Comparative assessment of bioanalytical method validation guidelines for pharmaceutical industry

Kadian, Naveen; Raju, K. Kanaka; Rashid, Mamunur; Malik, Monika; Taneja, Isha; Wahajuddin, Muhammad

doi:10.1016/j.jpba.2016.03.052

Cited by 136 publications

(76 citation statements)

References 19 publications

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“…The accuracy was within ±2.55% of the nominal value at each concentration level. According to the United States Food and Drug Administration and European Medical Agency guidelines , all the results were within the acceptable criteria ranges, indicating that the bioanalytical method was accurate, reproducible, and reliable.…”

Section: Resultsmentioning

confidence: 85%

A sensitive, high‐throughput, and ecofriendly method for the determination of lumefantrine, artemether, and its active metabolite dihydroartemisinin by supercritical fluid chromatography and tandem mass spectrometry

Yang

Gao

Hou

et al. 2018

J of Separation Science

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A quick and sensitive supercritical fluid chromatography with tandem mass spectrometry method for the simultaneous determination of lumefantrine, artemether, and its active metabolite dihydroartemisinin in rat plasma was developed and validated. The chromatographic separation was performed on an ACQUITY UPC ™ BEH 2-EP column within 2.5 min by gradient elution using compressed CO and methanol containing 2 mM ammonium acetate as the mobile phases. Detection was achieved by multiple reaction monitoring using electrospray ionization in the positive ionization mode. For sample preparation, 50 μL of the sample was processed by modified high-throughput, one-step protein precipitation using hydrogen peroxide as a stabilizer to protect the endoperoxide-containing artemisinin derivatives from degradation. The calibration curves were linear over the concentration range of 2.0-1000 ng/mL for both artemether and dihydroartemisinin, and 1.0-5000 ng/mL for lumefantrine. The values of selectivity, lower limit of quantification, linearity, accuracy, precision, matrix effects, stability, and recovery met the acceptable range according to the Food and Drug Administration guidelines. The developed method enables high resolution and speed as well as low cost, low solvent consumption, and short time and was successfully applied to pharmacokinetic studies through the intravenous administration of an artemether-lumefantrine lipid emulsion in rats.

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Section: Resultsmentioning

confidence: 85%

A sensitive, high‐throughput, and ecofriendly method for the determination of lumefantrine, artemether, and its active metabolite dihydroartemisinin by supercritical fluid chromatography and tandem mass spectrometry

Yang

Gao

Hou

et al. 2018

J of Separation Science

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“…The precision of the bioanalytical method was considered in terms of repeatability (intraday tests, n = 6) and intermediate precision (interday tests, n = 3) using spiked human plasma samples. The precision and accuracy results obtained were expressed in terms of the relative standard deviation (RSD %) and relative error (RE %), respectively . The stability studies of ARVs included: influence of freezing (−20°C) and thawing cycles (25 ± 3°C), short‐term temperature (12 h on the bench) and long‐term storage at −20°C (two and four days).…”

Section: Methodsmentioning

confidence: 99%

Hollow mesoporous structured molecularly imprinted polymer as adsorbent in pipette‐tip solid‐phase extraction for the determination of antiretrovirals from plasma of HIV‐infected patients

et al. 2018

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In this work a hollow mesoporous structured molecularly imprinted polymer was synthetized and used as adsorbent in pipette-tip solid-phase extraction for the determination of lamivudine (3TC), zidovudine (AZT) and efavirenz (EFZ) from plasma of human immunodeficiency virus (HIV) infected patients by high-performance liquid chromatography (HPLC). All parameters that influence the recovery of the pipette tip based on hollow mesoporous molecularly imprinted polymer solid-phase extraction (PT-HM-MIP-SPE) method were systematically studied and discussed in detail. The adsorbent material was prepared using methacrylic acid and 4-vinylpyridine as functional monomers, ethylene glycol dimethacrylate as crosslinker, acetonitrile as solvent, 4,4'-azobis(4-cyanovaleric acid) as radical initiator, benzalkonium chloride as surfactant, 3TC, and AZT as templates. The simultaneous separation of 3TC, AZT and EFZ by HPLC-UV was performed using a Gemini C18 Phenomenex® column (250 mm × 4.6 mm, 5 μm) and mobile phase consisting of acetonitrile: water pH 3.2 (68:32, v/v), flow rate of 1.0 mL/min and λ = 260 nm. The method was linear over the concentration range from 0.25 to 10 μg/mL for 3TC and EFZ, and 0.05 to 2.0 μg mL for AZT, with correlation coefficients larger than 0.99 for all analytes. Recovery ± relative standard deviations (RSDs %) were 41.99 ± 2.38%, 82.29 ± 1.63%, and 83.72 ± 7.52% for 3TC, AZT, and EFZ, respectively. The RSDs and relative errors (REs) were lower than 15% for intra and interday assays. The method has been successfully applied for monitoring HIV-infected patients outside the therapeutic dosage.

