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:
Selected papers from the latest issue:
A rapid and sensitive LC/ESI-MS/MS method for quantitative analysis of docetaxel in human plasma and its application to a pharmacokinetic study
10 February 2012, 00:31:26
Publication year: 2012
Source: Journal of Chromatography B, Available online 9 February 2012
Hiroaki Yamaguchi, Asuka Fujikawa, Hajime Ito, Nobuaki Tanaka, Ayako Furugen, ...
Docetaxel is a taxane family antineoplastic agent widely employed in cancer chemotherapy. We developed a liquid chromatography/tandem mass spectrometry method for the determination of docetaxel in human plasma. Plasma samples were deproteinized by acetonitrile containing internal standard paclitaxel. Chromatographic separation was performed on a TSKgel ODS-100 V 3 μm (50 mm × 2.0 mm i.d.) column using a mobile phase composed of acetonitrile-methanol-water-formic acid (50:5:45:0.1, v/v/v/v). Detection was performed on a triple-quadrupole tandem mass spectrometer with multiple reaction monitoring (MRM) mode via electrospray ionization (ESI) source. This method covered a linearity range of 5-5000 ng/mL with the lower limit of quantification of 5 ng/mL. The intra-day precision and inter-day precision (R.S.D.) of analysis were less than 6.7%, and the accuracy (R.E.) was within ±9.0% at the concentrations of 5, 20, 200, and 2000 ng/mL. The total run time was 5.0 min. This method was successfully applied for clinical pharmacokinetic investigation.
Source: Journal of Chromatography B, Available online 9 February 2012
Hiroaki Yamaguchi, Asuka Fujikawa, Hajime Ito, Nobuaki Tanaka, Ayako Furugen, ...
Docetaxel is a taxane family antineoplastic agent widely employed in cancer chemotherapy. We developed a liquid chromatography/tandem mass spectrometry method for the determination of docetaxel in human plasma. Plasma samples were deproteinized by acetonitrile containing internal standard paclitaxel. Chromatographic separation was performed on a TSKgel ODS-100 V 3 μm (50 mm × 2.0 mm i.d.) column using a mobile phase composed of acetonitrile-methanol-water-formic acid (50:5:45:0.1, v/v/v/v). Detection was performed on a triple-quadrupole tandem mass spectrometer with multiple reaction monitoring (MRM) mode via electrospray ionization (ESI) source. This method covered a linearity range of 5-5000 ng/mL with the lower limit of quantification of 5 ng/mL. The intra-day precision and inter-day precision (R.S.D.) of analysis were less than 6.7%, and the accuracy (R.E.) was within ±9.0% at the concentrations of 5, 20, 200, and 2000 ng/mL. The total run time was 5.0 min. This method was successfully applied for clinical pharmacokinetic investigation.
Highlights
► We developed a LC/ESI-MS/MS method for the determination of docetaxel in human plasma. ► One-step protein precipitation method was used for sample pretreatment without evaporation step. ► This method covered a linearity range of 5-5000 ng/mL with the lower limit of quantification of 5 ng/mL. ► The developed method was fully validated. ► This method was successfully applied for clinical pharmacokinetic investigation.Quantitation of bentysrepinine (Y101) in rat plasma by liquid chromatography tandem mass spectrometry: application to pharmacokinetic study
10 February 2012, 00:31:26
Publication year: 2012
Source: Journal of Chromatography B, Available online 9 February 2012
Huirong Fan, Ruixing Li, Yuan Gu, Duanyun Si, Changxiao Liu
A simple, accurate and sensitive liquid chromatography tandem mass spectrometry (LC-MS/MS) method was developed and validated for quantitation of bentysrepinine (Y101) in rat plasma. After the addition of diphenhydramine (internal standard, IS), plasma samples were pretreated by protein precipitation. Chromatographic separation was carried out on an Atlantisanalytical column (4.6 × 100 mm, 5 μm, Waters) with methanol: 20 mM ammonium formate consisting of 1.0% formic acid (65:35,v/v) as the mobile phase at an isocratic flow rate of 0.4 mL/min for 7.5 min. The multiple reaction monitoring (MRM) transitions were performed atm/z490.2→339.5 for Y101andm/z256.0→167.0 for IS on a SCIEX API 4000 mass spectrometer in the positive ion mode with electrospray ionization (ESI) source. Good linearity was achieved over the concentration range of 1–2500 ng/mL. The intra- and inter-day precisions were less than 8.3%, and the accuracy ranged from -4.0% to 2.8%. Y101 was stable during the analysis and the storage period. The pharmacokinetic profiles of Y101 at three dose levels were successfully studied for the first time in rats by this method. After single intra-gastric administration of Y101 at the doses of 25, 50 and 100 mg/kg, Cmaxand AUC0-twere proportional to the doses given.
