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New automated and high-throughput quantitative analysis of urinary ketones by multifiber exchange-solid phase microextraction coupled to fast gas chromatography/negative chemical-electron ionization/mass spectrometry.

Pacenti M, Dugheri S, Traldi P, Degli Esposti F, Perchiazzi N, Franchi E, Calamante M, Kikic I, Alessi P, Bonacchi A, Salvadori E, Arcangeli G, Cupelli V - J Autom Methods Manag Chem (2010)

Bottom Line: The present research is focused on automation, miniaturization, and system interaction with high throughput for multiple and specific Direct Immersion-Solid Phase Microextraction/Fast Gas Chromatography analysis of the urinary ketones.The specific Mass Spectrometry instrumentation, capable of supporting such the automated changeover from Negative Chemical to Electron Ionization mode, as well as the automation of the preparation procedure by new device called MultiFiber Exchange, through change of the fibers, allowed a friendly use of mass spectrometry apparatus with a number of advantages including reduced analyst time and greater reproducibility (2.01-5.32%).The detection limits for the seven ketones were less than 0.004 mg/L.

View Article: PubMed Central - PubMed

Affiliation: Occupational Health Division, Department of Public Health, Viale Morgagni 48, University of Florence, 50100 Florence, Italy.

ABSTRACT
The present research is focused on automation, miniaturization, and system interaction with high throughput for multiple and specific Direct Immersion-Solid Phase Microextraction/Fast Gas Chromatography analysis of the urinary ketones. The specific Mass Spectrometry instrumentation, capable of supporting such the automated changeover from Negative Chemical to Electron Ionization mode, as well as the automation of the preparation procedure by new device called MultiFiber Exchange, through change of the fibers, allowed a friendly use of mass spectrometry apparatus with a number of advantages including reduced analyst time and greater reproducibility (2.01-5.32%). The detection limits for the seven ketones were less than 0.004 mg/L. For an innovative powerful meaning in high-throughput routine, the generality of the structurally informative Mass Spectrometry fragmentation patterns together with the chromatographic separation and software automation are also investigated.

No MeSH data available.


Related in: MedlinePlus

Fast GC/MS chromatogram of the BOHO-/AcAc-TBDMS by EI mode.
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fig6: Fast GC/MS chromatogram of the BOHO-/AcAc-TBDMS by EI mode.

Mentions: (2)t=x22D for high-throughput analysis 2 mL vial was used instead of 10 mL vial [37]. For on-fiber derivatization low and high values for three variables (20–100 μL MTBSTFA, 25–50°C, and 10–60 minutes) were selected on the basis of previously reported results [38]. The volume of MTBSTFA and the derivatization time did not show significant effects and so they were fixed to 20 μL and 15 minutes, respectively. In order to avoid contamination problems between consecutive samples, on-fiber derivatization was performed in different 2 mL vials and the fibers were additionally desorbed after the analysis during 1 minute at 300°C. In spite of these slow kinetics rates, the extraction and derivatization time were limited to 15 minutes to speed up sample preparation (Figure 6). Obviously, the corresponding decrease in the sensitivity of the method was assumed.


New automated and high-throughput quantitative analysis of urinary ketones by multifiber exchange-solid phase microextraction coupled to fast gas chromatography/negative chemical-electron ionization/mass spectrometry.

Pacenti M, Dugheri S, Traldi P, Degli Esposti F, Perchiazzi N, Franchi E, Calamante M, Kikic I, Alessi P, Bonacchi A, Salvadori E, Arcangeli G, Cupelli V - J Autom Methods Manag Chem (2010)

Fast GC/MS chromatogram of the BOHO-/AcAc-TBDMS by EI mode.
© Copyright Policy - open-access
Related In: Results  -  Collection

Show All Figures
getmorefigures.php?uid=PMC2902044&req=5

fig6: Fast GC/MS chromatogram of the BOHO-/AcAc-TBDMS by EI mode.
Mentions: (2)t=x22D for high-throughput analysis 2 mL vial was used instead of 10 mL vial [37]. For on-fiber derivatization low and high values for three variables (20–100 μL MTBSTFA, 25–50°C, and 10–60 minutes) were selected on the basis of previously reported results [38]. The volume of MTBSTFA and the derivatization time did not show significant effects and so they were fixed to 20 μL and 15 minutes, respectively. In order to avoid contamination problems between consecutive samples, on-fiber derivatization was performed in different 2 mL vials and the fibers were additionally desorbed after the analysis during 1 minute at 300°C. In spite of these slow kinetics rates, the extraction and derivatization time were limited to 15 minutes to speed up sample preparation (Figure 6). Obviously, the corresponding decrease in the sensitivity of the method was assumed.

Bottom Line: The present research is focused on automation, miniaturization, and system interaction with high throughput for multiple and specific Direct Immersion-Solid Phase Microextraction/Fast Gas Chromatography analysis of the urinary ketones.The specific Mass Spectrometry instrumentation, capable of supporting such the automated changeover from Negative Chemical to Electron Ionization mode, as well as the automation of the preparation procedure by new device called MultiFiber Exchange, through change of the fibers, allowed a friendly use of mass spectrometry apparatus with a number of advantages including reduced analyst time and greater reproducibility (2.01-5.32%).The detection limits for the seven ketones were less than 0.004 mg/L.

View Article: PubMed Central - PubMed

Affiliation: Occupational Health Division, Department of Public Health, Viale Morgagni 48, University of Florence, 50100 Florence, Italy.

ABSTRACT
The present research is focused on automation, miniaturization, and system interaction with high throughput for multiple and specific Direct Immersion-Solid Phase Microextraction/Fast Gas Chromatography analysis of the urinary ketones. The specific Mass Spectrometry instrumentation, capable of supporting such the automated changeover from Negative Chemical to Electron Ionization mode, as well as the automation of the preparation procedure by new device called MultiFiber Exchange, through change of the fibers, allowed a friendly use of mass spectrometry apparatus with a number of advantages including reduced analyst time and greater reproducibility (2.01-5.32%). The detection limits for the seven ketones were less than 0.004 mg/L. For an innovative powerful meaning in high-throughput routine, the generality of the structurally informative Mass Spectrometry fragmentation patterns together with the chromatographic separation and software automation are also investigated.

No MeSH data available.


Related in: MedlinePlus