Design of Experiment (DOE) Utilization to Develop a Simple and Robust Reversed-Phase HPLC Technique for Related Substances’ Estimation of Omeprazole Formulations

Manranjan, Vayeda Chintan; Yadav, Devendra Singh; Jogia, Hitesh; Chauhan, Praful Lalitkumar

doi:10.3797/scipharm.1306-06

Cited by 13 publications

(6 citation statements)

References 12 publications

(10 reference statements)

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“…The definition for design space of an LC method can be a “multidimensional combination and interaction of mobile phase variables (solvent composition) and chromatographic parameters (column oven temperature) that have been demonstrated to provide assurance of results obtained with the method”. The yellow region in the design space graph indicates that the responses are in an acceptable range and the grey region shows that the responses are below the desired level [ 27 – 29 ]. The center point parameters (2-propanol content, 8 mL; dichloromethane content, 10 mL; and column oven temperature, 25°C) are lying in the middle of the design space, hence these parameters were finalized for normal operation.…”

Section: Resultsmentioning

confidence: 99%

Development of a Stability-Indicating Stereoselective Method for the Quantification of Enantiomer in Drug Ssubstance and Pharmaceutical Dosage form of Rosuvastatin Calcium by Enhanced Approach

Reddy

Jyothi

2015

Sci. Pharm.

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A novel, simple, precise, and stability-indicating stereoselective method was developed and validated for the accurate quantification of the enantiomer in the drug substance and pharmaceutical dosage forms of Rosuvastatin Calcium. The method is capable of quantifying the enantiomer in the presence of other related substances. The chromatographic separation was achieved with an immobilized cellulose stationary phase (Chiralpak IB) 250 mm x 4.6 mm x 5.0 μm particle size column with a mobile phase containing a mixture of n-hexane, dichloromethane, 2-propanol, and trifluoroacetic acid in the ratio 82:10:8:0.2 (v/v/v/v). The eluted compounds were monitored at 243 nm and the run time was 18 min. Multivariate analysis and statistical tools were used to develop this highly robust method in a short span of time. The stability-indicating power of the method was established by subjecting Rosuvastatin Calcium to the stress conditions (forced degradation) of acid, base, oxidative, thermal, humidity, and photolytic degradation. Major degradation products were identified and found to be well-resolved from the enantiomer peak, proving the stability-indicating power of the method. The developed method was validated as per International Conference on Harmonization (ICH) guidelines with respect to specificity, limit of detection and limit of quantification, precision, linearity, accuracy, and robustness. The method exhibited consistent, high-quality recoveries (100 ± 10%) with a high precision for the enantiomer. Linear regression analysis revealed an excellent correlation between the peak responses and concentrations (r2 value of 0.9977) for the enantiomer. The method is sensitive enough to quantify the enantiomer above 0.04% and detect the enantiomer above 0.015% in Rosuvastatin Calcium. The stability tests were also performed on the drug substances as per ICH norms.

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Section: Resultsmentioning

confidence: 99%

Development of a Stability-Indicating Stereoselective Method for the Quantification of Enantiomer in Drug Ssubstance and Pharmaceutical Dosage form of Rosuvastatin Calcium by Enhanced Approach

Reddy

Jyothi

2015

Sci. Pharm.

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“…17 When multiple analytes are to be separated in single chromatographic run, DoE tool was experimented for better evaluation and understanding of relation between variables of method on responses. 18 As optimized conditions with encouraging resolution between all closely eluting impurities was not achieved with OFAT experiments, response surface methodology a Height of peak is multiplied by a factor of 10 for ease of interpretation with historical data design (RSH) was implemented by combining all the fourteen OFAT experiments to DoE (Table 2). The study ranges were 0-5 g/L of 1-decane sulfonic acid as ion pair reagent in mobile phase, 1.87-4.30 range for pH of mobile phase and 0.2-1.5 %/ min of gradient change for ACN in mobile phase at 6 min.…”

Section: Application Of Doe For Chromatographic Separationmentioning

confidence: 99%

Chemometric Assisted Development and Validation of a Stability-indicating LC Method for Determination of Related Substances in Haloperidol Decanoate Injection

