色谱Issue(7)：779-783,5.DOI:10.3724/SP.J.1123.2014.03030
同位素稀释-气相色谱-质谱法检测大鼠血浆中的内源性胍丁胺
Determination of endogenous agmatine in rat plasma by isotope dilution-gas chromatography-mass spectrometry
丘忠丽 1林缨 2熊志立 1谢剑炜3
作者信息
- 1. 抗毒药物与毒理学国家重点实验室，军事医学科学院毒物药物研究所，北京 100850
- 2. 沈阳药科大学药学院，辽宁 沈阳 110016
- 3. 沈阳药科大学药学院，辽宁 沈阳 110016
- 折叠
摘要
Abstract
A method for the determination of endogenous agmatine in rat plasma was devel-oped by isotope dilution-gas chromatography-negative chemical ionization mass spectrometry ( GC-NCI/MS). The plasma samples were analyzed after protein precipitation,evaporation, derivatization by hexafluoroacetone( HFAA),and clean-up on a Florisil SPE column. The GC-MS analysis utilized stable isotope d8-agmatine as internal standard. The samples after treatment were tested by negative chemical ionization with selected ion monitoring( SIM )which was set at m/z 492( molecular ion of agmatine)and m/z 500( molecular ion of internal standard). The limit of detection( LOD ) of agmatine standard solution was 0. 005 7 ng/mL. The calibration curve of the agmatine spiked in rat plasma showed a good linear relationship at the range of 1. 14-57. 0 ng/mL( r=0. 997 ). The recoveries of agmatine spiked in rat plasma ranged from 92. 3% to 109. 8%. Inter-day and intra-day precisions were less than 15%. The average concen-tration level of agmatine in rat plasma was(22±9)ng/mL,and there was no significant differ-ence between male and female SD rats( p﹥0. 05). The method is high sensitive and specific, and can be used for the determination of endogenous agmatine in plasma. It provides a strong support for the subsequent research of agmatine.关键词
气相色谱-负离子化学电离质谱/同位素稀释/内源性胍丁胺/血浆/大鼠Key words
gas chromatography-negative chemical ionization mass spectrometry ( GC-NCI/MS)/isotope-dilution/endogenous agmatine/plasma/rat分类
化学化工引用本文复制引用
丘忠丽,林缨,熊志立,谢剑炜..同位素稀释-气相色谱-质谱法检测大鼠血浆中的内源性胍丁胺[J].色谱,2014,(7):779-783,5.
