High-performance liquid chromatography versus solid-phase extraction for post-derivatization cleanup prior to gas chromatography-electron-capture negative-ion mass spectrometry of N1,N3-bis-(pentafluorobenzyl)-N7- (2-[pentafluorobenzyloxy]ethyl)xanthine,
High-performance liquid chromatography versus solid-phase extraction for post-derivatization cleanup prior to gas chromatography-electron-capture negative-ion mass spectrometry of N1,N3-bis-(pentafluorobenzyl)-N7- (2-[pentafluorobenzyloxy]ethyl)xanthine,
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N1,N3-双-(五氟苄基)-N7-(2-[五氟苄氧基]乙基)黄嘌呤的气相色谱-电子捕获负离子质谱分析之前的衍生化后净化的高效液相色谱与固相萃取
DOI：
10.1016/0021-9673(93)80351-8
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发表时间：
1993
期刊：
影响因子：
--
通讯作者：
Giese,RW
中科院分区：
文献类型：
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作者：
Saha,M;Giese,RW
N7-以（2-羟乙基）黄嘌呤（N7-HEX）为标准品，通过以下步骤在低皮摩尔水平进行测定：（1）用五氟苄基溴衍生化：（2）衍生后样品用反相高效液相色谱（HPLC）或硅胶固相萃取净化;（3）气相色谱电子捕获负离子质谱（GC-ECNI-MS）分离/检测。应用于95 pg（0.48 pmol）N7-HEX的两种样品净化程序的产物平均产率相当：HPLC为60%;固相萃取为56%。HPLC净化后，反应空白（0 pg N7-HEX）显示干扰GC-ECNI-MS峰。固相萃取没有遇到这个问题，沿着其更大的便利性，使其成为衍生后样品净化的首选技术。
N7-(2-Hydroxyethyl)xanthine (N7-HEX), as a standard, has been measured at the low picomole level by the following sequence of steps: (1) derivatization with pentafluorobenzyl bromide: (2) post-derivatization sample cleanup by reversed-phase high-performance liquid chromatography (HPLC) or silica solid-phase extraction; and (3) separation/detection by gas chromatography electron-capture negative-ion mass spectrometry (GC-ECNI-MS). The average yield of product from the two sample cleanup procedures applied to 95 pg (0.48 pmol) of N7-HEX was comparable: 60% for HPLC; 56% for solid-phase extraction. The reaction blanks (0 pg N7-HEX) showed an interfering GC-ECNI-MS peak after HPLC cleanup. This problem was not encountered with solid-phase extraction, which, along with its greater convenience, made it the preferred technique for post-derivatization sample cleanup.