2012Yaowu fenxi zazhiRequires access

LC-MS/MS with Chiralcel OD-H chiral column simultaneously determination of four β-blocker enantioners

Xiaoli Wang

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Abstract

Objective:To develop a chiral stationary phase liquid chromatography-tandem mass spectrometry(HPLC-MS/MS) method for simultaneously determination of four β-blockers.Methods:Chromatographic separation was achieved on a Chiralcel OD-H(250 mm×4.6 mm,5 μm) chiral column with a run time of 23.0 min.ESI+ was performed in multiple reaction monitoring mode(MRM),using the transitions of m/z 260.2→116.0 for propranolol,m/z 268.4→116.0 for metoprolol,m/z 267.2→145.0 for atenolol,and m/z 326.2→116.0 for bisoprolol.Results:The effects of mobile phase formulation,column temperature,and flow rate on the chiral separation of the four β-blocking agents were investigated,and optimal conditions were obtained.The possible mechanism of chiral separation was discussed based on the structural characteristics of the agents and the sorts of stationary phase.Conclusion:The method developed in our study greatly improved the separation efficiency.It is simple,efficient and with good reproducibility,which can be used for routine and biological specimen analysis of β-blocking enantiomers.

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Objective:To develop a chiral stationary phase liquid chromatography-tandem mass spectrometry(HPLC-MS/MS) method for simultaneously determination of four β-blockers.Methods:Chromatographic separation was achieved on a Chiralcel OD-H(250 mm×4.6 mm,5 μm) chiral column with a run time of 23.0 min.ESI+ was performed in multiple reaction monitoring mode(MRM),using the transitions of m/z 260.2→116.0 for propranolol,m/z 268.4→116.0 for metoprolol,m/z 267.2→145.0 for atenolol,and m/z 326.2→116.0 for bisoprolol.Results:The effects of mobile phase formulation,column temperature,and flow rate on the chiral separation of the four β-blocking agents were investigated,and optimal conditions were obtained.The possible mechanism of chiral separation was discussed based on the structural characteristics of the agents and the sorts of stationary phase.Conclusion:The method developed in our study greatly improved the separation efficiency.It is simple,efficient and with good reproducibility,which can be used for routine and biological specimen analysis of β-blocking enantiomers.

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Available abstract

Objective:To develop a chiral stationary phase liquid chromatography-tandem mass spectrometry(HPLC-MS/MS) method for simultaneously determination of four β-blockers.Methods:Chromatographic separation was achieved on a Chiralcel OD-H(250 mm×4.6 mm,5 μm) chiral column with a run time of 23.0 min.ESI+ was performed in multiple reaction monitoring mode(MRM),using the transitions of m/z 260.2→116.0 for propranolol,m/z 268.4→116.0 for metoprolol,m/z 267.2→145.0 for atenolol,and m/z 326.2→116.0 for bisoprolol.Results:The effects of mobile phase formulation,column temperature,and flow rate on the chiral separation of the four β-blocking agents were investigated,and optimal conditions were obtained.The possible mechanism of chiral separation was discussed based on the structural characteristics of the agents and the sorts of stationary phase.Conclusion:The method developed in our study greatly improved the separation efficiency.It is simple,efficient and with good reproducibility,which can be used for routine and biological specimen analysis of β-blocking enantiomers.

Key concepts: Chemistry, Chromatography, Enantiomer, Atenolol, Bisoprolol, Chiral column chromatography, Mass spectrometry, Metoprolol

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