Development and validation of a hydrophilic interaction liquid chromatography‐tandem mass spectrometry method for the quantification of regadenoson in human plasma and its pharmacokinetic application
Regadenoson, the first selective adenosine A2A receptor agonist, is used to perform exercise stress test during radionuclide myocardial perfusion imaging. To detect the concentration of regadenoson in human plasma, a simple, fast, and sensitive tandem mass spectrometry method was established herein....
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| Published in | Journal of separation science Vol. 45; no. 6; pp. 1146 - 1152 |
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| Main Authors | , , , , , , , , |
| Format | Journal Article |
| Language | English |
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01.03.2022
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| Abstract | Regadenoson, the first selective adenosine A2A receptor agonist, is used to perform exercise stress test during radionuclide myocardial perfusion imaging. To detect the concentration of regadenoson in human plasma, a simple, fast, and sensitive tandem mass spectrometry method was established herein. Acetonitrile was used as a protein precipitation agent. Chromatographic separation was completed in 6.5 min using a BEH HILIC column (50 × 2.1 mm, 1.7 μm). The mobile phase consisted of 10 mmol/L ammonium acetate/acetonitrile (gradient elution). To quantify regadenoson and regadenoson‐d3, an API 4000 mass spectrometry in multiple reaction monitoring mode with transitions of 391.3→259.2 and 394.3→262.2, respectively, was utilized. The calibration curve was linear in the range of 0.100–50.0 μg/L, and the intrabatch and interbatch precisions were <9.7% and <13.0%, respectively, and the accuracy was 2.0–6.9%. There was no apparent matrix effect for regadenoson or regadenoson‐d3. The developed method was used to study the pharmacokinetic characteristics of regadenoson in healthy Chinese subjects. |
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| AbstractList | Regadenoson, the first selective adenosine A2A receptor agonist, is used to perform exercise stress test during radionuclide myocardial perfusion imaging. To detect the concentration of regadenoson in human plasma, a simple, fast, and sensitive tandem mass spectrometry method was established herein. Acetonitrile was used as a protein precipitation agent. Chromatographic separation was completed in 6.5 min using a BEH HILIC column (50 × 2.1 mm, 1.7 μm). The mobile phase consisted of 10 mmol/L ammonium acetate/acetonitrile (gradient elution). To quantify regadenoson and regadenoson‐d3, an API 4000 mass spectrometry in multiple reaction monitoring mode with transitions of 391.3→259.2 and 394.3→262.2, respectively, was utilized. The calibration curve was linear in the range of 0.100–50.0 μg/L, and the intrabatch and interbatch precisions were <9.7% and <13.0%, respectively, and the accuracy was 2.0–6.9%. There was no apparent matrix effect for regadenoson or regadenoson‐d3. The developed method was used to study the pharmacokinetic characteristics of regadenoson in healthy Chinese subjects. Regadenoson, the first selective adenosine A₂A receptor agonist, is used to perform exercise stress test during radionuclide myocardial perfusion imaging. To detect the concentration of regadenoson in human plasma, a simple, fast, and sensitive tandem mass spectrometry method was established herein. Acetonitrile was used as a protein precipitation agent. Chromatographic separation was completed in 6.5 min using a BEH HILIC column (50 × 2.1 mm, 1.7 μm). The mobile phase consisted of 10 mmol/L ammonium acetate/acetonitrile (gradient elution). To quantify regadenoson and regadenoson‐d3, an API 4000 mass spectrometry in multiple reaction monitoring mode with transitions of 391.3→259.2 and 394.3→262.2, respectively, was utilized. The calibration curve was linear in the range of 0.100–50.0 μg/L, and the intrabatch and interbatch precisions were <9.7% and <13.0%, respectively, and the accuracy was 2.0–6.9%. There was no apparent matrix effect for regadenoson or regadenoson‐d3. The developed method was used to study the pharmacokinetic characteristics of regadenoson in healthy Chinese subjects. Regadenoson, the first selective adenosine A2A receptor agonist, is used to perform exercise stress test during radionuclide myocardial perfusion imaging. To detect the concentration of regadenoson in human plasma, a simple, fast, and sensitive tandem mass spectrometry method was established herein. Acetonitrile was used as a protein precipitation agent. Chromatographic separation was completed in 6.5 min using a BEH HILIC column (50 × 2.1 