Babu¹,

Rao²,

Babu³

et al. 2021

IJPER

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Aim: Haloperidol decanoate injection is a phenyl butyl piperadine derivative with antipsychotic, neuroleptic, antiemetic effects and has multiple related substances as process and degradant impurities. Objectives: This study focuses on chemometric assisted liquid chromatographic approach to develop a stability indicating impurity profile of Haloperidol decanoate injection. Methodology: Dual experimental designs (combined mixture I-optimal design and response surface historical data design) were employed to resolve all thirteen known impurities of Haloperidol decanoate. Chromatographic separation was achieved on a Hypersil BDS C 18 (100 x 4.0 mm) 3-µm column to attain separation of related compounds. Results: The optimum conditions for the chromatographic system resulted in a mobile phase consisting of tetra butyl ammonium hydrogen sulphate/ 1-decane Sulphonate sodium buffer solution and acetonitrile with linear gradient elution at a flow rate of 1.4 mL/min. Selectivity, forced degradation, linearity, accuracy and precision were demonstrated in a range of 0.75-30.0 µg/mL. Conclusion: The optimized method was able to resolve the ghost peak observed because of gradient change of mobile phase and is able to separate both polar and non-polar impurities within 60 min, in single method, with resolution of more than 2.0 between adjacent impurities. The inter-day precision for all impurities and haloperidol decanoate were evaluated and found to have a % RSD of less than 10.

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“…The design of experiments (DoE) is a systematic approach for identifying and analyzing the critical attributes involved in the method development process [19]. The application of DoE during the analytical method has been reported at various stages right from initial screening and identification of critical chromatographic parameters, optimization, and robustness estimation [20–25].…”

Section: Introductionmentioning

confidence: 99%

Box–Behnken design aided optimization and validation of developed reverse phase HPLC analytical method for simultaneous quantification of dolutegravir sodium and lamivudine co‐loaded in nano‐liposomes

Mutalik

Mullick

Pandey

et al. 2021

J of Separation Science

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A stability‐indicating reversed‐phase high‐performance liquid chromatography method for simultaneous estimation of dolutegravir sodium and lamivudine encapsulated in the nanoliposomal formulation was developed. The chromatographic parameters namely, organic phase ratio, flow rate, and sample injection volume were selected as independent factors and were optimized by multivariate Box–Behnken design. Responses analyzed were retention time, peak area, and resolution. The optimized chromatographic method with Hypersil BDS C8 CN column as stationary phase and methanol and acetonitrile mixture and acidified Milli‐Q water (pH 2.8, adjusted with 0.02% v/v orthophosphoric acid) as the mobile phase in an isocratic elution mode was validated according to parameters of International Conference on Harmonization Q1(R2) guidelines. The validated reversed‐phase high‐performance liquid chromatography method exhibited specificity for both dolutegravir sodium and lamivudine in the presence of degradation products as well as the liposomal matrix. This method was effectively utilized to determine the amount of drug entrapped and drug loading efficiency of dolutegravir sodium and lamivudine in a nano‐liposomal formulation.

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Design of Experiment (DOE) Utilization to Develop a Simple and Robust Reversed-Phase HPLC Technique for Related Substances’ Estimation of Omeprazole Formulations

Cited by 13 publications

References 12 publications

Development of a Stability-Indicating Stereoselective Method for the Quantification of Enantiomer in Drug Ssubstance and Pharmaceutical Dosage form of Rosuvastatin Calcium by Enhanced Approach

Development of a Stability-Indicating Stereoselective Method for the Quantification of Enantiomer in Drug Ssubstance and Pharmaceutical Dosage form of Rosuvastatin Calcium by Enhanced Approach

Chemometric Assisted Development and Validation of a Stability-indicating LC Method for Determination of Related Substances in Haloperidol Decanoate Injection

Box–Behnken design aided optimization and validation of developed reverse phase HPLC analytical method for simultaneous quantification of dolutegravir sodium and lamivudine co‐loaded in nano‐liposomes

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