NMR spectroscopy validation of sodium estimation in API.
Journal name: World Journal of Pharmaceutical Research
Original article title: Validation of analytical method of estimation of sodium in api with the help of nmr spectroscopy
The WJPR includes peer-reviewed publications such as scientific research papers, reports, review articles, company news, thesis reports and case studies in areas of Biology, Pharmaceutical industries and Chemical technology while incorporating ancient fields of knowledge such combining Ayurveda with scientific data.
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Original source:
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Partha Mukherjee, Prasant K Deb, Kartikewa Dwivedi
World Journal of Pharmaceutical Research:
(An ISO 9001:2015 Certified International Journal)
Full text available for: Validation of analytical method of estimation of sodium in api with the help of nmr spectroscopy
Source type: An International Peer Reviewed Journal for Pharmaceutical and Medical and Scientific Research
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Summary of article contents:
Introduction
The study conducted by Mukherjee et al. in 2015 aimed to develop and validate an analytical method to estimate sodium content in active pharmaceutical ingredients (APIs) using Nuclear Magnetic Resonance (NMR) spectroscopy. This method is specifically designed to address the challenges of sodium quantification, which is typically complicated due to the overlapping NMR signals of sodium and other compounds. The work discusses the advantages of this NMR technique over traditional methods like flame photometry and atomic absorption spectrophotometry, focusing on the novel approach of using separate standard and analyte solutions to improve accuracy and ease of measurement.
Importance of Method Validation
One of the key components of this study was the validation of the NMR method according to International Council for Harmonisation (ICH) guidelines. The validation process involved evaluating several characteristics, including specificity, linearity, accuracy, and precision. The linearity of the method was assessed using sodium chloride (NaCl) as an internal standard in varying concentrations, resulting in a linear calibration curve from 0.35 mg/ml to 2.74 mg/ml. The accuracy of the method was demonstrated through recovery studies, achieving an average recovery rate of nearly 99.44%, showcasing the reliability of the developed method in quantifying sodium.
Precision and Robustness of the Method
The precision of the NMR method was rigorously tested through both intraday and interday variability studies, yielding percentage relative standard deviation (%RSD) values of less than 2% for both measurements, indicating high precision. Furthermore, the robustness of the method was confirmed by slight modifications to experimental conditions, such as varying delay times and temperatures, which resulted in minimal impact on the outcomes. This aspect highlights the method’s capability to maintain accuracy across different operating conditions, affirming its robustness for routine laboratory analysis.
Comparison with Other Analytical Techniques
In addition to validating the method, the comparison between the results obtained using NMR and those from atomic absorption spectrometry (AAS) showed strong correlation across various samples. The sodium content results from both analytical methods were very similar, which further establishes the credibility of the NMR technique as a valid alternative for sodium quantification in pharmaceutical applications. This comparison underscores the potential of NMR spectroscopy to serve as a reliable tool in quality control and assurance within pharmaceutical research and development.
Conclusion
In summary, the study presents a significant advancement in the quantification of sodium in APIs, demonstrating that the proposed NMR method is not only accurate and precise but also simple and robust enough for practical applications. The ability to independently measure standard and analyte solutions minimizes interference and improves reliability, making it an important contribution to analytical methodologies in pharmaceutical sciences. This validated method could facilitate more efficient monitoring and control of sodium levels in drug formulations, ensuring product safety and efficacy.
FAQ section (important questions/answers):
What is the purpose of the analytical method developed?
The method aims to estimate the percentage of sodium present as salt or inorganic impurity in Active Pharmaceutical Ingredients (API) and drug molecules using NMR spectroscopy.
How does this method differ from conventional quantitative NMR techniques?
Unlike traditional Q-NMR, which mixes the internal standard and analyte, this method utilizes separate preparations for the standard and analyte solutions to avoid overlapping peaks.
What were the validation parameters used for the method?
The method was validated based on specificity, linearity, range, accuracy, precision, robustness, and ruggedness, following ICH guidelines to ensure reliability and effectiveness.
How was the accuracy of the method assessed?
Accuracy was determined by preparing different concentrations of solutions and calculating percent recovery from known amounts, yielding high recovery percentages indicating method reliability.
