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  • 1
    In: Journal of AOAC International, Oxford University Press (OUP), ( 2024-07-17)
    Abstract: Accurate determination of active pharmaceutical ingredients and impurities is essential for ensuring the safety and effectiveness of medications. This study focuses on the validation of a high-performance liquid chromatography (HPLC) method for quantifying Atorvastatin and its impurities, addressing a critical aspect of pharmaceutical analysis. Objective The primary objective is to conduct a comprehensive validation study for the HPLC method, covering specificity assessment, response function establishment, and a detailed analysis of precision, trueness, and tolerance intervals. The emphasis is on demonstrating the method's precision, accuracy, and stability-indicating capabilities across various concentrations and compounds. Methods The HPLC method is validated through rigorous assessments, including specificity, response function establishment, and analyses of precision, trueness, and tolerance intervals. Induced degradation experiments are conducted to explore Atorvastatin's behavior under extreme conditions. Insights into the compound's synthesis and degradation pathways are provided through a proposed mechanism for intramolecular esterification. Results The results affirm the precision, accuracy, and stability-indicating capabilities of the validated HPLC method. The method effectively differentiates between Atorvastatin and its impurities, showcasing its suitability for pharmaceutical quality control. Conclusion The validated HPLC method emerges as a robust and reliable tool for Atorvastatin analysis, contributing significantly to pharmaceutical research and quality control. Its application ensures the safety and efficacy of medications, reinforcing its role in pharmaceutical analysis. Highlights This study not only validates a crucial HPLC method for Atorvastatin analysis but also provides insights into the compound's behavior under extreme conditions and its synthesis and degradation pathways. The validated method serves as a cornerstone in pharmaceutical research and quality control, ensuring medication safety and efficacy.
    Type of Medium: Online Resource
    ISSN: 1060-3271 , 1944-7922
    Language: English
    Publisher: Oxford University Press (OUP)
    Publication Date: 2024
    detail.hit.zdb_id: 2049936-X
    detail.hit.zdb_id: 1103149-9
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  • 2
    In: Methods and Objects of Chemical Analysis, Taras Shevchenko National University of Kyiv, Vol. 18, No. 3 ( 2023), p. 152-159
    Abstract: Chemicals with high manufacturing volumes, such as bisphenol A (BPA), find widespread use in thermal paper, epoxy resins, and polycarbonate plastics. However, due to its endocrine-disrupting properties, several consumer items have restricted or banned its use. As a result, BPA has been replaced by other chemical substances with similar structures in consumer goods. This study aims to enhance and validate a chromatographic method for detecting BPA in baby bottles using chemometrics tools. A Box-Behnken experimental design was employed to optimize the laboratory conditions for the maximum release of BPA through forced degradation. The study utilized three parameters as independent variables, including incubation temperature (35°C, 40°C, and 60°C), time (12 hours, 24 hours, and 36 hours), and solvent acetic acid concentration (2%, 3%, and 4%). A second-order polynomial model was proposed, and a total of 15 experiments with two replicates were conducted to determine the optimal extraction conditions. The high-performance liquid chromatography (HPLC) partitioning method was used to determine peak areas of the different extracts, serving as responses. By applying the individual desirability approach, the optimal extraction conditions were found to be a temperature of 35 °C, an extraction time of 36 hours, and an acetic acid concentration of 4% (pH = 2.72). The method was validated according to the conditions recommended by the International Conference on Harmonization (ICH) and SFSTP (Société Française des Sciences et Techniques Pharmaceutiques), ensuring high linearity, accuracy, precision, sensitivity, and robustness compared to existing liquid chromatographic methods. The improved method was applied to assess BPA levels in commercially available baby bottles, with 3 out of 7 samples testing positive for BPA, ranging from 0.615 ppb to 3.802 ppb. Notably, the enhanced method demonstrated a 12% increase in yield compared to the ISO EN 14350-2:2004 method. This study provides a reliable and effective approach for detecting BPA in baby bottles, addressing critical concerns related to consumer safety and regulatory compliance.
