Analysis of non-derivatised bacteriohopanepolyols by ultrahigh-performance liquid chromatography/tandem mass spectrometry.
Analysis of non-derivatised bacteriohopanepolyols by ultrahigh-performance liquid chromatography/tandem mass spectrometry.
复制标题
通过超高效液相色谱/串联质谱法分析非衍生化细菌藿烷多元醇。
DOI：
10.1002/rcm.7696
复制
发表时间：
2016
期刊：
影响因子：
--
通讯作者：
C. Spencer
中科院分区：
文献类型：
--
作者：
H. Talbot;F. Sidgwick;J. Bischoff;Kate A Osborne;D. Rush;A. Sherry;C. Spencer
基本原理
RATIONALE
Traditional investigation of bacteriohopanepolyols (BHPs) has relied on derivatisation by acetylation prior to gas chromatography/mass spectrometry (GC/MS) or liquid chromatography/MS (LC/MS) analysis. Here, modern chromatographic techniques (ultrahigh-performance liquid chromatography (UPLC)) and new column chemistries were tested to develop a method for BHP analysis without the need for derivatisation.
METHODS
Bacterial culture and sedimentary lipid extracts were analysed using a Waters Acquity Xevo TQ-S triple quadrupole mass spectrometer in positive ion atmospheric pressure chemical ionisation (APCI) mode. Waters BEH C18 and ACE Excel C18 were the central columns evaluated using a binary solvent gradient with 0.1% formic acid in the polar solvent phase in order to optimise performance and selectivity.
RESULTS
Non-amine BHPs and adenosylhopane showed similar performance on each C18 column; however, BHP-containing terminal amines were only identified eluting from the ultra-inert ACE Excel C18 column. APCI-MS/MS product ion scans revealed significant differences in fragmentation pathways from previous methods for acetylated compounds. The product ions used for targeted multiple reaction monitoring (MRM) are summarised.
CONCLUSIONS
UPLC/MS/MS analysis using an ACE Excel C18 column produced superior separation for amine-containing BHPs and reduced run times from 60 to 9 min compared with previous methods. Unexpected variations in fragmentation pathways between structural subgroups must be taken into account when optimising MRM transitions for future quantitative studies. Copyright © 2016 John Wiley & Sons, Ltd.
影响因子：
3
作者：
A. D. Selver;R. Sparkes;J. Bischoff;H. Talbot;Ö. Gustafsson;I. Semiletov;O. Dudarev;S. Boult;B. Dongen
通讯作者：
A. D. Selver;R. Sparkes;J. Bischoff;H. Talbot;Ö. Gustafsson;I. Semiletov;O. Dudarev;S. Boult;B. Dongen
影响因子：
4.9
作者：
Bischoff, Juliane;Sparkes, Robert B.;Talbot, Helen M.
通讯作者：
Talbot, Helen M.
刚果河流域热带土壤和沉积物中的细菌藿烷多元醇
影响因子：
3
作者：
Spencer-Jones C
通讯作者：
Spencer-Jones C