Abstract
A Quality by Design approach was used to develop a sensitive spectrophotometric method for determination of glucosamine Sulphate in pharmaceutical dosage forms and optimize a derivatization reaction of glucosamine with o-phthalaldhyde. This strategy was focused on derivatization process understanding and analytical method development and validation. Both of them were evaluated by applying risk assessment and Design Space tools. The scouting step was carried out by analyzing different derivatizing agents, type of buffers, pH of buffers, and time of reaction. Five critical process parameters (CPPs) were selected related to, pH of borate buffer, volume of 2-mercaptoethanol (ME), volume of o-phthalaldhyde (OPA), and the time of reaction. The effect of different levels of CPPs on critical quality attributes (CQAs) (the absorbance of derivative) was evaluated in the screening design using fractional factorial design. Using response surface methodology and contour plots the optimum values of the selected factors were determined and the design space of the method was defined. Finally, control strategy was designed and the method was validated and applied to a real sample of glucosamine dosage forms using the optimum derivatization conditions of the reaction; pH of borate buffer 10.5, concentration of buffer 0.05M, Time of reaction 10.7 minutes, volume of ME 100μL, and volume of OPA 5.1mL at room temperature. The results of the present study clearly shown that the developed method was sensitive relative to the other published spectrophotometric and HPLC methods with identification of the most significant factors affecting the derivatization reaction.
Highlights
Glucosamine sulphate (GLS) is commonly used as a therapeutic agent for treatment of osteoarthritis, its acceptance as a medical therapy varies
Since glucosamine is a precursor for glycosaminoglycan and glycosaminoglycan is a major component of joint cartilage, and supplemental glucosamine may help to rebuild cartilage and treat arthritis. (Sweetman, 2007) Different methods of analysis were published for determination of GLS as spectrophotometric methods (Wu et al, 2005; Gaonkar et al, 2006), HPLC methods, (Kumar et al, 2014; Song et al, 2012) HPTLC methods (Sullivan, et al, 2005; Sam Solomon, et al, 2010) and electrophoresis methods (8) (Vaclavikova et al, 2013)
critical quality attributes (CQAs) of spectrophotometric method was formation of derivative which influences the performance of the method
Summary
Glucosamine sulphate (GLS) is commonly used as a therapeutic agent for treatment of osteoarthritis, its acceptance as a medical therapy varies. The control strategy is obtained from the process understanding gained from modeling the design space and its purpose is to ensure the final quality of the method (Huang et al, 2009) In this presented work, a sensitive, rapid spectrophotometric method was developed for determination of GLS by derivatization using ophthaladehyde and by implementing the key elements of QbD to study the factors affecting the derivatization process and the performance of the method. (1) Different methods of analysis were published for determination of GLS as spectrophotometric methods (2-3), HPLC methods (4-5), HPTLC methods (6, 7), and electrophoresis methods (8, Quality by Design (QbD) has become an important paradigm in the pharmaceutical industry since its introduction by the US Food and Drug Administration. The control strategy is obtained from the process understanding gained from modeling the design space and its purpose is to ensure the final quality of the method. (15) In this presented work, a sensitive, rapid spectrophotometric method was developed for determination of GLS by derivatization using ophthaladehyde and by implementing the key elements of QbD to study the factors affecting the derivatization process and the performance of the method
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