FarFaR - Pharmacy Repository
University of Belgrade, Faculty of Pharmacy
    • English
    • Српски
    • Српски (Serbia)
  • English 
    • English
    • Serbian (Cyrillic)
    • Serbian (Latin)
  • Login
View Item 
  •   FarFaR
  • Pharmacy
  • Radovi istraživača / Researchers’ publications
  • View Item
  •   FarFaR
  • Pharmacy
  • Radovi istraživača / Researchers’ publications
  • View Item
JavaScript is disabled for your browser. Some features of this site may not work without it.

Preanalytical and analytical challenges in gas chromatographic determination of cholesterol synthesis and absorption markers

Authorized Users Only
2018
Authors
Gojković, Tamara
Vladimirov, Sandra
Spasojević-Kalimanovska, Vesna
Zeljković, Aleksandra
Vekić, Jelena
Arsenijević, Jelena
Đuričić, Ivana
Šobajić, Slađana
Jelić-Ivanović, Zorana
Article (Published version)
Metadata
Show full item record
Abstract
Introduction: Cholesterol homeostasis disruption contributes to the development of different pathologies. Non cholesterol sterols (NCSs) serve as cholesterol synthesis markers (desmosterol and lathosterol), and cholesterol absorption surrogate markers (campesterol, stigmasterol and beta-sitosterol). The study aimed to resolve certain new pre-analytical and analytical problems and ensure a reliable and validated method. Materials and methods: Method optimization, validation and stability studies were executed in human serum and plasma. Freeze-thaw cycles were done with and without antioxidant. Gas chromatography-mass spectrometer (GC-MS) was used for NCSs confirmation and plasticizer identification, while GC-flame ionization detector (GC-FID) was used for NCSs quantitation. Results: Infra-and inter-assay variabilities for all NCSs were 2.75-9.55% and 5.80-7.75% for plasma and 3.10-5.72% and 3.05-10.92% for serum, respectively. Recovery studies showed satisfactory percentage errors for a...ll NCSs: 93.4-105.7% in plasma and 87.5-106.9 in serum. Derivatized samples were stable up to 7 days at 20 degrees C and derivatization yield was affected by presence of plasticizers. Fatty acid amids were identified as interfering plastic leachates. Statistically different NCSs concentrations were observed after the 1st freeze-thaw cycle, in antioxidant-free samples, and after the 4th cycle in antioxidant-enriched samples. Conclusions: All of the in-house procedures proved to be useful for minimizing the preanalytical and analytical variations, as proven by the validation results.

Keywords:
Method validation / Sterols / Stability / Freeze-thaw / Plasticizers
Source:
Clinica Chimica Acta, 2018, 478, 74-81
Publisher:
  • Elsevier Science BV, Amsterdam
Funding / projects:
  • Interactive role of dyslipidemia, oxidative stress and inflammation in atherosclerosis and other diseases: genetic and biochemical markers (RS-175035)

