Abstract
A sensitive, accurate and reproducible procedure has been developed for the quantitative determination of gemcitabine (2′,2′ -difluorodeoxycytidine, dFdC) and its metabolite 2′,2′ -difluorodeoxyuridine (2dFdU) in human urine. The samples (2 mL) were extracted by solid-phase extraction (SPE) and analyzed by reversed-phase high-performance liquid chromatography coupled with tandem mass spectrometry (HPLC/MS/MS), operating in multiple reaction monitoring (MRM mode). This procedure was validated using 2′-deoxycytidine as internal standard (IS). The urine assay was linear over the range 0-50 μg/L, with a limit of quantification (LLOQ) of 0.2 μg/L for gemcitabine and 1.0 μg/L for the metabolite. The respective limits of detection (LODs) for dFdC and 2dFdU were 0.05 and 0.3 μg/L. The precision and accuracy of the assay were determined on three different days. The within-series precision was found to be always less than 8. 5 and 12.7% for gemcitabine and 2dFdU, respectively. The overall precision expressed as relative standard deviation (CVr) was always less than 7.1% for both analytes. The recovery of gemcitabine was always greater than 90% with a CVr
| Original language | English |
|---|---|
| Pages (from-to) | 1017-1023 |
| Number of pages | 7 |
| Journal | Rapid Communications in Mass Spectrometry |
| Volume | 18 |
| Issue number | 10 |
| Publication status | Published - 2004 |
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ASJC Scopus subject areas
- Analytical Chemistry
- Spectroscopy
Cite this
Validated procedure for simultaneous trace level determination of the anti-cancer agent gemcitabine and its metabolite in human urine by high-performance liquid chromatography with tandem mass spectrometry. / Sottani, Cristina; Zucchetti, Massimo; Zaffaroni, Marco; Bettinelli, Maurizio; Minoia, Claudio.
In: Rapid Communications in Mass Spectrometry, Vol. 18, No. 10, 2004, p. 1017-1023.Research output: Contribution to journal › Article
}
TY - JOUR
T1 - Validated procedure for simultaneous trace level determination of the anti-cancer agent gemcitabine and its metabolite in human urine by high-performance liquid chromatography with tandem mass spectrometry
AU - Sottani, Cristina
AU - Zucchetti, Massimo
AU - Zaffaroni, Marco
AU - Bettinelli, Maurizio
AU - Minoia, Claudio
PY - 2004
Y1 - 2004
N2 - A sensitive, accurate and reproducible procedure has been developed for the quantitative determination of gemcitabine (2′,2′ -difluorodeoxycytidine, dFdC) and its metabolite 2′,2′ -difluorodeoxyuridine (2dFdU) in human urine. The samples (2 mL) were extracted by solid-phase extraction (SPE) and analyzed by reversed-phase high-performance liquid chromatography coupled with tandem mass spectrometry (HPLC/MS/MS), operating in multiple reaction monitoring (MRM mode). This procedure was validated using 2′-deoxycytidine as internal standard (IS). The urine assay was linear over the range 0-50 μg/L, with a limit of quantification (LLOQ) of 0.2 μg/L for gemcitabine and 1.0 μg/L for the metabolite. The respective limits of detection (LODs) for dFdC and 2dFdU were 0.05 and 0.3 μg/L. The precision and accuracy of the assay were determined on three different days. The within-series precision was found to be always less than 8. 5 and 12.7% for gemcitabine and 2dFdU, respectively. The overall precision expressed as relative standard deviation (CVr) was always less than 7.1% for both analytes. The recovery of gemcitabine was always greater than 90% with a CVr
AB - A sensitive, accurate and reproducible procedure has been developed for the quantitative determination of gemcitabine (2′,2′ -difluorodeoxycytidine, dFdC) and its metabolite 2′,2′ -difluorodeoxyuridine (2dFdU) in human urine. The samples (2 mL) were extracted by solid-phase extraction (SPE) and analyzed by reversed-phase high-performance liquid chromatography coupled with tandem mass spectrometry (HPLC/MS/MS), operating in multiple reaction monitoring (MRM mode). This procedure was validated using 2′-deoxycytidine as internal standard (IS). The urine assay was linear over the range 0-50 μg/L, with a limit of quantification (LLOQ) of 0.2 μg/L for gemcitabine and 1.0 μg/L for the metabolite. The respective limits of detection (LODs) for dFdC and 2dFdU were 0.05 and 0.3 μg/L. The precision and accuracy of the assay were determined on three different days. The within-series precision was found to be always less than 8. 5 and 12.7% for gemcitabine and 2dFdU, respectively. The overall precision expressed as relative standard deviation (CVr) was always less than 7.1% for both analytes. The recovery of gemcitabine was always greater than 90% with a CVr
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M3 - Article
C2 - 15150823
AN - SCOPUS:2542457707
VL - 18
SP - 1017
EP - 1023
JO - Rapid Communications in Mass Spectrometry
JF - Rapid Communications in Mass Spectrometry
SN - 0951-4198
IS - 10
ER -