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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

Typical overlay chromatogram of the blank, placebo, and standard preparation
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Figure 2: Typical overlay chromatogram of the blank, placebo, and standard preparation

Mentions: Extraction of the active components from the semisolid sample matrix with acceptable recovery is a very critical aspect for sample preparation and was achieved by selecting the right diluent in the following manner. Considering the solubility of all the components, acetonitrile was used as diluent and satisfactory recovery was obtained. Based on the above experimental data, the chromatographic separation was finalized by the following gradient program time (min)/mobile phase A (%)/mobile phase B (%); 0.0/100/0, 9/100/0, 19/55/45, 31/15/85, 34/10/90, 44/10/90, 50/100/0, 55/100/0, at a flow rate of 1.2 mL/min at 30°C (column oven) temperature, detection wavelength 257 nm with 10 μL injection volume. By using the above chromatographic conditions and diluent, the standard, sample, and placebo preparation were made and injected into the HPLC with the developed parameters (Fig. 2).


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)

Typical overlay chromatogram of the blank, placebo, and standard preparation
© Copyright Policy - open-access
Related In: Results  -  Collection

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

Figure 2: Typical overlay chromatogram of the blank, placebo, and standard preparation
Mentions: Extraction of the active components from the semisolid sample matrix with acceptable recovery is a very critical aspect for sample preparation and was achieved by selecting the right diluent in the following manner. Considering the solubility of all the components, acetonitrile was used as diluent and satisfactory recovery was obtained. Based on the above experimental data, the chromatographic separation was finalized by the following gradient program time (min)/mobile phase A (%)/mobile phase B (%); 0.0/100/0, 9/100/0, 19/55/45, 31/15/85, 34/10/90, 44/10/90, 50/100/0, 55/100/0, at a flow rate of 1.2 mL/min at 30°C (column oven) temperature, detection wavelength 257 nm with 10 μL injection volume. By using the above chromatographic conditions and diluent, the standard, sample, and placebo preparation were made and injected into the HPLC with the developed parameters (Fig. 2).

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