mm, 1.7 μm). The mobile phase consisted of 10 mmol/L ammonium acetate/acetonitrile (gradient elution). To quantify regadenoson and regadenoson-d3, an API 4000 mass spectrometry in multiple reaction monitoring mode with transitions of 391.3→259.2 and 394.3→262.2, respectively, was utilized. The calibration curve was linear in the range of 0.100-50.0 μg/L, and the intrabatch and interbatch precisions were <9.7% and <13.0%, respectively, and the accuracy was 2.0-6.9%. There was no apparent matrix effect for regadenoson or regadenoson-d3. The developed method was used to study the pharmacokinetic characteristics of regadenoson in healthy Chinese subjects.Regadenoson, the first selective adenosine A2A receptor agonist, is used to perform exercise stress test during radionuclide myocardial perfusion imaging. To detect the concentration of regadenoson in human plasma, a simple, fast, and sensitive tandem mass spectrometry method was established herein. Acetonitrile was used as a protein precipitation agent. Chromatographic separation was completed in 6.5 min using a BEH HILIC column (50 × 2.1 mm, 1.7 μm). The mobile phase consisted of 10 mmol/L ammonium acetate/acetonitrile (gradient elution). To quantify regadenoson and regadenoson-d3, an API 4000 mass spectrometry in multiple reaction monitoring mode with transitions of 391.3→259.2 and 394.3→262.2, respectively, was utilized. The calibration curve was linear in the range of 0.100-50.0 μg/L, and the intrabatch and interbatch precisions were <9.7% and <13.0%, respectively, and the accuracy was 2.0-6.9%. There was no apparent matrix effect for regadenoson or regadenoson-d3. The developed method was used to study the pharmacokinetic characteristics of regadenoson in healthy Chinese subjects. Regadenoson, the first selective adenosine A 2A receptor agonist, is used to perform exercise stress test during radionuclide myocardial perfusion imaging. To detect the concentration of regadenoson in human plasma, a simple, fast, and sensitive tandem mass spectrometry method was established herein. Acetonitrile was used as a protein precipitation agent. Chromatographic separation was completed in 6.5 min using a BEH HILIC column (50 × 2.1 mm, 1.7 μm). The mobile phase consisted of 10 mmol/L ammonium acetate/acetonitrile (gradient elution). To quantify regadenoson and regadenoson‐d3, an API 4000 mass spectrometry in multiple reaction monitoring mode with transitions of 391.3→259.2 and 394.3→262.2, respectively, was utilized. The calibration curve was linear in the range of 0.100–50.0 μg/L, and the intrabatch and interbatch precisions were <9.7% and <13.0%, respectively, and the accuracy was 2.0–6.9%. There was no apparent matrix effect for regadenoson or regadenoson‐d3. The developed method was used to study the pharmacokinetic characteristics of regadenoson in healthy Chinese subjects. Regadenoson, the first selective adenosine A receptor agonist, is used to perform exercise stress test during radionuclide myocardial perfusion imaging. To detect the concentration of regadenoson in human plasma, a simple, fast, and sensitive tandem mass spectrometry method was established herein. Acetonitrile was used as a protein precipitation agent. Chromatographic separation was completed in 6.5 min using a BEH HILIC column (50 × 2.1 mm, 1.7 μm). The mobile phase consisted of 10 mmol/L ammonium acetate/acetonitrile (gradient elution). To quantify regadenoson and regadenoson-d3, an API 4000 mass spectrometry in multiple reaction monitoring mode with transitions of 391.3→259.2 and 394.3→262.2, respectively, was utilized. The calibration curve was linear in the range of 0.100-50.0 μg/L, and the intrabatch and interbatch precisions were <9.7% and <13.0%, respectively, and the accuracy was 2.0-6.9%. There was no apparent matrix effect for regadenoson or regadenoson-d3. The developed method was used to study the pharmacokinetic characteristics of regadenoson in healthy Chinese subjects. Regadenoson, the first selective adenosine A2A receptor agonist, is used to perform exercise stress test during radionuclide myocardial perfusion imaging. To detect the concentration of regadenoson in human plasma, a simple, fast, and sensitive tandem mass spectrometry method was established herein. Acetonitrile was used as a protein precipitation agent. Chromatographic separation was completed in 6.5 min using a BEH HILIC column (50 × 2.1 mm, 1.7 μm). The mobile phase consisted of 10 mmol/L ammonium acetate/acetonitrile (gradient elution). To quantify regadenoson and regadenoson‐d3, an API 4000 mass spectrometry in multiple reaction monitoring mode with transitions of 391.3→259.2 and 394.3→262.2, respectively, was utilized. The calibration curve was linear in the range of 0.100–50.0 μg/L, and the intrabatch and interbatch precisions were <9.7% and <13.0%, respectively, and the accuracy was 2.0–6.9%. There was no apparent matrix effect for regadenoson or regadenoson‐d3. The developed method was used to study the pharmacokinetic characteristics of regadenoson in healthy Chinese subjects. |