DOI: 10.1016/j.cca.2017.12.032

ISSN: 0009-8981

PubMed: 29274328

WoS: 000425070000013

Scopus: 2-s2.0-85039173890
[ Google Scholar ]
5
4
URI
https://farfar.pharmacy.bg.ac.rs/handle/123456789/3185
Collections
  • Radovi istraživača / Researchers’ publications
Institution/Community
Pharmacy
TY  - JOUR
AU  - Gojković, Tamara
AU  - Vladimirov, Sandra
AU  - Spasojević-Kalimanovska, Vesna
AU  - Zeljković, Aleksandra
AU  - Vekić, Jelena
AU  - Arsenijević, Jelena
AU  - Đuričić, Ivana
AU  - Šobajić, Slađana
AU  - Jelić-Ivanović, Zorana
PY  - 2018
UR  - https://farfar.pharmacy.bg.ac.rs/handle/123456789/3185
AB  - Introduction: Cholesterol homeostasis disruption contributes to the development of different pathologies. Non cholesterol sterols (NCSs) serve as cholesterol synthesis markers (desmosterol and lathosterol), and cholesterol absorption surrogate markers (campesterol, stigmasterol and beta-sitosterol). The study aimed to resolve certain new pre-analytical and analytical problems and ensure a reliable and validated method. Materials and methods: Method optimization, validation and stability studies were executed in human serum and plasma. Freeze-thaw cycles were done with and without antioxidant. Gas chromatography-mass spectrometer (GC-MS) was used for NCSs confirmation and plasticizer identification, while GC-flame ionization detector (GC-FID) was used for NCSs quantitation. Results: Infra-and inter-assay variabilities for all NCSs were 2.75-9.55% and 5.80-7.75% for plasma and 3.10-5.72% and 3.05-10.92% for serum, respectively. Recovery studies showed satisfactory percentage errors for all NCSs: 93.4-105.7% in plasma and 87.5-106.9 in serum. Derivatized samples were stable up to 7 days at 20 degrees C and derivatization yield was affected by presence of plasticizers. Fatty acid amids were identified as interfering plastic leachates. Statistically different NCSs concentrations were observed after the 1st freeze-thaw cycle, in antioxidant-free samples, and after the 4th cycle in antioxidant-enriched samples. Conclusions: All of the in-house procedures proved to be useful for minimizing the preanalytical and analytical variations, as proven by the validation results.
PB  - Elsevier Science BV, Amsterdam
T2  - Clinica Chimica Acta
T1  - Preanalytical and analytical challenges in gas chromatographic determination of cholesterol synthesis and absorption markers
VL  - 478
SP  - 74
EP  - 81
DO  - 10.1016/j.cca.2017.12.032
ER  - 
@article{
author = "Gojković, Tamara and Vladimirov, Sandra and Spasojević-Kalimanovska, Vesna and Zeljković, Aleksandra and Vekić, Jelena and Arsenijević, Jelena and Đuričić, Ivana and Šobajić, Slađana and Jelić-Ivanović, Zorana",
year = "2018",
abstract = "Introduction: Cholesterol homeostasis disruption contributes to the development of different pathologies. Non cholesterol sterols (NCSs) serve as cholesterol synthesis markers (desmosterol and lathosterol), and cholesterol absorption surrogate markers (campesterol, stigmasterol and beta-sitosterol). The study aimed to resolve certain new pre-analytical and analytical problems and ensure a reliable and validated method. Materials and methods: Method optimization, validation and stability studies were executed in human serum and plasma. Freeze-thaw cycles were done with and without antioxidant. Gas chromatography-mass spectrometer (GC-MS) was used for NCSs confirmation and plasticizer identification, while GC-flame ionization detector (GC-FID) was used for NCSs quantitation. Results: Infra-and inter-assay variabilities for all NCSs were 2.75-9.55% and 5.80-7.75% for plasma and 3.10-5.72% and 3.05-10.92% for serum, respectively. Recovery studies showed satisfactory percentage errors for all NCSs: 93.4-105.7% in plasma and 87.5-106.9 in serum. Derivatized samples were stable up to 7 days at 20 degrees C and derivatization yield was affected by presence of plasticizers. Fatty acid amids were identified as interfering plastic leachates. Statistically different NCSs concentrations were observed after the 1st freeze-thaw cycle, in antioxidant-free samples, and after the 4th cycle in antioxidant-enriched samples. Conclusions: All of the in-house procedures proved to be useful for minimizing the preanalytical and analytical variations, as proven by the validation results.",
publisher = "Elsevier Science BV, Amsterdam",
journal = "Clinica Chimica Acta",
title = "Preanalytical and analytical challenges in gas chromatographic determination of cholesterol synthesis and absorption markers",
volume = "478",
pages = "74-81",
doi = "10.1016/j.cca.2017.12.032"
}
Gojković, T., Vladimirov, S., Spasojević-Kalimanovska, V., Zeljković, A., Vekić, J., Arsenijević, J., Đuričić, I., Šobajić, S.,& Jelić-Ivanović, Z.. (2018). Preanalytical and analytical challenges in gas chromatographic determination of cholesterol synthesis and absorption markers. in Clinica Chimica Acta
Elsevier Science BV, Amsterdam., 478, 74-81.
https://doi.org/10.1016/j.cca.2017.12.032
Gojković T, Vladimirov S, Spasojević-Kalimanovska V, Zeljković A, Vekić J, Arsenijević J, Đuričić I, Šobajić S, Jelić-Ivanović Z. Preanalytical and analytical challenges in gas chromatographic determination of cholesterol synthesis and absorption markers. in Clinica Chimica Acta. 2018;478:74-81.
doi:10.1016/j.cca.2017.12.032 .
Gojković, Tamara, Vladimirov, Sandra, Spasojević-Kalimanovska, Vesna, Zeljković, Aleksandra, Vekić, Jelena, Arsenijević, Jelena, Đuričić, Ivana, Šobajić, Slađana, Jelić-Ivanović, Zorana, "Preanalytical and analytical challenges in gas chromatographic determination of cholesterol synthesis and absorption markers" in Clinica Chimica Acta, 478 (2018):74-81,
https://doi.org/10.1016/j.cca.2017.12.032 . .

DSpace software copyright © 2002-2015  DuraSpace
About FarFaR - Pharmacy Repository | Send Feedback

OpenAIRERCUB
 

 

All of DSpaceCommunitiesAuthorsTitlesSubjectsThis institutionAuthorsTitlesSubjects

Statistics

View Usage Statistics

DSpace software copyright © 2002-2015  DuraSpace
About FarFaR - Pharmacy Repository | Send Feedback

OpenAIRERCUB