PMID- 25022478
OWN - NLM
STAT- MEDLINE
DCOM- 20141010
LR  - 20171116
IS  - 1873-3778 (Electronic)
IS  - 0021-9673 (Linking)
VI  - 1358
DP  - 2014 Sep 5
TI  - Determination of sterols using liquid chromatography with off-line 
      surface-assisted laser desorption/ionization mass spectrometry.
PG  - 102-9
LID - S0021-9673(14)01020-6 [pii]
LID - 10.1016/j.chroma.2014.06.077 [doi]
AB  - A new method, reversed phase liquid chromatography with off-line surface-assisted 
      laser desorption/ionization mass spectrometry (RPLC-SALDI MS) for the 
      determination of brassicasterol (BR), cholesterol (CH), stigmasterol (ST), 
      campesterol (CA) and beta-sitosterol (SI) in oil samples has been developed. The 
      sample preparation consisted of alkaline saponification followed by extraction of 
      the unsaponificable fraction with diethyl ether. The recovery of the sterols 
      ranged from 91 to 95% with RSD less than 4%. Separation of the five major sterols 
      on a C18 column using methanol-water gradient was achieved in about 10min. An 
      on-line UV detector was employed for the initial sterol detection prior to 
      effluent deposition using a laboratory-built spotter with 1:73 splitter. Off-line 
      SALDI MS was then applied for mass determination/identification and 
      quantification of the separated sterols. Ionization of the nonpolar analytes was 
      achieved by silver ion cationization with silver nanoparticles used as the SALDI 
      matrix providing limits of detection 12, 6 and 11fmol for CH, ST and SI, 
      respectively. Because of the incorporated splitter, the effective limits of 
      detection of the RPLC-SALDI MS analysis were 4, 3 and 4pmol (or 0.08, 0.06 and 
      0.08mug/mL) for CH, ST and SI, respectively. For quantification, 6-ketocholestanol 
      (KE) was used as the internal standard. The method has been applied for the 
      identification and quantification of sterols in olive, linseed and sunflower oil 
      samples. The described off-line coupling of RPLC to SALDI MS represents an 
      alternative to GC-MS for analysis of nonpolar compounds.
CI  - Copyright (c) 2014 Elsevier B.V. All rights reserved.
FAU - Vrbkova, Blanka
AU  - Vrbkova B
AD  - Department of Chemistry, Faculty of Science, Masaryk University, Brno, Czech 
      Republic.
FAU - Roblova, Vendula
AU  - Roblova V
AD  - Department of Chemistry, Faculty of Science, Masaryk University, Brno, Czech 
      Republic.
FAU - Yeung, Edward S
AU  - Yeung ES
AD  - Department of Chemistry, Iowa State University, Ames, 50011 IA, USA.
FAU - Preisler, Jan
AU  - Preisler J
AD  - Department of Chemistry, Faculty of Science, Masaryk University, Brno, Czech 
      Republic; Central European Institute of Technology (CEITEC), Masaryk University, 
      Brno, Czech Republic. Electronic address: preisler@chemi.muni.cz.
LA  - eng
PT  - Journal Article
PT  - Research Support, Non-U.S. Gov't
DEP - 20140701
PL  - Netherlands
TA  - J Chromatogr A
JT  - Journal of chromatography. A
JID - 9318488
RN  - 0 (Cholestadienols)
RN  - 0 (Ketocholesterols)
RN  - 0 (Olive Oil)
RN  - 0 (Phytosterols)
RN  - 0 (Plant Oils)
RN  - 0 (Sitosterols)
RN  - 0 (Sunflower Oil)
RN  - 2B0KG2XFOF (brassicasterol)
RN  - 2V12D4A742 (6-ketocholestanol)
RN  - 3M4G523W1G (Silver)
RN  - 5L5O665639 (campesterol)
RN  - 5LI01C78DD (gamma-sitosterol)
RN  - 8001-26-1 (Linseed Oil)
RN  - 97C5T2UQ7J (Cholesterol)
RN  - 99WUK5D0Y8 (Stigmasterol)
SB  - IM
MH  - Cholestadienols/chemistry/*isolation & purification
MH  - Cholesterol/*analogs & derivatives/chemistry/isolation & purification
MH  - Chromatography, Reverse-Phase/methods/standards
MH  - Ketocholesterols/chemistry/isolation & purification
MH  - Linseed Oil/analysis/chemistry
MH  - Olive Oil
MH  - Phytosterols/chemistry/*isolation & purification
MH  - Plant Oils/analysis/chemistry
MH  - Reference Standards
MH  - Silver/chemistry
MH  - Sitosterols/chemistry/*isolation & purification
MH  - Spectrometry, Mass, Matrix-Assisted Laser Desorption-Ionization/methods/standards
MH  - Stigmasterol/chemistry/*isolation & purification
MH  - Sunflower Oil
OTO - NOTNLM
OT  - Off-line coupling
OT  - Oil sample
OT  - RPLC
OT  - SALDI MS
OT  - Silver nanoparticles
OT  - Sterols
EDAT- 2014/07/16 06:00
MHDA- 2014/10/11 06:00
CRDT- 2014/07/16 06:00
PHST- 2014/04/29 00:00 [received]
PHST- 2014/06/23 00:00 [revised]
PHST- 2014/06/24 00:00 [accepted]
PHST- 2014/07/16 06:00 [entrez]
PHST- 2014/07/16 06:00 [pubmed]
PHST- 2014/10/11 06:00 [medline]
AID - S0021-9673(14)01020-6 [pii]
AID - 10.1016/j.chroma.2014.06.077 [doi]
PST - ppublish
SO  - J Chromatogr A. 2014 Sep 5;1358:102-9. doi: 10.1016/j.chroma.2014.06.077. Epub 
      2014 Jul 1.