| Author | Wang, Da‐Wei Zeng, Nv‐Jin Yang, Yan‐Ling Zhang, Hong‐Wen Sun, Lu‐Ning Wang, Dun‐Jian Wang, Yong‐Qing Shen, Ye Fang, Qiu‐Chen |
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| References_xml | – volume: 79 start-page: 2 year: 1997 end-page: 10 article-title: Adenosine and adenosine receptors in the cardiovascular system: biochemistry, physiology, and pharmacology publication-title: Am J Cardiol – volume: 20 start-page: 284 year: 2013 end-page: 8 article-title: Regadenoson: a focused update publication-title: J Nucl Cardiol – volume: 140 start-page: 121 year: 2013 end-page: 32 article-title: Pharmacologic manipulation of coronary vascular physiology for the evaluation of coronary artery disease publication-title: Pharmacol Ther – volume: 14 start-page: 514 year: 2007 end-page: 20 article-title: Regadenoson, a selective A2A adenosine receptor agonist, causes dose‐dependent increases in coronary blood flow velocity in humans publication-title: J Nucl Cardiol – volume: 63 start-page: 1 year: 2011 end-page: 34 article-title: International Union of Basic and Clinical Pharmacology. LXXXI. Nomenclature and classification of adenosine receptors—an update publication-title: Pharmacol Rev – volume: 54 start-page: 1123 year: 2009 end-page: 30 article-title: Regadenoson: a new myocardial stress agent publication-title: J Am Coll Cardiol. – volume: 57 start-page: 3623 year: 2014 end-page: 50 article-title: Adenosine A2A receptor as a drug discovery target publication-title: J Med Chem – volume: 33 start-page: 698 year: 2010 end-page: 715 article-title: HILIC methods in pharmaceutical analysis publication-title: J Sep Sci – volume: 38 start-page: 3876 year: 2015 end-page: 83 article-title: Hydrophilic interaction liquid chromatography coupled with tandem mass spectrometry method for the simultaneous determination of l‐valine, l‐leucine, l‐isoleucine, l‐phenylalanine, and l‐tyrosine in human serum publication-title: J Sep Sci – volume: 46 start-page: 2069 year: 2005 end-page: 75 article-title: Initial clinical experience with regadenoson, a novel selective A2A agonist for pharmacologic stress single‐photon emission computed tomography myocardial perfusion imaging publication-title: J Am Coll Cardiol – ident: e_1_2_9_12_1 – ident: e_1_2_9_2_1 doi: 10.1016/j.pharmthera.2013.06.004 – ident: e_1_2_9_6_1 doi: 10.1021/jm4011669 – ident: e_1_2_9_5_1 doi: 10.1016/j.jacc.2009.04.089 – ident: e_1_2_9_7_1 doi: 10.1016/j.nuclcard.2007.02.016 – ident: e_1_2_9_8_1 doi: 10.1016/j.jacc.2005.05.097 – ident: e_1_2_9_4_1 doi: 10.1016/S0002-9149(97)00256-7 – ident: e_1_2_9_11_1 doi: 10.1002/jssc.201500512 – ident: e_1_2_9_3_1 doi: 10.1124/pr.110.003285 – ident: e_1_2_9_10_1 doi: 10.1002/jssc.200900742 – ident: e_1_2_9_9_1 doi: 10.1007/s12350-012-9661-3 |
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| Snippet | Regadenoson, the first selective adenosine A2A receptor agonist, is used to perform exercise stress test during radionuclide myocardial perfusion imaging. To... Regadenoson, the first selective adenosine A 2A receptor agonist, is used to perform exercise stress test during radionuclide myocardial perfusion imaging. To... Regadenoson, the first selective adenosine A receptor agonist, is used to perform exercise stress test during radionuclide myocardial perfusion imaging. To... Regadenoson, the first selective adenosine A₂A receptor agonist, is used to perform exercise stress test during radionuclide myocardial perfusion imaging. To... |
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| SubjectTerms | Acetonitrile Adenosine agonists Ammonium acetate Blood plasma calibration Cardiac stress tests Chromatography, High Pressure Liquid Chromatography, Liquid - methods exercise Humans hydrophilic interaction liquid chromatography hydrophilicity Hydrophobic and Hydrophilic Interactions Ions Liquid chromatography Mass spectrometry Pharmacokinetics Pharmacology Purines Pyrazoles Radioisotopes regadenoson, tandem mass spectrometry Reproducibility of Results Scientific imaging separation Spectroscopy tandem mass spectrometry Tandem Mass Spectrometry - methods |
| Title | Development and validation of a hydrophilic interaction liquid chromatography‐tandem mass spectrometry method for the quantification of regadenoson in human plasma and its pharmacokinetic application |
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