What were the limits of detection and quantitation for sodium?
The limit of detection (LOD) was determined to be 0.10 mg/ml, while the limit of quantitation (LOQ) was 0.31 mg/ml, indicating the method's sensitivity.
What conclusion was drawn regarding the proposed method?
The study concluded that the developed method is accurate, precise, robust, and suitable for estimating sodium in both APIs and small organic compounds.
Glossary definitions and references:
Scientific and Ayurvedic Glossary list for “NMR spectroscopy validation of sodium estimation in API.”. This list explains important keywords that occur in this article and links it to the glossary for a better understanding of that concept in the context of Ayurveda and other topics.
1) Table:
[see source text or glossary: #Table#] The term 'Table' refers to numerical or visual data representations that summarize findings and observations in studies and methodologies. In this context, tables are used to present quantitative results from experiments, showcasing calibration curves, accuracy percentages, and other validation parameters relevant to the analytical method of estimating sodium.
2) Study (Studying):
[see source text or glossary: #Studying#] The act of 'Studying' signifies the careful examination and evaluation of methodologies, data, and results, particularly regarding the sodium estimation process via NMR spectroscopy. It involves exploring various experimental parameters and validation characteristics as part of improving analytical techniques in pharmaceutical research.
3) Drug:
The term 'Drug' is used to describe active pharmaceutical ingredients (APIs) analyzed in the study for sodium content. Estimating the sodium levels in drugs is crucial for ensuring product safety, efficacy, and compliance with regulatory standards, which is a central aim of the research presented in the document.
4) Partha:
Partha Mukherjee is the lead author of the research study. As a significant contributor, he directs the research framework and presents methodologies that leverage NMR spectroscopy for sodium estimation. His expertise and guidance are critical for formulating accurate analytical methods applicable to pharmaceutical research.
5) India:
India is the geographical context of the research, housing Jubilant Chemsys Limited, the institution where the study was conducted. The country serves as a base for pharmaceutical innovations, regulatory frameworks, and research development practices that ensure the safety and efficiency of APIs and drug formulations.
6) Discussion:
The 'Discussion' section in research involves analyzing and interpreting the results obtained from the study. In this document, it allows the authors to draw comparisons between the proposed method and existing techniques for sodium estimation, presenting insights into the method’s efficiency, reliability, and potential applications in pharmaceutical analysis.
7) Knowledge:
Knowledge in this context refers to the understanding and insights gained through the study about sodium estimation using NMR spectroscopy. It contributes to the scientific community's overall expertise in analytical methodologies, enhancing the validation processes for pharmaceuticals and providing guidelines for improved accuracy in drug analysis.
8) Nature:
[see source text or glossary: #Nature#] The 'Nature' of the study relates to the essential qualities and characteristics of the sodium present in APIs and drug formulations. Understanding the nature of these substances is vital for accurate analytical measurements and helps in distinguishing between sodium as a salt or inorganic impurity within the drug compounds.
9) Patil:
[see source text or glossary: #Patil#] Patil is cited in the text as a reference for existing methods of sodium estimation, indicating a previous contribution to the field. The mention of Patil acknowledges the historical context of the research and the ongoing evolution of analytical techniques in sodium quantification.
10) Pulse:
[see source text or glossary: #Pulse#] In the context of NMR spectroscopy, 'Pulse' refers to the specific pulse sequences used during the acquisition of NMR data. The pulse length parameters specified in the research are essential for optimizing signal detection and ensuring accurate integration values during sodium analysis, thereby enhancing method precision.
11) Salt (Salty):
The term 'Salt' is particularly relevant in the analysis of sodium as it can represent its presence in the form of sodium chloride (NaCl), which was utilized as an internal standard in the experiments. Mixing salt with the analyte facilitates the accurate quantification of sodium concentrations, serving as a crucial element in the research methodology.
Other Science Concepts:
Discover the significance of concepts within the article: ‘NMR spectroscopy validation of sodium estimation in API.’. Further sources in the context of Science might help you critically compare this page with similair documents:
Sodium chloride, Analytical method, Limit of detection, Internal standard, Calibration curve, Specificity of method, Spectrophotometric method, Limit of quantitation.