An analysis of the SFSTP guide on validation of chromatographic bioanalytical methods: progresses and limitations

Boulanger, Bruno; Chiap, Patrice; Dewé, Walthère; Crommen, Jacques; Hubert, Philippe

doi:10.1016/s0731-7085(03)00182-1

Cited by 145 publications

(101 citation statements)

References 10 publications

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“…The results are shown in table 2. The precision results indicate that the current method was reliable and repeatable [23]. Thus, the methodology can be applied for the determination of drug in different formulations like targeting of pancreatic as well as for bladder cancer.…”

Section: Interday Precisionmentioning

confidence: 65%

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Development and Validation of Uv-Spectrophotometric Methods for Determination of Gemcitabine Hydrochloride in Bulk and Polymeric Nanoparticles

Kaur

2017

Int J App Pharm

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Objective: The objective of the present work was to develop and validate a novel, specific, precise and reliable method for estimation of gemcitabine hydrochloride in bulk and polymeric nanoparticles using UV-visible spectroscopy method. Methods:The UV-Visible spectrophotometric determination was performed with double beam Systronics UV-visible spectrophotometer; model UV-2201 (India). The proposed methods were validated for various parameters like linearity, precision, accuracy, robustness, ruggedness, detection, quantification limits, and formulation analysis as per international conference on harmonization (ICH) guidelines. Results:The method was based on measurement of absorbance at wavelength maxima i.e. 267.2 nm, λmax of the drug in distilled water, phosphate buffer pH 6.8 and 7.4. The method obeyed Beer Lambert's law in the concentration range of 5-30 µg/ml andR 2 -value was found to be 0.999. Moreover, the % drug recovered from polymeric nanoparticles was found to be 97.97%. Conclusion:According to results, the currently developed method shows compliance with acceptance criteria with Q2 (R1) and international conference on harmonization (2005) guidelines, because the % RSD was found to be less than 2%. The developed method was simple, accurate and précised.

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Section: Interday Precisionmentioning

confidence: 65%

“…The result was indicated as %RSD, which should be less than 2 as shown in table 6. The ruggedness analysis, indicates that there was no significant change in reliability and repeatability of methodology with the change of analyst [23].…”

Section: Ruggedness Studymentioning

confidence: 95%

Development and Validation of Uv-Spectrophotometric Methods for Determination of Gemcitabine Hydrochloride in Bulk and Polymeric Nanoparticles

Kaur

2017

Int J App Pharm

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“…Sendo assim, uma vez otimizados, os procedimentos de análise precisam ser validados segundo critérios estabelecidos na literatura [115][116][117][118][119] . Normalmente, o processo de validação é feito empregando o fármaco na forma de mistura racêmica.…”

Section: Aspectos Relevantes Na Análise Enantiosseletivaunclassified

Análise enantiosseletiva de fármacos: contribuições da cromatografia líquida de alta eficiência e eletroforese capilar

Bonato¹,

Jabor²,

Gaitani³

2005

Quím. Nova

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Recebido em 2/7/04; aceito em 6/10/04; publicado na web em 17/2/05 ENANTIOSELECTIVE ANALYSIS OF DRUGS: CONTRIBUTIONS OF HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY AND CAPILLARY ELECTROPHORESIS. The demand for analytical methods suitable for accurate and reproducible determination of drug enantiomers has increased significantly in the last years. High-performance liquid chromatography (HPLC) using chiral stationary phases and capillary electrophoresis (CE) are the most important techniques used for this purpose. In this paper, the fundamental aspects of chiral separations using both techniques are presented. Some important aspects for the development of enantioselective methods, particularly for the analysis of drugs and metabolites in biological samples, are also discussed.Keywords: chiral drugs; high-performance liquid chromatography; capillary electrophoresis. INTRODUÇÃOPor razões econômicas e dificuldades de ordem prática nos processos de produção, a maioria dos fármacos quirais obtidos por vias sintéticas é comercializada como racemato, ou seja, mistura contendo quantidades iguais dos dois enantiômeros 1 . No entanto, existem inúmeros exemplos de fármacos que apresentam atividades farmacológicas estereosseletivas (propriedades farmacodinâmicas), conseqüência de interações com receptores biológi-cos, que são altamente específicas 2 . Um exemplo clássico que não pode ser esquecido é o da talidomida. Somente depois das investigações da contribuição das propriedades estereosseletivas desse fármaco, é que foi possível estabelecer que as propriedades teratogênicas da talidomida, que causaram deformidades físicas em recém nascidos cujas mães fizeram uso desse fármaco durante a gravidez, estavam relacionadas com o enantiômero (-)-(S)-3 . Infelizmente, em estudos posteriores foi constatada a inversão de configuração não apenas in vitro mas também in vivo da talidomida 4,5 , evidenciando que se o enantiômero (+)-(R)-puro tivesse sido administrado, teria sido parcialmente convertido no isômero responsável pelo efeito teratogênico. Exemplos menos drásticos que esse são bastante comuns, nos quais as diferenças existentes entre os dois enantiômeros podem ser qualitativas ou quantitativas, sendo que, nesse último caso, o enantiômero mais ativo é chamado de eutômero enquanto que ao outro dá-se o nome de distômero 6 . Estudos têm mostrado que β-bloqueadores, propranolol é um exemplo, se ligam estereosseletivamente a receptores β-adrenérgicos e que os enantiômeros (-)-são os principais responsáveis pela atividade β-bloqueadora dessa classe de fármacos 7 . Adicionalmente, quando um fármaco quiral é administrado como racemato, os dois enantiômeros podem apresentar os processos de absorção, distribuição, metabolização e excreção (disposição cinética) de forma estereosseletiva [8][9][10][11] . Desses processos, a estereosseletividade é mais significativa no metabolismo, devido ao envolvimento do sistema enzimático. Dentre os inúmeros exemplos, pode-se destacar o verapamil; o enantiômero ativo (-)-(S) é preferencialmente metabolizado ...

