000060964 001__ 60964
000060964 005__ 20170502141033.0
000060964 0247_ $$2doi$$a10.1016/j.talanta.2014.10.029
000060964 0248_ $$2sideral$$a88100
000060964 037__ $$aART-2015-88100
000060964 041__ $$aeng
000060964 100__ $$0(orcid)0000-0001-8830-6554$$aMendiara Negredo, Isabel
000060964 245__ $$aOnline solid-phase extraction–liquid chromatography–mass spectrometry to determine free sterols in human serum
000060964 260__ $$c2015
000060964 5060_ $$aAccess copy available to the general public$$fUnrestricted
000060964 5203_ $$an automated method for analyzing free non-cholesterol sterols in human serum using online solid phase extraction–liquid chromatography–mass spectrometry is proposed herein. The method allows the determination of three phytosterols (sitosterol, stigmasterol and campesterol) and two cholesterol precursors (desmosterol and lanosterol). The analysis of sterols in human serum is critical in the study of cholesterol-related disorders, such as inherited familial hypercholesterolemias. Special effort was made to isolate the analytes from the serum lipoproteins, their natural conveyance through the bloodstream. The sample treatment consisted of a Bligh–Dyer extraction followed by dilution of the extract. This treatment allowed the sample to be injected into the online system and ensured the correct detection of the analytes, while avoiding the matrix effects commonly related to serum samples.
The analytical performance showed linear ranges that covered two orders of magnitude, with correlation coefficients above 0.99. Limits of detection and quantification ranged from 0.2 ng/mL to 13 ng/mL and from 1.0 ng/mL to 43 ng/mL, respectively. Recovery when spiking serum with a half or a tenth of the average concentration reported in human serum ranged from 99% to 111% and from 102% to 120%, respectively. Intra-day precision and inter-day precision were below 20%.
000060964 536__ $$9info:eu-repo/grantAgreement/ES/DGA/PI037-09$$9info:eu-repo/grantAgreement/ES/DGA/T10
000060964 540__ $$9info:eu-repo/semantics/openAccess$$aby-nc-nd$$uhttp://creativecommons.org/licenses/by-nc-nd/3.0/es/
000060964 590__ $$a4.035$$b2015
000060964 591__ $$aCHEMISTRY, ANALYTICAL$$b9 / 75 = 0.12$$c2015$$dQ1$$eT1
000060964 655_4 $$ainfo:eu-repo/semantics/article$$vinfo:eu-repo/semantics/acceptedVersion
000060964 700__ $$0(orcid)0000-0002-3399-9987$$aBentayeb Martinez, Karim
000060964 700__ $$0(orcid)0000-0003-2685-5739$$aNerín de la Puerta, Cristina$$uUniversidad de Zaragoza
000060964 700__ $$0(orcid)0000-0001-8893-0963$$aDomeño Recalde, Celia$$uUniversidad de Zaragoza
000060964 7102_ $$12009$$2750$$aUniversidad de Zaragoza$$bDepartamento de Química Analítica$$cQuímica Analítica
000060964 773__ $$g132 (2015), 690-697$$pTalanta$$tTALANTA$$x0039-9140
000060964 8564_ $$s1533918$$uhttps://zaguan.unizar.es/record/60964/files/texto_completo.pdf$$yPostprint
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000060964 909CO $$ooai:zaguan.unizar.es:60964$$particulos$$pdriver
000060964 951__ $$a2017-05-02-12:03:59
000060964 980__ $$aARTICLE