    Type of Medium: Online Resource
    ISSN: 1991-0290 , 2413-6166
    URL: Issue
    Language: Unknown
    Publisher: Taras Shevchenko National University of Kyiv
    Publication Date: 2023
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  • 3
    In: Methods and Objects of Chemical Analysis, Taras Shevchenko National University of Kyiv, Vol. 18, No. 3 ( 2023), p. 160-169
    Abstract: Adulteration of olive oil is a common practice in the industry, where old and commercial oils are mixed with fresh olive oils. Adulteration can negatively affect the quality and authenticity of olive oil, leading to economic fraud and health concerns. Therefore, identifying and quantifying adulteration in olive oil is crucial for ensuring product quality and consumer protection. The objective of this study was to identify and measure the adulteration of fresh olive oils with old oil and commercial oil from the previous harvest year. The study aimed to achieve this goal using spectroscopic techniques in combination with chemometrics. Different spectroscopic techniques, such as FT-MIR and UV-vis spectroscopy, were utilized in this study. Partial least squares (PLS) regression was applied to predict the levels of adulteration in the samples with varying concentrations (0.84 - 52.13 % w/w). Various pre-treatment methods were employed for both FTMIR and UV-Vis spectral data. All the PLS models generated for FT-MIR and UV-Vis spectral data were successful in predicting the levels of adulteration, with high coefficients of determination for both calibration (0.963 - 0.995) and cross validation (0.935 - 0.993) models. The error values for calibration (0.621 % - 2.728 %) and cross validation (0.730 % - 3.314 %) were also low. Based on the results, it was found that the use of second derivative preprocessing for FT-MIR data and SNV preprocessing for UV-Vis data led to the best performance results in quantifying the level of adulteration of olive oil. Spectroscopic techniques in combination with chemometrics can be used to identify and measure the adulteration of olive oil.
    Type of Medium: Online Resource
    ISSN: 1991-0290 , 2413-6166
    URL: Issue
    Language: Unknown
    Publisher: Taras Shevchenko National University of Kyiv
    Publication Date: 2023
    Location Call Number Limitation Availability
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  • 4
    In: Methods and Objects of Chemical Analysis, Taras Shevchenko National University of Kyiv, Vol. 18, No. 1 ( 2023), p. 42-50
    Abstract: Artemisinin-based combination therapy (ACTs) has become the primary first-line treatment for mild falciparum malaria in the majority of African countries. A fixed-dose combination of amodiaquine and artesunate is commonly employed to enhance treatment compliance and achieve successful malaria outcomes. In this study, a specific, accurate, linear, precise, and repeatable method was optimized, verified, and applied for the simultaneous estimation of artesunate and amodiaquine HCl in a commercially available artesunate-amodiaquine tablet with a dosage of 100 mg/270 mg. The optimization process involved two steps. Firstly, the top three were carefully selected out of seven characteristics influencing the separation. These key elements required fine-tuning, namely the column type, ion pair, and the residual amount of acetonitrile (ACN) remaining after elution. In the second step, a Box-Behnken experimental design, coupled with Derrenguer's desirability approach, was utilized to identify the ideal target conditions. The optimized method demonstrated excellent specificity, accuracy, linearity, precision, and repeatability, allowing for the reliable simultaneous estimation of artesunate and amodiaquine HCl in the artesunate-amodiaquine tablet. This method offers a valuable tool for quality control and dosage determination in the pharmaceutical industry. By employing advanced experimental techniques and focusing on critical parameters, the study contributes to analytical methodologies in malaria treatment.
    Type of Medium: Online Resource
    ISSN: 1991-0290 , 2413-6166
    URL: Issue
    Language: Unknown
    Publisher: Taras Shevchenko National University of Kyiv
    Publication Date: 2023
    Location Call Number Limitation Availability
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  • 5
    In: Journal of AOAC International, Oxford University Press (OUP), Vol. 106, No. 6 ( 2023-11-02), p. 1443-1454
    Abstract: Monitoring impurities in drug products is a principal requirement of pharmaceutical regulatory authorities all over the world to ensure drug safety. For this reason, there is a great need for analytical QC of dugs products. Objective In this study, a simple, efficient, and direct HPLC method was developed for the determination of three impurities of diclofenac. Methods The HPLC method was developed using a mobile phase which consisted of an HPLC grade mixture, acetonitrile–0.01M phosphoric acid adjusted to pH 2.3 (1 + 3, by volume). Results The separation was performed in 15 min. The calibration curves of the three impurities were linear; the correlation coefficients were 0.999 at concentrations of 0.00015–0.003 µg/mL. Conclusion The validation of this method shows that it meets all validation criteria. This shows the reliability of this method for the routine control of diclofenac impurities. Highlights The validation of a robust HPLC method for the determination of diclofenac impurities is of great importance for the pharmaceutical industry to control its products.
    Type of Medium: Online Resource
    ISSN: 1060-3271 , 1944-7922
    Language: English
    Publisher: Oxford University Press (OUP)
    Publication Date: 2023
    detail.hit.zdb_id: 2049936-X
    detail.hit.zdb_id: 1103149-9
    Location Call Number Limitation Availability
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