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  • 标题:A Simple and Highly Sensitive HPLC Method with Fluorescent Detection for Determination of Pipecolic Acid in Mouse Brain Areas
  • 本地全文:下载
  • 作者:Hirofumi Inoue ; Yasuhiko Sakata ; Hiroaki Nishio
  • 期刊名称:Biological and Pharmaceutical Bulletin
  • 印刷版ISSN:0918-6158
  • 电子版ISSN:1347-5215
  • 出版年度:2011
  • 卷号:34
  • 期号:2
  • 页码:287-289
  • DOI:10.1248/bpb.34.287
  • 出版社:The Pharmaceutical Society of Japan
  • 摘要:A simple and highly sensitive high-performance liquid chromatography method for the determination of pipecolic acid in mouse brain areas was developed. After homogenization of brain and pretreatment with o -phthalaldehyde, the pipecolic acid and (2 S ,3 S )-3-methylpyrrolidine-2-carboxylic acid (internal standard) were derivatized with 4-(5,6-dimethoxy-2-phthalimidinyl)-2-methoxyphenylsulfonyl chloride at 70 °C for 15 min in basic medium (pH 9.0). The fluorescent derivatives of pipecolic acid and internal standard were separated on a reversed-phase column by stepwise elution using acetic acid (30 m M )–acetonitrile at 50 °C and detected by fluorescence measurement at 316 nm (excitation) and 403 nm (emission). The detection limit (signal-to-noise ratio=3) of pipecolic acid was 13 fmol per injection. The recovery was about 106.7%. The precision (relative standard deviation) was 3.2%.
  • 关键词:pipecolic acid;brain;fluorescent detection;HPLC;4-(5,6-dimethoxy-2-phthalimidinyl)-2-methoxyphenylsulfonyl chloride
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