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“…Method validation and documentation were performed according to guidelines set by the United States Food and Drug Administration (FDA) for bioanalytical method validation [28, 29]. This method was validated for linearity, specificity, intra- and inter-day accuracy and precision, recovery, and stability of the analytes [29, 30].…”

Section: Methodsmentioning

confidence: 99%

“…This method was validated for linearity, specificity, intra- and inter-day accuracy and precision, recovery, and stability of the analytes [29, 30]. Analytical runs included a double blank (without internal standard), a blank (with internal standard), nine calibration standards (0.5 to 1,000 ng/mL), and six sets of QCs: LLOQ QC at 0.5 ng/mL, low QC at 2 ng/mL, medium QCs at 20 and 200 ng/mL, and high QC at 800 ng/mL.…”

Section: Methodsmentioning

confidence: 99%

Development and validation of a sensitive assay for analysis of midazolam, free and conjugated 1-hydroxymidazolam and 4-hydroxymidazolam in pediatric plasma: Application to Pediatric Pharmacokinetic Study

Moorthy

Jogiraju

Vedar

et al. 2017

Journal of Chromatography B

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Pharmacokinetic, pharmacodynamic and pharmacogenomic studies of midazolam are currently being performed in critically ill children to find suitable dose regimens. Sensitive assays using small volumes of plasma are necessary to determine the concentrations of midazolam and its respective metabolites in pediatric studies. Midazolam is metabolized to hydroxylated midazolam isomers, which are present as free as well as the corresponding glucuronide conjugates. A high-performance liquid chromatographic method with tandem mass spectrometry has been developed and validated for the quantification of midazolam, and free and total 1-hydroxymidazolam and 4-hydroxymidazolam metabolites in small volumes of plasma. Cleanup consisted of 96-well µ-elution solid phase extraction (SPE). The analytes were separated by gradient elution using a C18 analytical column with a total run time of 5 min. Multiple reaction monitoring was employed using precursor to product ion transitions of m/z 326.2 →291.3 for midazolam, m/z 342.1 →203.0 for 1-hydroxymidazolam, m/z 342.1 →325.1 for 4-hydroxymidazolam and m/z 330.2 →295.3 for 2H4-midazolam (internal standard). Since authentic hydroxymidazolamglucuronide standards are not available, samples were hydrolyzed with β-glucuronidase under optimized conditions. Assay conditions were modified and optimized to provide appropriate recovery and stability because 4-hydroxymidazolam was very acid sensitive. Standard curves were linear from 0.5 to 1,000 ng/mL for all three analytes. Intra- and inter day accuracy and precision for quality control samples (2, 20, 200 and 800 ng/mL) were within 85–115% and 15% (coefficient of variation), respectively. Stability in plasma and extracts were sufficient under assay conditions. Plasma samples were processed and analyzed for midazolam, and free 1-hydroxymidazolam and 4-hydroxymidazolam metabolites. Plasma samples that were hydrolyzed with β-glucuronidase were processed and analyzed for midazolam, and total 1-hydroxymidazolam and 4-hydroxymidazolam metabolites under the same assay conditions. The difference in concentration between the total and free hydroxymidazolam metabolites provided an estimate of conjugated hydroxymidazolam metabolites. The combination of 96-well µ-elution SPE and LC-MS/MS allows reliable quantification of midazolam and its metabolites in small volumes of plasma for pediatric patients. This assay is currently being successfully utilized for analysis of samples from ongoing clinical trials.

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Comparative assessment of bioanalytical method validation guidelines for pharmaceutical industry

Cited by 136 publications

References 19 publications

A sensitive, high‐throughput, and ecofriendly method for the determination of lumefantrine, artemether, and its active metabolite dihydroartemisinin by supercritical fluid chromatography and tandem mass spectrometry

A sensitive, high‐throughput, and ecofriendly method for the determination of lumefantrine, artemether, and its active metabolite dihydroartemisinin by supercritical fluid chromatography and tandem mass spectrometry

Hollow mesoporous structured molecularly imprinted polymer as adsorbent in pipette‐tip solid‐phase extraction for the determination of antiretrovirals from plasma of HIV‐infected patients

Development and validation of a sensitive assay for analysis of midazolam, free and conjugated 1-hydroxymidazolam and 4-hydroxymidazolam in pediatric plasma: Application to Pediatric Pharmacokinetic Study

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