Validation issues arising from the new FDA guidance for industry on bioanalytical method validation

Brodie, R.R.; Hill, Howard

doi:10.1007/bf02493361

Cited by 42 publications

(20 citation statements)

References 3 publications

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“…Full validation of the analytical methods described in this report was performed in line with US Food and Drug Administration guidelines for validation of bioanalytical methods [11], including tests for selectivity, calibration curve, lower limit of quantfication (LLOQ), accuracy, precision and stability.…”

Section: Methods Validationmentioning

confidence: 99%

LC–MS–MS Quantitative Determination of Brivudine in Human Plasma and Its Application to Pharmacokinetic Studies

PeiShan¹,

Chen²,

FanWei³

2011

Chromatographia

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A sensitive and specific liquid chromatography-electrospray ionization-tandem mass spectrometry method has been developed and validated for the identification and quantification of brivudine in human plasma using diclofenac as an internal standard. The method involves extraction with ethyl acetate. The analyte was separated on a C 18 column and analyzed in multiple reaction monitoring mode with a negative electrospray ionization interface using the [M-H] -ions, m/z 332.8? m/z 80.9 for brivudine, m/z 293.6?m/z 249.5 for diclofenac. The method was validated over the concentration range of 5.54-2,836 lg L -1 for brivudine. The intra-and inter-day precisions were less than 8.91% in terms of relative standard deviation (RSD), and the accuracy was within -4.22% in terms of relative error (RE). The lower limit of quantification (LLOQ) was 5.54 lg L -1 with acceptable precision and accuracy. There were almost no matrix effects. Recovery of brivudine spiked in drug-free plasma was higher than 77.17%. The method was used to study the pharmacokinetic profile of brivudine in human plasma after oral administration of brivudine tablets.

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Section: Methods Validationmentioning

confidence: 99%

LC–MS–MS Quantitative Determination of Brivudine in Human Plasma and Its Application to Pharmacokinetic Studies

PeiShan¹,

Chen²,

FanWei³

2011

Chromatographia

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“…Therefore, a series of decreasing MEA concentrations were tested. The LOD was defined to correspond to the lowest concentration with S/N higher than 3 while LOQ was the lowest concentration with an S/N higher than 10 and an acceptable accuracy ranged between ±20% and the acceptable precision was <20% . The linearity within a range of MEA concentrations (0.5, 1, 5, 20, 50, and 80 μg/mL) was assessed using the correlation coefficient R 2 .…”

Section: Methodsmentioning

confidence: 99%

A simple gas chromatography method for the analysis of monoethanolamine in air

Gerster

Hopf²,

Huynh³

et al. 2012

J of Separation Science

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A simple method determining airborne monoethanolamine has been developed. Monoethanolamine determination has traditionally been difficult due to analytical separation problems. Even in recent sophisticated methods, this difficulty remains as the major issue often resulting in time-consuming sample preparations. Impregnated glass fiber filters were used for sampling. Desorption of monoethanolamine was followed by capillary GC analysis and nitrogen phosphorous selective detection. Separation was achieved using a specific column for monoethanolamines (35% diphenyl and 65% dimethyl polysiloxane). The internal standard was quinoline. Derivatization steps were not needed. The calibration range was 0.5-80 μg/mL with a good correlation (R(2) = 0.996). Averaged overall precisions and accuracies were 4.8% and -7.8% for intraday (n = 30), and 10.5% and -5.9% for interday (n = 72). Mean recovery from spiked filters was 92.8% for the intraday variation, and 94.1% for the interday variation. Monoethanolamine on stored spiked filters was stable for at least 4 weeks at 5°C. This newly developed method was used among professional cleaners and air concentrations (n = 4) were 0.42 and 0.17 mg/m(3) for personal and 0.23 and 0.43 mg/m(3) for stationary measurements. The monoethanolamine air concentration method described here was simple, sensitive, and convenient both in terms of sampling and analytical analysis.

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“…For all the concentration levels of letosteine, the result was within the requirements of the guidelines for bioanalytical methods [14].…”

Section: Precision and Accuracymentioning

confidence: 99%

Development of a novel LC–MS/MS method for the determination of letosteine in human plasma and its application on pharmacokinetic studies

Liu

Zheng

Tang

et al. 2011

Journal of Chromatography B

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Validation issues arising from the new FDA guidance for industry on bioanalytical method validation

Cited by 42 publications

References 3 publications

LC–MS–MS Quantitative Determination of Brivudine in Human Plasma and Its Application to Pharmacokinetic Studies

LC–MS–MS Quantitative Determination of Brivudine in Human Plasma and Its Application to Pharmacokinetic Studies

A simple gas chromatography method for the analysis of monoethanolamine in air

Development of a novel LC–MS/MS method for the determination of letosteine in human plasma and its application on pharmacokinetic studies

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