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Selected papers from this issue:High Resolution Magic Angle Spinning NMR to investigate ligand-receptor binding events for mass-limited samples in liquids
15 October 2011, 21:59:57
Publication year: 2011
Source: Journal of Pharmaceutical and Biomedical Analysis, Available online 15 October 2011
Fabio Ziarelli, Ling Peng, Cheng-Cai Zhang, Stéphane Viel
This work shows that High Resolution Magic Angle Spinning (HR-MAS) can be used to elucidate ligand-receptor binding phenomena for mass-limited samples in liquid solution. With respect to conventional 5 mm liquid-state NMR probe heads, HR-MAS allows for a considerable reduction (about one order of magnitude) in sample volume requirement, which represents a considerable advantage when working with biological samples present in low amount. More specifically, using a 20-μL active volume HR-MAS probe head, NMR experiments typically used to describe binding events (e.g.saturation transfer difference, WaterLOGSY, Diffusion Ordered Spectroscopy) were successfully recorded. In fact, contrary to other NMR experiments (e.g.TOCSY), which require special care when performed on liquid samples by HR-MAS, no interferences due to fast sample spinning were observed here. Collectively, the results indicate that HR-MAS allows for a significant mass sensitivity enhancement (a 3-fold increase in signal-to-noise ratio per unit of measuring time and mass was obtained here), hereby improving correspondingly the detection limit of the previously mentioned NMR experiments. More importantly, because MAS removes magnetic susceptibility broadenings in the sample, a good spectral resolution can be easily achieved in HR-MAS even for slightly heterogeneous samples, such as those arising from incomplete purification.
Source: Journal of Pharmaceutical and Biomedical Analysis, Available online 15 October 2011
Fabio Ziarelli, Ling Peng, Cheng-Cai Zhang, Stéphane Viel
This work shows that High Resolution Magic Angle Spinning (HR-MAS) can be used to elucidate ligand-receptor binding phenomena for mass-limited samples in liquid solution. With respect to conventional 5 mm liquid-state NMR probe heads, HR-MAS allows for a considerable reduction (about one order of magnitude) in sample volume requirement, which represents a considerable advantage when working with biological samples present in low amount. More specifically, using a 20-μL active volume HR-MAS probe head, NMR experiments typically used to describe binding events (e.g.saturation transfer difference, WaterLOGSY, Diffusion Ordered Spectroscopy) were successfully recorded. In fact, contrary to other NMR experiments (e.g.TOCSY), which require special care when performed on liquid samples by HR-MAS, no interferences due to fast sample spinning were observed here. Collectively, the results indicate that HR-MAS allows for a significant mass sensitivity enhancement (a 3-fold increase in signal-to-noise ratio per unit of measuring time and mass was obtained here), hereby improving correspondingly the detection limit of the previously mentioned NMR experiments. More importantly, because MAS removes magnetic susceptibility broadenings in the sample, a good spectral resolution can be easily achieved in HR-MAS even for slightly heterogeneous samples, such as those arising from incomplete purification.
Qualitative and quantitative analysis of the major constituents in Chinese medicinal preparation Guan-Xin-Ning injection by HPLC-DAD-ESI-MS
15 October 2011, 21:59:57
Publication year: 2011
Source: Journal of Pharmaceutical and Biomedical Analysis, Available online 15 October 2011
Ming Ruan, Yi Li, Xin Li, Jianguang Luo, Lingyi Kong
Guan-Xin-Ning (GXN) injection, a traditional Chinese medicinal preparation consisting of RadixSalvia miltiorrhizaand RhizomaLigusticum chuanxiong, has been used to treat coronary heart disease and angina pectoris in China for decades. In this paper, a HPLC/DAD/ESI-MSmethod was successfully developed for qualitative and quantitative analysis of the active components in GXN injection for the first time. 28 compounds were identified by comparison of their retention times and MS spectra (HPLC/DAD/ESI-MS) with those elucidated standards or recorded literature. 19 of them (danshensu, furoic acid, 3-O-caffeoylquinic acid, protocatechuic aldehyde,p-hydroxybenzoic acid, chlorogenic acid, caffeic acid, 4-O-caffeoylquinic acid, vanillin, 1,3-dicaffeoylquinic acid, 4-hydroxycinnamic acid, ferulic acid, senkyunolide I, senkyunolide H, isosalvianolic acid A, rosmarinic acid, salvianolic acid B, salvianolic acid A and isosalvianolic acid C) were simultaneously determined by HPLC-DAD quantitatively. The analytical method was validated and successfully applied for simultaneous determination of major components in GXN injections from seven different production batches, indicating that the proposed approach was applicable for the routine analysis and quality control of GXN injection.
