Determination of azatadine in human plasma by liquid chromatography/tandem mass spectrometry

A sensitive method using liquid chromatography with tandem mass spectrometric detection (LC–MS/MS) was developed and validated for the analysis of antihistamine drug azatadine in human plasma. Loratadine was used as internal standard (IS). Analytes were extracted from human plasma by liquid/liquid e...

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Veröffentlicht in:Journal of chromatography. B, Analytical technologies in the biomedical and life sciences Analytical technologies in the biomedical and life sciences, 2011-08, Vol.879 (23), p.2189-2193
Hauptverfasser: Zhu, Yan-rong, Jia, Yan-yan, Jiang, Ling, Wang, Chao, Ding, Li-kun, Yang, Jing, Li, Liang, Zhao, Pei-xi, Liu, Wen-xin, Yi-Ding, Wang, Li, Wen, Ai-dong
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container_issue 23
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container_title Journal of chromatography. B, Analytical technologies in the biomedical and life sciences
container_volume 879
creator Zhu, Yan-rong
Jia, Yan-yan
Jiang, Ling
Wang, Chao
Ding, Li-kun
Yang, Jing
Li, Liang
Zhao, Pei-xi
Liu, Wen-xin
Yi-Ding
Wang, Li
Wen, Ai-dong
description A sensitive method using liquid chromatography with tandem mass spectrometric detection (LC–MS/MS) was developed and validated for the analysis of antihistamine drug azatadine in human plasma. Loratadine was used as internal standard (IS). Analytes were extracted from human plasma by liquid/liquid extraction using ethyl acetate. The organic phase was reduced to dryness under a stream of nitrogen at 30 °C and the residue was reconstituted with the mobile phase. 5 μL of the resulting solution was injected onto the LC–MS/MS system. A 4.6 mm × 150 mm, I.D. 5 μm, Agilent TC-C 18 column was used to perform the chromatographic analysis. The mobile phase consisted of ammonium formate buffer 0.010 M (adjusted to pH 4.3 with 1 M formic acid)/acetonitrile (20:80, v/ v) The chromatographic run time was 5 min per injection and flow rate was 0.6 mL/min. The retention time was 2.4 and 4.4 min for azatadine and IS, respectively. The tandem mass spectrometric detection mode was achieved with electrospray ionization (ESI) iron source and the multiple reaction monitoring (MRM) (291.3 → 248.2 m/ z for azatadine, 383.3 → 337.3 m/ z for IS) was operated in positive ion modes. The low limit of quantitation (LLOQ) was 0.05 ng/mL. The intra-day and inter-day precision of the quality control (QC) samples was 8.93–11.57% relative standard deviation (RSD). The inter-day accuracy of the QC samples was 96.83–105.07% of the nominal values.
doi_str_mv 10.1016/j.jchromb.2011.05.050
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Loratadine was used as internal standard (IS). Analytes were extracted from human plasma by liquid/liquid extraction using ethyl acetate. The organic phase was reduced to dryness under a stream of nitrogen at 30 °C and the residue was reconstituted with the mobile phase. 5 μL of the resulting solution was injected onto the LC–MS/MS system. A 4.6 mm × 150 mm, I.D. 5 μm, Agilent TC-C 18 column was used to perform the chromatographic analysis. The mobile phase consisted of ammonium formate buffer 0.010 M (adjusted to pH 4.3 with 1 M formic acid)/acetonitrile (20:80, v/ v) The chromatographic run time was 5 min per injection and flow rate was 0.6 mL/min. The retention time was 2.4 and 4.4 min for azatadine and IS, respectively. The tandem mass spectrometric detection mode was achieved with electrospray ionization (ESI) iron source and the multiple reaction monitoring (MRM) (291.3 → 248.2 m/ z for azatadine, 383.3 → 337.3 m/ z for IS) was operated in positive ion modes. The low limit of quantitation (LLOQ) was 0.05 ng/mL. The intra-day and inter-day precision of the quality control (QC) samples was 8.93–11.57% relative standard deviation (RSD). The inter-day accuracy of the QC samples was 96.83–105.07% of the nominal values.</description><identifier>ISSN: 1570-0232</identifier><identifier>EISSN: 1873-376X</identifier><identifier>DOI: 10.1016/j.jchromb.2011.05.050</identifier><identifier>PMID: 21737359</identifier><language>eng</language><publisher>Amsterdam: Elsevier B.V</publisher><subject>Analysis ; Analytical, structural and metabolic biochemistry ; antihistamines ; Azatadine ; Biological and medical sciences ; Chromatography, Liquid - methods ; Cyproheptadine - analogs &amp; derivatives ; Cyproheptadine - blood ; ethyl acetate ; formic acid ; Fundamental and applied biological sciences. 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B, Analytical technologies in the biomedical and life sciences</title><addtitle>J Chromatogr B Analyt Technol Biomed Life Sci</addtitle><description>A sensitive method using liquid chromatography with tandem mass spectrometric detection (LC–MS/MS) was developed and validated for the analysis of antihistamine drug azatadine in human plasma. Loratadine was used as internal standard (IS). Analytes were extracted from human plasma by liquid/liquid extraction using ethyl acetate. The organic phase was reduced to dryness under a stream of nitrogen at 30 °C and the residue was reconstituted with the mobile phase. 5 μL of the resulting solution was injected onto the LC–MS/MS system. A 4.6 mm × 150 mm, I.D. 5 μm, Agilent TC-C 18 column was used to perform the chromatographic analysis. 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B, Analytical technologies in the biomedical and life sciences</jtitle><addtitle>J Chromatogr B Analyt Technol Biomed Life Sci</addtitle><date>2011-08-01</date><risdate>2011</risdate><volume>879</volume><issue>23</issue><spage>2189</spage><epage>2193</epage><pages>2189-2193</pages><issn>1570-0232</issn><eissn>1873-376X</eissn><abstract>A sensitive method using liquid chromatography with tandem mass spectrometric detection (LC–MS/MS) was developed and validated for the analysis of antihistamine drug azatadine in human plasma. Loratadine was used as internal standard (IS). Analytes were extracted from human plasma by liquid/liquid extraction using ethyl acetate. The organic phase was reduced to dryness under a stream of nitrogen at 30 °C and the residue was reconstituted with the mobile phase. 5 μL of the resulting solution was injected onto the LC–MS/MS system. A 4.6 mm × 150 mm, I.D. 5 μm, Agilent TC-C 18 column was used to perform the chromatographic analysis. 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identifier ISSN: 1570-0232
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subjects Analysis
Analytical, structural and metabolic biochemistry
antihistamines
Azatadine
Biological and medical sciences
Chromatography, Liquid - methods
Cyproheptadine - analogs & derivatives
Cyproheptadine - blood
ethyl acetate
formic acid
Fundamental and applied biological sciences. Psychology
General pharmacology
Histamine Antagonists - blood
Human plasma
Humans
ionization
LC–MS/MS
liquid chromatography
Medical sciences
monitoring
nitrogen
Pharmacokinetics
Pharmacology. Drug treatments
quality control
Spectrometry, Mass, Electrospray Ionization - methods
streams
tandem mass spectrometry
Tandem Mass Spectrometry - methods
title Determination of azatadine in human plasma by liquid chromatography/tandem mass spectrometry
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