Enhancement of the LC/ESI-MS Quantitative Analysis of Ketoprofen Enantiomers through One-Pot Two-Step Stable Isotope-Coded Derivatization
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- 英文论文题名：Enhancement of the LC/ESI-MS Quantitative Analysis of Ketoprofen Enantiomers through One-Pot Two-Step Stable Isotope-Coded Derivatization
- 论文作者：Dan Ma ; Dongri Jin
- 英文论文作者：Dan Ma ; Dongri Jin ; Department of Chemistry ; College of Science ; Yanbian University
- 年：2016
- 作者机构：Department of Chemistry, College of Science, Yanbian University;
- 英文论文关键词：(S)-1-Methyl-4-(5-(3-aminopyrrolidin-1-yl)-2 ; 4-dinitro-phenyl)piperazine(APy-PPZ) ; LC/ESI-MS ; derivatize
- 会议召开时间：2016-07-01
- 会议录名称：中国化学会第30届学术年会摘要集-第二十三分会：复杂样品分离分析
- 语种：英文
- 分类号：O657.63
- 学会代码：ZGHY
- 会议名称：中国化学会第30届学术年会-第二十三分会 ; 复杂样品分离分析
- 会议地点：中国辽宁大连
- 主办单位：中国化学会
- 学会名称：中国化学会
- 页数：1
- 文件大小：364k
- 原文格式：D
- 会议级别：全国
摘要
This paper focuses on the development of an enhanced LC/ESI-MS method for the quantification of ketoprofen(KET) enantiomers.KET was first derivatized with(S)-1-methyl-4-(5-(3-aminopyrrolidin-l-yl)-2,4-dinitro-phenyl)piperazine(APy-PPZ),forming(KET-Apy-PPZ) derivative,and then was further converted to(KET-Apy-MPPZ)iodide or(d_3-KET-Apy-MPPZ) iodide by reacting with CH_3I or CD_3I in one-pot.This process attached not only a quaternary amine to analytes and enabled ESI-MS in the positive mode of ionization with common LC-mobile phases,but also a deuterium atom to analyte standards and enhancing quantification.The limits of detection were 1 nM(or 2 pmol/injection)(S/N = 3) for each standard KET enantiomer.After mixing experimental and control samples,they were analyzed by LC/ESI-MS.Abusolute quantification was achieved by adding differentially labeled KET standard to experimental samples containing unknown quantities of KET.Utility of the method was examined in the analysis of human saliva samples.
This paper focuses on the development of an enhanced LC/ESI-MS method for the quantification of ketoprofen(KET) enantiomers.KET was first derivatized with(S)-1-methyl-4-(5-(3-aminopyrrolidin-l-yl)-2,4-dinitro-phenyl)piperazine(APy-PPZ),forming(KET-Apy-PPZ) derivative,and then was further converted to(KET-Apy-MPPZ)iodide or(d_3-KET-Apy-MPPZ) iodide by reacting with CH_3I or CD_3I in one-pot.This process attached not only a quaternary amine to analytes and enabled ESI-MS in the positive mode of ionization with common LC-mobile phases,but also a deuterium atom to analyte standards and enhancing quantification.The limits of detection were 1 nM(or 2 pmol/injection)(S/N = 3) for each standard KET enantiomer.After mixing experimental and control samples,they were analyzed by LC/ESI-MS.Abusolute quantification was achieved by adding differentially labeled KET standard to experimental samples containing unknown quantities of KET.Utility of the method was examined in the analysis of human saliva samples.
This paper focuses on the development of an enhanced LC/ESI-MS method for the quantification of ketoprofen(KET) enantiomers.KET was first derivatized with(S)-1-methyl-4-(5-(3-aminopyrrolidin-l-yl)-2,4-dinitro-phenyl)piperazine(APy-PPZ),forming(KET-Apy-PPZ) derivative,and then was further converted to(KET-Apy-MPPZ)iodide or(d_3-KET-Apy-MPPZ) iodide by reacting with CH_3I or CD_3I in one-pot.This process attached not only a quaternary amine to analytes and enabled ESI-MS in the positive mode of ionization with common LC-mobile phases,but also a deuterium atom to analyte standards and enhancing quantification.The limits of detection were 1 nM(or 2 pmol/injection)(S/N = 3) for each standard KET enantiomer.After mixing experimental and control samples,they were analyzed by LC/ESI-MS.Abusolute quantification was achieved by adding differentially labeled KET standard to experimental samples containing unknown quantities of KET.Utility of the method was examined in the analysis of human saliva samples.
引文
[1]Shoujiro Ogawa,Hiroaki Tadokoro,Maho Sato,Takehisa Hanawa,Tatsuya Higashi*,Journal of Chromatography B.,2013,940;7.
[2]Shoujiro Ogawa,Hiroaki Tadokoro,Maho Sato,Tatsuya Higashi*,Journal of Pharmaceutical and Biomedical Analysis 2014,98;387(The present research was supported in part by the National Natural Science Foundation of China(21365022,21565027)).
[2]Shoujiro Ogawa,Hiroaki Tadokoro,Maho Sato,Tatsuya Higashi*,Journal of Pharmaceutical and Biomedical Analysis 2014,98;387(The present research was supported in part by the National Natural Science Foundation of China(21365022,21565027)).