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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
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作者：Hirofumi Inoue ; Yasuhiko Sakata ; Hiroaki Nishio 等
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