A new issue of this journal has just been published. To see abstracts of the papers it contains (with links through to the full papers) click here:
Journal of Chromatography B
http://rss.sciencedirect.com/publication/science/7220
http://rss.sciencedirect.com/publication/science/7220
Selected papers from the latest issue:
LC-ESI-MS/MS determination of in vivo metabolites of almotriptan in rat plasma, urine and feces: Application to pharmacokinetics
Publication year: 2012
Source: Journal of Chromatography B, Available online 20 February 2012
R. Nageswara Rao, K. Guruprasad, Ch. Gangu Naidu, B. Raju, R. Srinivas
A highly sensitive and specific liquid chromatography-electrospray ionization tandem mass spectrometric (LC-ESI-MS/MS) method for investigating the in vivo metabolites of almotriptan in rat plasma, feces and urine was developed. Chromatographic separation was achieved on a Lichrospher RP-18 column (250 × 4.6 mm, 5 μm), using 20 mM ammonium acetate (pH 3.5) and acetonitrile (60:40 v/v) as a mobile phase at 25 °C. MS/MS detection was performed by positive ion electrospray ionization using target ions atm/z336 [M + H], m/z368 &m/z282 [M + H]for almotriptan and its two metabolites, respectively. Two metabolitesviz., γ-aminobutyric acid and sulphonamide were detected in plasma as well as feces after 24 h of oral administration of almotriptan, while only γ-aminobutyric acid was found in urine. The method was sensitive with a lower limit of quantification of 1.43 ng/mL and linear over the range of 1.43-5000 ng/mL in plasma. The method was validated and successfully applied to a pharmacokinetic study of almotriptan in rat plasma using sumatriptan as an internal standard. The peak plasma concentration (Cmax) after 0.3 h of 5 mg/kg oral dose of almotriptan was determined to be 69.85 ng/mL.
Source: Journal of Chromatography B, Available online 20 February 2012
R. Nageswara Rao, K. Guruprasad, Ch. Gangu Naidu, B. Raju, R. Srinivas
A highly sensitive and specific liquid chromatography-electrospray ionization tandem mass spectrometric (LC-ESI-MS/MS) method for investigating the in vivo metabolites of almotriptan in rat plasma, feces and urine was developed. Chromatographic separation was achieved on a Lichrospher RP-18 column (250 × 4.6 mm, 5 μm), using 20 mM ammonium acetate (pH 3.5) and acetonitrile (60:40 v/v) as a mobile phase at 25 °C. MS/MS detection was performed by positive ion electrospray ionization using target ions atm/z336 [M + H], m/z368 &m/z282 [M + H]for almotriptan and its two metabolites, respectively. Two metabolitesviz., γ-aminobutyric acid and sulphonamide were detected in plasma as well as feces after 24 h of oral administration of almotriptan, while only γ-aminobutyric acid was found in urine. The method was sensitive with a lower limit of quantification of 1.43 ng/mL and linear over the range of 1.43-5000 ng/mL in plasma. The method was validated and successfully applied to a pharmacokinetic study of almotriptan in rat plasma using sumatriptan as an internal standard. The peak plasma concentration (Cmax) after 0.3 h of 5 mg/kg oral dose of almotriptan was determined to be 69.85 ng/mL.
Highlights
► Metabolite identification has been facilitated in high resolution LC-MS/MS. ► The method was successfully applied to study pharmacokinetics of almotriptan. ► Simple protein precipitation method was used for rat plasma in sample preparation. ► Good separation and resolution were obtained on Lichrospher RP-18 column.Measurements of Polybrominated Diphenyl Ethers and Polychlorinated Biphenyls in a Single Drop of Blood
Publication year: 2012
Source: Journal of Chromatography B, Available online 19 February 2012
Dasheng Lu, Dongli Wang, Ho Sai Simon Ip, Frank Barley, Bob Ramage, ...
A quantitative method that requires only small volume (50 μL) of blood sample has been developed for the determination of polybrominated diphenyl ethers (PBDEs) and polychlorinated biphenyls (PCBs). Target analytes in both plasma blood sample (DBSV) and dried blood spot (DBS) were analyzed by a gas chromatography/high resolution mass spectrometer (GC/HRMS). Measurements of standard reference materials by the developed method were in agreement with those certified values. Linear correlation coefficients were found to be 0.9985 and 0.9968 for DBS and DBSV analysis, respectively. Other analytical criteria, such as limits of detection, recoveries, precision, accuracy and linearity of the proposed method were also reported. From recovery studies, the addition of formic acid in the extraction solvent was found to be effective in extracting PBDEs and PCBs from filter paper. The PBDE and PCB levels in spiked DBS were monitored at room temperature for up to 30 days and the variations of target analytes were found to be insignificant. Our results suggest that DBS sampling technique is feasible for PBDE and PCBs biomonitoring in human population.
Source: Journal of Chromatography B, Available online 19 February 2012
Dasheng Lu, Dongli Wang, Ho Sai Simon Ip, Frank Barley, Bob Ramage, ...
A quantitative method that requires only small volume (50 μL) of blood sample has been developed for the determination of polybrominated diphenyl ethers (PBDEs) and polychlorinated biphenyls (PCBs). Target analytes in both plasma blood sample (DBSV) and dried blood spot (DBS) were analyzed by a gas chromatography/high resolution mass spectrometer (GC/HRMS). Measurements of standard reference materials by the developed method were in agreement with those certified values. Linear correlation coefficients were found to be 0.9985 and 0.9968 for DBS and DBSV analysis, respectively. Other analytical criteria, such as limits of detection, recoveries, precision, accuracy and linearity of the proposed method were also reported. From recovery studies, the addition of formic acid in the extraction solvent was found to be effective in extracting PBDEs and PCBs from filter paper. The PBDE and PCB levels in spiked DBS were monitored at room temperature for up to 30 days and the variations of target analytes were found to be insignificant. Our results suggest that DBS sampling technique is feasible for PBDE and PCBs biomonitoring in human population.
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