Analytical Validation of Quantitative High-Performance Liquid Chromatographic Methods in Pharmaceutical Analysis: A Practical Approach

Bonfílio, Rudy; Cazedey, Edith Cristina Laignier; Araújo, Magali Benjamim; Salgado, Hérida Regina Nunes

doi:10.1080/10408347.2012.630926

Cited by 44 publications

(35 citation statements)

References 58 publications

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“…N is the number of design experiments. Both graphical and statistical interpretation methods are described [22,129,132,133] for identifying significant effects.…”

Section: Experimental Design Of Ruggedness/robustness T Experimentalmentioning

confidence: 99%

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Tutorial review on validation of liquid chromatography–mass spectrometry methods: Part I

Kruve

Rebane

Kipper

et al. 2015

Analytica Chimica Acta

243

145

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This is the part I of a tutorial review intending to give an overview of the state of the art of method validation in liquid chromatography mass spectrometry (LC-MS) and discuss specific issues that arise with MS (and MS/MS) detection in LC (as opposed to the "conventional" detectors). The Part I briefly introduces the principles of operation of LC-MS (emphasizing the aspects important from the validation point of view, in particular the ionization process and ionization suppression/enhancement); reviews the main validation guideline documents and discusses in detail the following performance parameters: selectivity/specificity/identity, ruggedness/robustness, limit of detection, limit of quantification, decision limit and detection capability. With every method performance characteristic its essence and terminology are addressed, the current status of treating it is reviewed and recommendations are given, how to determine it, specifically in the case of LC-MS methods.

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“…N is the number of design experiments. Both graphical and statistical interpretation methods are described [22,129,132,133] for identifying significant effects.…”

Section: Experimental Design Of Ruggedness/robustness T Experimentalmentioning

confidence: 99%

“…In the Plackett-Burmann approach, N-1 parameters (variables) are studied in N experimental runs (with N being a multiple of 4) [22,118,130]. The factors are investigated at two levels:…”

Section: Experimental Design Of Ruggedness/robustness T Experimentalmentioning

confidence: 99%

Tutorial review on validation of liquid chromatography–mass spectrometry methods: Part I

Kruve

Rebane

Kipper

et al. 2015

Analytica Chimica Acta

243

145

View full text Add to dashboard Cite

show abstract

“…O desenvolvimento de métodos analíticos envolve a avaliação e otimização de condições, incluindo etapas de preparação da amostra, detecção e quantificação. A validação é necessária para demonstrar, se o método atende às exigências das aplicações analíticas, assegurando a confiabilidade e reprodutibilidade dos resultados obtidos (Swartz et al, 1998;Ribani et al, 2004;Bonfilio et al, 2012).…”

Section: Validação De Métodos Analíticosunclassified

“…Os parâmetros fundamentais de avaliação incluem linearidade, precisão, limites de quantificação e detecção(AOAC, 2010;Ribani et al, 2004;Bonfilio et al, 2012).A linearidade corresponde à capacidade do método em fornecer resultados diretamente proporcionais à concentração da substância em exame, dentro de uma determinada faixa de aplicação. Na maioria das vezes ela é determinada por uma curva analítica de no mínimo cinco pontos, que não incluam o ponto zero na curva, minimizando assim, possíveis erros associados.…”

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Validação de metodologias e determinação da composição de fitosteróis em cremes vegetais, farináceos e cafés comercializados em São Paulo

Akaishi¹

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Determination of phytosterols composition in vegetable creams, farinaceous and coffees commercialized in Sao Paulo. [Dissertation]. Sao Paulo (BR). Public Health School of the University of Sao Paulo; 2014. Introduction: Phytosterols (PS) are plant sterols, known as functional components due to its hypocholesterolemic role. The recommendation for daily intake of these compounds is 1.6-2 g/day, however there are few studies that evaluate the content of these compounds in foods, requiring its quantification. Objective: the objective of this project was to develop a methodology and determine the content of PS in some foods usually consumed and traded in Sao Paulo. Methodology: Were evaluated samples of: unsalted vegetable cream (in natura, and heated to 100 o C and 140 o C), farinaceous: wheat, corn and cassava flour, breadcrumbs and cornstarch, powdered coffee (roasts: traditional, strong and extra strong, decaffeinated and gourmet), instant coffee, cappuccino and strained drink coffee. Samples in triplicate were subjected to cold saponification process and unsaponificable matter was extracted, derivatized and subsequently injected into the gas chromatograph. Results: The main PS founded in the samples were: β-sitosterol, campesterol and stigmasterol. The highest average levels of PS were found in vegetable creams (186.2 ± 21.7 mg / 100g) and powdered coffee (92.24 ± 3.95 mg / 100g). Farinaceous had intermediate levels, 42.

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Development and optimization of SPE-HPLC-UV/ELSD for simultaneous determination of nine bioactive components in Shenqi Fuzheng Injection based on Quality by Design principles

Wang

2016

Anal Bioanal Chem

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A method combining solid phase extraction, high performance liquid chromatography, and ultraviolet/evaporative light scattering detection (SPE-HPLC-UV/ELSD) was developed according to Quality by Design (QbD) principles and used to assay nine bioactive compounds within a botanical drug, Shenqi Fuzheng Injection. Risk assessment and a Plackett-Burman design were utilized to evaluate the impact of 11 factors on the resolutions and signal-to-noise of chromatographic peaks. Multiple regression and Pareto ranking analysis indicated that the sorbent mass, sample volume, flow rate, column temperature, evaporator temperature, and gas flow rate were statistically significant (p < 0.05) in this procedure. Furthermore, a Box-Behnken design combined with response surface analysis was employed to study the relationships between the quality of SPE-HPLC-UV/ELSD analysis and four significant factors, i.e., flow rate, column temperature, evaporator temperature, and gas flow rate. An analytical design space of SPE-HPLC-UV/ELSD was then constructed by calculated Monte Carlo probability. In the presented approach, the operating parameters of sample preparation, chromatographic separation, and compound detection were investigated simultaneously. Eight terms of method validation, i.e., system-suitability tests, method robustness/ruggedness, sensitivity, precision, repeatability, linearity, accuracy, and stability, were accomplished at a selected working point. These results revealed that the QbD principles were suitable in the development of analytical procedures for samples in complex matrices. Meanwhile, the analytical quality and method robustness were validated by the analytical design space. The presented strategy provides a tutorial on the development of a robust QbD-compliant quantitative method for samples in complex matrices.

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Analytical Validation of Quantitative High-Performance Liquid Chromatographic Methods in Pharmaceutical Analysis: A Practical Approach

Cited by 44 publications

References 58 publications

Tutorial review on validation of liquid chromatography–mass spectrometry methods: Part I

Tutorial review on validation of liquid chromatography–mass spectrometry methods: Part I

Validação de metodologias e determinação da composição de fitosteróis em cremes vegetais, farináceos e cafés comercializados em São Paulo

Development and optimization of SPE-HPLC-UV/ELSD for simultaneous determination of nine bioactive components in Shenqi Fuzheng Injection based on Quality by Design principles

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