Source: Journal of Chromatography B, Available online 9 February 2012
Huirong Fan, Ruixing Li, Yuan Gu, Duanyun Si, Changxiao Liu
A simple, accurate and sensitive liquid chromatography tandem mass spectrometry (LC-MS/MS) method was developed and validated for quantitation of bentysrepinine (Y101) in rat plasma. After the addition of diphenhydramine (internal standard, IS), plasma samples were pretreated by protein precipitation. Chromatographic separation was carried out on an Atlantisanalytical column (4.6 × 100 mm, 5 μm, Waters) with methanol: 20 mM ammonium formate consisting of 1.0% formic acid (65:35,v/v) as the mobile phase at an isocratic flow rate of 0.4 mL/min for 7.5 min. The multiple reaction monitoring (MRM) transitions were performed atm/z490.2→339.5 for Y101andm/z256.0→167.0 for IS on a SCIEX API 4000 mass spectrometer in the positive ion mode with electrospray ionization (ESI) source. Good linearity was achieved over the concentration range of 1–2500 ng/mL. The intra- and inter-day precisions were less than 8.3%, and the accuracy ranged from -4.0% to 2.8%. Y101 was stable during the analysis and the storage period. The pharmacokinetic profiles of Y101 at three dose levels were successfully studied for the first time in rats by this method. After single intra-gastric administration of Y101 at the doses of 25, 50 and 100 mg/kg, Cmaxand AUC0-twere proportional to the doses given.
Highlights
► The first LC-MS/MS method for quantitation of Y101 was established. ► The method provided good sensitivity (1 ng/mL for Y101). ► A simple one-step protein precipitation was chosen to pretreat samples. ► The method has been successfully applied to a pharmacokinetic study for the first time in rats.Quantification of blending of olive oils and edible vegetable oils by triacylglycerol fingerprint gas chromatography and chemometric tools
10 February 2012, 00:31:26
Publication year: 2012
Source: Journal of Chromatography B, Available online 9 February 2012
Cristina Ruiz-Samblás, Federico Marini, Luis Cuadros-Rodríguez, Antonio González-Casado
A reliable procedure for the identification and quantification of the adulteration of olive oils in terms of blending with other vegetable oils (sunflower, corn, seeds, sesame and soya) has been developed. From the analytical viewpoint, the whole procedure relies only on the results of the determination of the triacylglycerol profile of the oils by high temperature gas chromatography-mass spectrometry. The chromatographic profiles were pre-treated (baseline correction, peak alignment using iCoshift algorithm and mean centering) before building the models. At first, a class-modelling approach, Soft Independent Modeling of Class Analogy (SIMCA) was used to identify the vegetable oil used blending. Successively, a separate calibration model for each kind of blending was built using Partial Least Square (PLS). The correlation coefficients of actual versus predicted concentrations resulting from multivariate calibration models were between 0.95 and 0.99. In addition, Genetic Algorithms (GA-PLS), were used, as variable selection method, to improve the models which yielded Rvalues higher than 0.90 for calibration set. This model had a better predictive ability than the PLS without feature selection. The results obtained showed the potential of this method and allowed quantification of blends of olive oil in the vegetable oils tested containing at least 10% of olive oil.
Source: Journal of Chromatography B, Available online 9 February 2012
Cristina Ruiz-Samblás, Federico Marini, Luis Cuadros-Rodríguez, Antonio González-Casado
A reliable procedure for the identification and quantification of the adulteration of olive oils in terms of blending with other vegetable oils (sunflower, corn, seeds, sesame and soya) has been developed. From the analytical viewpoint, the whole procedure relies only on the results of the determination of the triacylglycerol profile of the oils by high temperature gas chromatography-mass spectrometry. The chromatographic profiles were pre-treated (baseline correction, peak alignment using iCoshift algorithm and mean centering) before building the models. At first, a class-modelling approach, Soft Independent Modeling of Class Analogy (SIMCA) was used to identify the vegetable oil used blending. Successively, a separate calibration model for each kind of blending was built using Partial Least Square (PLS). The correlation coefficients of actual versus predicted concentrations resulting from multivariate calibration models were between 0.95 and 0.99. In addition, Genetic Algorithms (GA-PLS), were used, as variable selection method, to improve the models which yielded Rvalues higher than 0.90 for calibration set. This model had a better predictive ability than the PLS without feature selection. The results obtained showed the potential of this method and allowed quantification of blends of olive oil in the vegetable oils tested containing at least 10% of olive oil.
