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Quality by Design-Based Development of a Stability-Indicating RP-HPLC Method for the Simultaneous Determination of Methylparaben, Propylparaben, Diethylamino Hydroxybenzoyl Hexyl Benzoate, and Octinoxate in Topical Pharmaceutical Formulation.

Roy C, Chakrabarty J - Sci Pharm (2014)

Bottom Line: Recovery for all the components was found to be in the range of 98-102%.The design expert with ANOVA software with the linear model was applied and a 2(4) full factorial design was employed to estimate the model coefficients and also to check the robustness of the method.Results of the two-level full factorial design, 2(4) with 20 runs including four centrepoint analysis based on the variance analysis (ANOVA), demonstrated that all four factors, as well as the interactions of resolution between DAHHB and OCT are statistically significant.

View Article: PubMed Central - PubMed

Affiliation: Analytical Research and Development, Integrated Product Development, Dr. Reddy's Laboratories Ltd., Bachupally, Hyderabad-500090, Andhra Pradesh, India. ; Department of Chemistry, National Institute of Technology, Durgapur-713209, West Bengal, India.

ABSTRACT
A stability-indicating RP-HPLC method has been developed and validated for the simultaneous determination of methylparaben (MP), propylparaben (PP), diethylamino hydroxybenzoyl hexyl benzoate (DAHHB), and octinoxate (OCT) in topical pharmaceutical formulation. The desired chromatographic separation was achieved on the Kinetex(TM) C18 (250 × 4.6 mm, 5 μm) column using gradient elution at 257 nm detection wavelength. The optimized mobile phase consisted of a buffer : acetonitrile : tetrahydrofuran (60 : 30 : 10, v/v/v) as solvent A and acetonitrile : tetrahydrofuran (70 : 30, v/v) as solvent B. The method showed linearity over the range of 0.19-148.4 μg/mL, 0.23-15.3 μg/mL, 1.97-600.5 μg/mL, and 1.85-451.5 μg/mL for MP, PP, DAHHB, and OCT, respectively. Recovery for all the components was found to be in the range of 98-102%. The stability-indicating capability of the developed method was established by analysing the forced degradation samples in which the spectral purity of MP, PP, DAHHB, and OCT, along with the separation of the degradation products from the analyte peaks, was achieved. The proposed method was successfully applied for the quantitative determination of MP, PP, DAHHB, and OCT in the lotion sample. The design expert with ANOVA software with the linear model was applied and a 2(4) full factorial design was employed to estimate the model coefficients and also to check the robustness of the method. Results of the two-level full factorial design, 2(4) with 20 runs including four centrepoint analysis based on the variance analysis (ANOVA), demonstrated that all four factors, as well as the interactions of resolution between DAHHB and OCT are statistically significant.

No MeSH data available.


Related in: MedlinePlus

Graphical plot of the full factorial design space for between two factors A (flow rate) and B (column temperature) at fixed factor C (THF composition in mobile phase A) and factor D (THF composition in mobile phase B)
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Figure 7: Graphical plot of the full factorial design space for between two factors A (flow rate) and B (column temperature) at fixed factor C (THF composition in mobile phase A) and factor D (THF composition in mobile phase B)

Mentions: DOE revolves around the concept of the design space, the multidimensional combination and interaction of input variables and process parameters that have demonstrated to provide the assurance of quality. Working within the design space is not considered as a change. Movement out of the design space is considered to be a change and would normally initiate a regulatory post-approval change process. Design space is proposed by the applicant and is subject to regulatory assessment and approval [27–30]. Design space was established by employing full factorial design variables of the flow rate (A) 1.0–1.4 mL/ min, column temperature (B) 25–35°C, % tetrahydrofuran composition in mobile phase A (C) 8–12%, and % tetrahydrofuran composition in mobile phase B (C) 25–35% and their respective responses which are presented in Figure 7.


