Microfluidic direct injection method for analysis of urinary 4-(methylnitrosamino)-1-(3-pyridyl)-1-butanol (NNAL) using molecularly imprinted polymers coupled on-line with LC–MS/MS

The work described in this paper involves development of a high-throughput on-line microfluidic sample extraction method using capillary micro-columns packed with MIP beads coupled with tandem mass spectrometry for the analysis of urinary NNAL. The method was optimized and matrix effects were evalua...

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Veröffentlicht in:Journal of pharmaceutical and biomedical analysis 2011-01, Vol.54 (2), p.368-378
Hauptverfasser: Shah, Kumar A., Peoples, Michael C., Halquist, Matthew S., Rutan, Sarah C., Karnes, H. Thomas
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container_end_page 378
container_issue 2
container_start_page 368
container_title Journal of pharmaceutical and biomedical analysis
container_volume 54
creator Shah, Kumar A.
Peoples, Michael C.
Halquist, Matthew S.
Rutan, Sarah C.
Karnes, H. Thomas
description The work described in this paper involves development of a high-throughput on-line microfluidic sample extraction method using capillary micro-columns packed with MIP beads coupled with tandem mass spectrometry for the analysis of urinary NNAL. The method was optimized and matrix effects were evaluated and resolved. The method enabled low sample volume (200 μL) and rapid analysis of urinary NNAL by direct injection onto the microfluidic column packed with molecularly imprinted beads engineered to NNAL. The method was validated according to the FDA bioanalytical method validation guidance. The dynamic range extended from 20.0 to 2500.0 pg/mL with a percent relative error of ±5.9% and a run time of 7.00 min. The lower limit of quantitation was 20.0 pg/mL. The method was used for the analysis of NNAL and NNAL–Gluc concentrations in smokers’ urine.
doi_str_mv 10.1016/j.jpba.2010.09.001
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Psychology</subject><subject>General pharmacology</subject><subject>Glucuronates - urine</subject><subject>Humans</subject><subject>LC–MS/MS</subject><subject>Male</subject><subject>Medical sciences</subject><subject>Microfluidics - methods</subject><subject>Middle Aged</subject><subject>Molecular Imprinting</subject><subject>Molecular Structure</subject><subject>Molecular Weight</subject><subject>Molecularly imprinted polymer</subject><subject>Nitrosamines - urine</subject><subject>NNAL</subject><subject>On-line microfluidic solid phase extraction</subject><subject>Online Systems</subject><subject>Pharmacology. 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source MEDLINE; ScienceDirect Journals (5 years ago - present)
subjects Adult
Analysis
Analytical, structural and metabolic biochemistry
Biological and medical sciences
Butanols - urine
Calibration
Chromatography, Liquid - methods
Female
Fundamental and applied biological sciences. Psychology
General pharmacology
Glucuronates - urine
Humans
LC–MS/MS
Male
Medical sciences
Microfluidics - methods
Middle Aged
Molecular Imprinting
Molecular Structure
Molecular Weight
Molecularly imprinted polymer
Nitrosamines - urine
NNAL
On-line microfluidic solid phase extraction
Online Systems
Pharmacology. Drug treatments
polymers
Polymers - chemistry
Pyridines - urine
Quality Control
rapid methods
Reference Standards
Reproducibility of Results
tandem mass spectrometry
Tandem Mass Spectrometry - methods
Time Factors
Tobacco specific nitrosamine
urine
title Microfluidic direct injection method for analysis of urinary 4-(methylnitrosamino)-1-(3-pyridyl)-1-butanol (NNAL) using molecularly imprinted polymers coupled on-line with LC–MS/MS
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