Highlights
► Reliable method for quantification of olive oils adulteration with vegetable oils ► Determination triglycerides profile by HTGC-MS, use of all data points to get results ► Chromatograms were pre-treated (baseline correction, peak alignment) before building models ► Genetic algorithms were used as variable selection method to improve the modelsMolecular imprinting based composite cryogel membranes for purification of anti-hepatitis B surface antibody by fast protein liquid chromatography
10 February 2012, 00:31:26
Publication year: 2012
Source: Journal of Chromatography B, Available online 9 February 2012
Sevgi Asliyuce, Lokman Uzun, Abbas Taner, Serhat Unal, Ridvan Say, ...
In the present study, we have focused our attention to prepare molecular imprinted composite cryogel membranes for purification of hepatitis B surface antibody (anti-HBs) by fast protein liquid chromatography. Before the preparation of the molecular imprinted composite cryogel membranes (MI-CMs) by free radical polymerization at sub-zero temperature, we have synthesized and characterized the anti-HBs imprinted particles. Then, the cryogel membranes (CMs) were characterized by swelling test, scanning electron microscopy and Fourier transform infrared spectroscopy. Prior to chromatographic purification studies, the effective parameters on the anti-HBs adsorption process were evaluated by investigating the dependency of the adsorption capacity on flow-rate, anti-HBs concentration, contact time and ionic strength. The maximum anti-HBs adsorption capacity was calculated as 701.4 mIU/g CM. The selectivity of the MI-CMs was shown by competitive adsorption of anti-HBs, total anti-hepatitis A antibody (anti-HAV) and total immunoglobulin E (IgE) adsorption studies. The MI-CMs have relative selectivity coefficients as 5.45 for anti-HBs/total anti-HAV and 9.05 for anti-HBs/total IgE, respectively. The phosphate buffer solution (pH 7.4) containing 1.0 M NaCl was used for elution, almost completely, of adsorbed anti-HBs molecules. The MI-CMs could be used many times without any significant decrease in the adsorption capacity. The chromatographic purification performances of the MI-CMs were also investigated. The chromatographic parameters such as capacity and separation factors, the theoretical plate number and resolution of the MI-CMs were calculated as 5.48, 6.02, 1153.9, and 1.72 for anti-HBs molecules, respectively. As a conclusion, we can say that the MI-CMs could be used for specific purification of anti-HBs from anti-HBs positive human plasma.
Source: Journal of Chromatography B, Available online 9 February 2012
Sevgi Asliyuce, Lokman Uzun, Abbas Taner, Serhat Unal, Ridvan Say, ...
In the present study, we have focused our attention to prepare molecular imprinted composite cryogel membranes for purification of hepatitis B surface antibody (anti-HBs) by fast protein liquid chromatography. Before the preparation of the molecular imprinted composite cryogel membranes (MI-CMs) by free radical polymerization at sub-zero temperature, we have synthesized and characterized the anti-HBs imprinted particles. Then, the cryogel membranes (CMs) were characterized by swelling test, scanning electron microscopy and Fourier transform infrared spectroscopy. Prior to chromatographic purification studies, the effective parameters on the anti-HBs adsorption process were evaluated by investigating the dependency of the adsorption capacity on flow-rate, anti-HBs concentration, contact time and ionic strength. The maximum anti-HBs adsorption capacity was calculated as 701.4 mIU/g CM. The selectivity of the MI-CMs was shown by competitive adsorption of anti-HBs, total anti-hepatitis A antibody (anti-HAV) and total immunoglobulin E (IgE) adsorption studies. The MI-CMs have relative selectivity coefficients as 5.45 for anti-HBs/total anti-HAV and 9.05 for anti-HBs/total IgE, respectively. The phosphate buffer solution (pH 7.4) containing 1.0 M NaCl was used for elution, almost completely, of adsorbed anti-HBs molecules. The MI-CMs could be used many times without any significant decrease in the adsorption capacity. The chromatographic purification performances of the MI-CMs were also investigated. The chromatographic parameters such as capacity and separation factors, the theoretical plate number and resolution of the MI-CMs were calculated as 5.48, 6.02, 1153.9, and 1.72 for anti-HBs molecules, respectively. As a conclusion, we can say that the MI-CMs could be used for specific purification of anti-HBs from anti-HBs positive human plasma.
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