Quality by Design-Based Development of a Stability-Indicating RP-HPLC Method for the Simultaneous Determination of Methylparaben, Propylparaben, Diethylamino Hydroxybenzoyl Hexyl Benzoate, and Octinoxate in Topical Pharmaceutical Formulation.

Roy C, Chakrabarty J - Sci Pharm (2014)

Graphical plot of the full factorial design space for between two factors A (flow rate) and B (column temperature) at fixed factor C (THF composition in mobile phase A) and factor D (THF composition in mobile phase B)
© Copyright Policy - open-access
Related In: Results  -  Collection

License
Show All Figures
getmorefigures.php?uid=PMC4318166&req=5

Figure 7: Graphical plot of the full factorial design space for between two factors A (flow rate) and B (column temperature) at fixed factor C (THF composition in mobile phase A) and factor D (THF composition in mobile phase B)
Mentions: DOE revolves around the concept of the design space, the multidimensional combination and interaction of input variables and process parameters that have demonstrated to provide the assurance of quality. Working within the design space is not considered as a change. Movement out of the design space is considered to be a change and would normally initiate a regulatory post-approval change process. Design space is proposed by the applicant and is subject to regulatory assessment and approval [27–30]. Design space was established by employing full factorial design variables of the flow rate (A) 1.0–1.4 mL/ min, column temperature (B) 25–35°C, % tetrahydrofuran composition in mobile phase A (C) 8–12%, and % tetrahydrofuran composition in mobile phase B (C) 25–35% and their respective responses which are presented in Figure 7.

Bottom Line: Recovery for all the components was found to be in the range of 98-102%.The design expert with ANOVA software with the linear model was applied and a 2(4) full factorial design was employed to estimate the model coefficients and also to check the robustness of the method.Results of the two-level full factorial design, 2(4) with 20 runs including four centrepoint analysis based on the variance analysis (ANOVA), demonstrated that all four factors, as well as the interactions of resolution between DAHHB and OCT are statistically significant.

View Article: PubMed Central - PubMed

Affiliation: Analytical Research and Development, Integrated Product Development, Dr. Reddy's Laboratories Ltd., Bachupally, Hyderabad-500090, Andhra Pradesh, India. ; Department of Chemistry, National Institute of Technology, Durgapur-713209, West Bengal, India.

ABSTRACT
A stability-indicating RP-HPLC method has been developed and validated for the simultaneous determination of methylparaben (MP), propylparaben (PP), diethylamino hydroxybenzoyl hexyl benzoate (DAHHB), and octinoxate (OCT) in topical pharmaceutical formulation. The desired chromatographic separation was achieved on the Kinetex(TM) C18 (250 × 4.6 mm, 5 μm) column using gradient elution at 257 nm detection wavelength. The optimized mobile phase consisted of a buffer : acetonitrile : tetrahydrofuran (60 : 30 : 10, v/v/v) as solvent A and acetonitrile : tetrahydrofuran (70 : 30, v/v) as solvent B. The method showed linearity over the range of 0.19-148.4 μg/mL, 0.23-15.3 μg/mL, 1.97-600.5 μg/mL, and 1.85-451.5 μg/mL for MP, PP, DAHHB, and OCT, respectively. Recovery for all the components was found to be in the range of 98-102%. The stability-indicating capability of the developed method was established by analysing the forced degradation samples in which the spectral purity of MP, PP, DAHHB, and OCT, along with the separation of the degradation products from the analyte peaks, was achieved. The proposed method was successfully applied for the quantitative determination of MP, PP, DAHHB, and OCT in the lotion sample. The design expert with ANOVA software with the linear model was applied and a 2(4) full factorial design was employed to estimate the model coefficients and also to check the robustness of the method. Results of the two-level full factorial design, 2(4) with 20 runs including four centrepoint analysis based on the variance analysis (ANOVA), demonstrated that all four factors, as well as the interactions of resolution between DAHHB and OCT are statistically significant.

No MeSH data available.


Related in: MedlinePlus