Determination of sterols using liquid chromatography with
off-line surface-assisted laser desorption/ionization mass
spectrometry

J 2014

Determination of sterols using liquid chromatography with off-line surface-assisted laser desorption/ionization mass spectrometry

VRBKOVÁ, Blanka, Vendula ROBLOVÁ, Edward S. YEUNG and Jan PREISLER

Basic information

Original name

Determination of sterols using liquid chromatography with off-line surface-assisted laser desorption/ionization mass spectrometry

Authors

VRBKOVÁ, Blanka (203 Czech Republic, belonging to the institution), Vendula ROBLOVÁ (203 Czech Republic, belonging to the institution), Edward S. YEUNG (840 United States of America) and Jan PREISLER (203 Czech Republic, guarantor, belonging to the institution)

Edition

Journal of Chromatography A, Amsterdam, Elsevier, 2014, 0021-9673

Other information

Language

English

Type of outcome

Článek v odborném periodiku

Field of Study

10406 Analytical chemistry

Country of publisher

Netherlands

Confidentiality degree

není předmětem státního či obchodního tajemství

References:

URL

Impact factor

Impact factor: 4.169

RIV identification code

RIV/00216224:14740/14:00073825

Organization unit

Central European Institute of Technology

DOI

http://dx.doi.org/10.1016/j.chroma.2014.06.077

UT WoS

000340979200013

Keywords in English

sterols; SALDI MS; HPLC

Abstract

V originále

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 b-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 10 min. 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 11 fmol 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 4 pmol (or 0.08, 0.06 and 0.08 ug/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.

Links

ED1.1.00/02.0068, research and development project

Name: CEITEC - central european institute of technology

GAP206/12/0538, research and development project

Name: Nové strategie úpravy vzorků pro desorpční hmotnostní spektrometrii

Investor: Czech Science Foundation

Citovat

VRBKOVÁ, Blanka, Vendula ROBLOVÁ, Edward S. YEUNG and Jan PREISLER. Determination of sterols using liquid chromatography with off-line surface-assisted laser desorption/ionization mass spectrometry. Journal of Chromatography A. Amsterdam: Elsevier, 2014, vol. 1358, 5 September, p. 102-109. ISSN 0021-9673. Available from: https://dx.doi.org/10.1016/j.chroma.2014.06.077.

@article{1196667,
   author = {Vrbková, Blanka and Roblová, Vendula and Yeung, Edward S. and Preisler, Jan},
   article_location = {Amsterdam},
   article_number = {5 September},
   doi = {http://dx.doi.org/10.1016/j.chroma.2014.06.077},
   keywords = {sterols; SALDI MS; HPLC},
   language = {eng},
   issn = {0021-9673},
   journal = {Journal of Chromatography A},
   title = {Determination of sterols using liquid chromatography with off-line surface-assisted laser desorption/ionization mass spectrometry},
   url = {http://www.sciencedirect.com/science/article/pii/S0021967314010206},
   volume = {1358},
   year = {2014}
}

TY  - JOUR
ID  - 1196667
AU  - Vrbková, Blanka - Roblová, Vendula - Yeung, Edward S. - Preisler, Jan
PY  - 2014
TI  - Determination of sterols using liquid chromatography with off-line surface-assisted laser desorption/ionization mass spectrometry
JF  - Journal of Chromatography A
VL  - 1358
IS  - 5 September
SP  - 102-109
EP  - 102-109
PB  - Elsevier
SN  - 00219673
KW  - sterols
KW  - SALDI MS
KW  - HPLC
UR  - http://www.sciencedirect.com/science/article/pii/S0021967314010206
L2  - http://www.sciencedirect.com/science/article/pii/S0021967314010206
N2  - 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 b-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 10 min. 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 11 fmol 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 4 pmol (or 0.08, 0.06 and 0.08 ug/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.
ER  -

VRBKOVÁ, Blanka, Vendula ROBLOVÁ, Edward S. YEUNG and Jan PREISLER. Determination of sterols using liquid chromatography with off-line surface-assisted laser desorption/ionization mass spectrometry. \textit{Journal of Chromatography A}. Amsterdam: Elsevier, 2014, vol.~1358, 5 September, p.~102-109. ISSN~0021-9673. Available from: https://dx.doi.org/10.1016/j.chroma.2014.06.077.

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