Source: Journal of Pharmaceutical and Biomedical Analysis, Available online 15 October 2011
Ming Ruan, Yi Li, Xin Li, Jianguang Luo, Lingyi Kong
Guan-Xin-Ning (GXN) injection, a traditional Chinese medicinal preparation consisting of RadixSalvia miltiorrhizaand RhizomaLigusticum chuanxiong, has been used to treat coronary heart disease and angina pectoris in China for decades. In this paper, a HPLC/DAD/ESI-MSmethod was successfully developed for qualitative and quantitative analysis of the active components in GXN injection for the first time. 28 compounds were identified by comparison of their retention times and MS spectra (HPLC/DAD/ESI-MS) with those elucidated standards or recorded literature. 19 of them (danshensu, furoic acid, 3-O-caffeoylquinic acid, protocatechuic aldehyde,p-hydroxybenzoic acid, chlorogenic acid, caffeic acid, 4-O-caffeoylquinic acid, vanillin, 1,3-dicaffeoylquinic acid, 4-hydroxycinnamic acid, ferulic acid, senkyunolide I, senkyunolide H, isosalvianolic acid A, rosmarinic acid, salvianolic acid B, salvianolic acid A and isosalvianolic acid C) were simultaneously determined by HPLC-DAD quantitatively. The analytical method was validated and successfully applied for simultaneous determination of major components in GXN injections from seven different production batches, indicating that the proposed approach was applicable for the routine analysis and quality control of GXN injection.
Highlights
► We identify 28 compounds in Guan-Xin-Ning (GXN) injection by HPLC-DAD-MS. ► 19 main components in GXN injections are simultaneously quantified by HPLC-DAD. ► The established method can be used in quality control of GXN injection.HPLC-MS method for the simultaneous quantification of the antileukemia drugs imatinib, dasatinib and nilotinib in human peripheral blood mononuclear cell (PBMC)
15 October 2011, 21:59:57
Publication year: 2011
Source: Journal of Pharmaceutical and Biomedical Analysis, Available online 14 October 2011
Antonio D’Avolio, Marco Simiele, Silvia De Francia, Alessandra Ariaudo, Lorena Baietto, ...
A new method using high performance liquid chromatography coupled with electrospray mass spectrometry is described for the quantification of PBMC concentration of tyrosine kinase inhibitors imatinib, dasatinib and nilotinib. A simple PBMC isolation and extraction procedure were applied on 10-14 mL of blood aliquots. Chromatographic separation of drugs and Internal Standard (quinoxaline) was achieved with a gradient (acetonitrile and water + formic acid 0.05%) on a C18 reverse phase analytical column with 25 min of analytical run, at flow rate of 0.25 mL/min. Mean intra- and inter-day precision for all compounds were 8.76 and 12.20%; mean accuracy was -3.86%; extraction recovery ranged within 79 and 91%. Calibration curves ranged from 50.0 to 0.25 ng. The limit of quantification was set at 0.25 ng for all the analyzed drugs.This novel developed methodology allows a specific, sensitive and reliable simultaneous intracellular determination of the three tyrosine kinase inhibitors imatinib, dasatinib and nilotinib in a single chromatographic run, useful for drugs estimation in PBMC of patients affected by chronic myeloid leukemia.
Source: Journal of Pharmaceutical and Biomedical Analysis, Available online 14 October 2011
Antonio D’Avolio, Marco Simiele, Silvia De Francia, Alessandra Ariaudo, Lorena Baietto, ...
A new method using high performance liquid chromatography coupled with electrospray mass spectrometry is described for the quantification of PBMC concentration of tyrosine kinase inhibitors imatinib, dasatinib and nilotinib. A simple PBMC isolation and extraction procedure were applied on 10-14 mL of blood aliquots. Chromatographic separation of drugs and Internal Standard (quinoxaline) was achieved with a gradient (acetonitrile and water + formic acid 0.05%) on a C18 reverse phase analytical column with 25 min of analytical run, at flow rate of 0.25 mL/min. Mean intra- and inter-day precision for all compounds were 8.76 and 12.20%; mean accuracy was -3.86%; extraction recovery ranged within 79 and 91%. Calibration curves ranged from 50.0 to 0.25 ng. The limit of quantification was set at 0.25 ng for all the analyzed drugs.This novel developed methodology allows a specific, sensitive and reliable simultaneous intracellular determination of the three tyrosine kinase inhibitors imatinib, dasatinib and nilotinib in a single chromatographic run, useful for drugs estimation in PBMC of patients affected by chronic myeloid leukemia.
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