytical approach utilizing quality by design (QbD) and green chemistry principles. Initially, the critical method parameters (CMPs) were screened using a D-optimal design. The robust final method conditions were optimized using a systematic central composite design (CCD). Through graphical and numerical optimization, the protocol conditions were augmented. The pH of mobile phase buffer (25 mM KH2PO4) (MP-A), initial gradient composition (% MP-A), flow rate (mL min−1), and column oven temperatures (°C) are 4.05, 87, 0.4, and 30, respectively. The best possible separation between the critical pairs was achieved while using the Waters Acquity UPLC BEH C18 (100 × 2.1) mm, 1.7 µm analytical column. A mixture of water and acetonitrile in the ratio of 30:70 (v/v) was used as mobile phase-B for the gradient elution. The analytical method was validated in agreement with ICH and USP guidelines. The specificity results revealed that no peaks interfered with the impurities and MPM. The mean recovery of the impurities ranged between 96.2 and 102.7%, and the linearity results r > 0.999 across the range of LOQ – 150%. The precision results (%RSD) ranged between 0.8 and 4.5%. The degradation products formed during the base-induced degradation were identified as isomers of mycophenolic acid and sorbitol esters using Q-ToF LC–MS and their molecular and fragment ion peaks. The developed method eco-friendliness and greenness were assessed using analytical greenness (AGREE), green analytical procedure index (GAPI), and analytical eco score, and found it is green.

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Implementation of analytical quality by design and green chemistry principles to develop an ultra-high performance liquid chromatography method for the determination of Fluocinolone Acetonide impurities from its drug substance and topical oil formulations

Cited by 63 publications

References 32 publications

Development and validation of a stability‐indicating, single HPLC method for sacubitril–valsartan and their stereoisomers and identification of forced degradation products using LC–MS/MS

Development and validation of a stability‐indicating, single HPLC method for sacubitril–valsartan and their stereoisomers and identification of forced degradation products using LC–MS/MS

Analytical Quality by Design (AQbD) Approach to the Development of Analytical Procedures for Medicinal Plants

AQbD based green UPLC method to determine mycophenolate mofetil impurities and Identification of degradation products by QToF LCMS

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