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“…A slight constant carry over effect was still observed, being <0.3% for both substances after analysis of a plasma sample spiked with 50 ng ml −1 of CPA and 2.5 ng ml −1 of MPA. [25][26][27] The validation results of the response function are presented in Table 1. A weighted linear regression (1/X 2 ) with Table 1 Validation results six concentration levels was used and its goodness of fit is illustrated in Fig.…”

Section: Selectivitymentioning

confidence: 99%

“…A novel approach based on the accuracy profile as decision tool has been used for the validation of the present method [25,26]. By this approach, using two-sided 95% ␤-expectation tolerance intervals for the total measurement error, the performance of the procedure can be better visualized.…”

Section: Introductionmentioning

confidence: 99%

Fully automated method for the liquid chromatographic–tandem mass spectrometric determination of cyproterone acetate in human plasma using restricted access material for on-line sample clean-up

Christiaens

Fillet

Chiap

et al. 2004

Journal of Chromatography A

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A new automated method for the quantitative analysis of cyproterone acetate (CPA) in human plasma has been developed using on-line solid phase extraction (SPE) prior to the LC-MS/MS determination. The method was based on the use of a pre-column packed with internal-surface reversed-phase material (LiChrospher RP-4 ADS, 25 mm × 2 mm) for sample clean-up coupled to LC separation on an octadecyl silica stationary phase by means of a column switching system. A 30 l plasma sample volume was injected directly onto the pre-column using a mixture of water, acetonitrile and formic acid (90:10:0.1 (v/v/v)) adjusted to pH 4.0 with diluted ammonia as washing liquid. The analyte was then eluted in the back-flush mode with the LC mobile phase consisting of water, methanol and formic acid (10:90:0.1 (v/v/v)). The dispensing flow rates of the washing liquid and the LC mobile phase were 300 l min −1 . Medroxyprogesterone acetate (MPA) was used as internal standard. The MS ionization of the analytes was achieved using electrospray (ESI) in the positive ion mode. The pseudomolecular ionic species of CPA and MPA (417.4 and 387.5) were selected to generate daughter ions at 357.4 and 327.5, respectively. Finally, the developed method was validated according to a new approach using accuracy profiles as a decision tool. Very good results with respect to accuracy, detectability, repeatability, intermediate precision and selectivity were obtained. The LOQ of cyproterone acetate was 300 pg ml −1 .

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An analysis of the SFSTP guide on validation of chromatographic bioanalytical methods: progresses and limitations

Cited by 145 publications

References 10 publications

Development and Validation of Uv-Spectrophotometric Methods for Determination of Gemcitabine Hydrochloride in Bulk and Polymeric Nanoparticles

Development and Validation of Uv-Spectrophotometric Methods for Determination of Gemcitabine Hydrochloride in Bulk and Polymeric Nanoparticles

Análise enantiosseletiva de fármacos: contribuições da cromatografia líquida de alta eficiência e eletroforese capilar

Fully automated method for the liquid chromatographic–tandem mass spectrometric determination of cyproterone acetate in human plasma using restricted access material for on-line sample clean-up

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