A simplified liquid chromatography tandem mass spectrometry assay, using on-line solid-phase extraction, for the quantitation of cortisol in saliva and comparison with a routine DELFIA method

Background We have developed a liquid chromatography tandem mass spectrometry (LC-MS/MS) method for measuring salivary cortisol, which requires only 200 μL sample and no extraction. Methods Sample (200 μL) and 25 μL internal standard were added directly to a 96-deep-well plate. Of this, 50 μL was lo...

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Published in:Annals of clinical biochemistry 2010-03, Vol.47 (2), p.131-136
Main Authors: Owen, L J, Haslam, S, Adaway, J E, Wood, P, Glenn, C, Keevil, B G
Format: Article
Language:English
Subjects:
Adult
Biological Assay - methods
Chromatography, Liquid - methods
Clinical Laboratory Techniques
Female
Fluorescent Antibody Technique - methods
Humans
Hydrocortisone - analysis
Immunoassay - methods
Lanthanoid Series Elements - analysis
Male
Middle Aged
Reference Values
Saliva - chemistry
Solid Phase Extraction - methods
Tandem Mass Spectrometry - methods
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cited_by cdi_FETCH-LOGICAL-c333t-7663b5f0445767b4b36ed56167bfbc8ce1999e3d5102c8cae8a5eaab1b97cb593
cites cdi_FETCH-LOGICAL-c333t-7663b5f0445767b4b36ed56167bfbc8ce1999e3d5102c8cae8a5eaab1b97cb593
container_end_page 136
container_issue 2
container_start_page 131
container_title Annals of clinical biochemistry
container_volume 47
creator Owen, L J
Haslam, S
Adaway, J E
Wood, P
Glenn, C
Keevil, B G
description Background We have developed a liquid chromatography tandem mass spectrometry (LC-MS/MS) method for measuring salivary cortisol, which requires only 200 μL sample and no extraction. Methods Sample (200 μL) and 25 μL internal standard were added directly to a 96-deep-well plate. Of this, 50 μL was loaded onto a guard cartridge, the cartridge was then washed and the eluate was diverted to waste. The compounds were eluted from the guard cartridge onto the C18 analytical column. Cortisol and deuterated cortisol were monitored using transitions m/z 363.2 > 121.1 and 365.1 > 122.2, respectively. Results The method had a lower limit of quantitation of 2 nmol/L. Intra-assay and inter-assay imprecision were better than 9.5%. Comparison with an established dissociation enhanced lanthanide fluorescent immunoassay (DELFIA) gave good agreement for the majority of samples; LC-MS/MS = 1.0065 × DELFIA − 3.7 (n = 130). The reference range was determined to be 5.8–45.7 nmol/L at 08:00 h and
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Methods Sample (200 μL) and 25 μL internal standard were added directly to a 96-deep-well plate. Of this, 50 μL was loaded onto a guard cartridge, the cartridge was then washed and the eluate was diverted to waste. The compounds were eluted from the guard cartridge onto the C18 analytical column. Cortisol and deuterated cortisol were monitored using transitions m/z 363.2 &gt; 121.1 and 365.1 &gt; 122.2, respectively. Results The method had a lower limit of quantitation of 2 nmol/L. Intra-assay and inter-assay imprecision were better than 9.5%. Comparison with an established dissociation enhanced lanthanide fluorescent immunoassay (DELFIA) gave good agreement for the majority of samples; LC-MS/MS = 1.0065 × DELFIA − 3.7 (n = 130). The reference range was determined to be 5.8–45.7 nmol/L at 08:00 h and &lt;6.4 nmol/L at 23:00 h (n = 44). Conclusions We have developed a simple, robust assay to measure salivary cortisol using on-line solid-phase extraction to reduce sample clean-up requirements.</description><identifier>ISSN: 0004-5632</identifier><identifier>EISSN: 1758-1001</identifier><identifier>DOI: 10.1258/acb.2009.009053</identifier><identifier>PMID: 20150214</identifier><language>eng</language><publisher>London, England: SAGE Publications</publisher><subject>Adult ; Biological Assay - methods ; Chromatography, Liquid - methods ; Clinical Laboratory Techniques ; Female ; Fluorescent Antibody Technique - methods ; Humans ; Hydrocortisone - analysis ; Immunoassay - methods ; Lanthanoid Series Elements - analysis ; Male ; Middle Aged ; Reference Values ; Saliva - chemistry ; Solid Phase Extraction - methods ; Tandem Mass Spectrometry - methods</subject><ispartof>Annals of clinical biochemistry, 2010-03, Vol.47 (2), p.131-136</ispartof><rights>2010 The Association for Clinical Biochemistry</rights><lds50>peer_reviewed</lds50><woscitedreferencessubscribed>false</woscitedreferencessubscribed><citedby>FETCH-LOGICAL-c333t-7663b5f0445767b4b36ed56167bfbc8ce1999e3d5102c8cae8a5eaab1b97cb593</citedby><cites>FETCH-LOGICAL-c333t-7663b5f0445767b4b36ed56167bfbc8ce1999e3d5102c8cae8a5eaab1b97cb593</cites></display><links><openurl>$$Topenurl_article</openurl><openurlfulltext>$$Topenurlfull_article</openurlfulltext><thumbnail>$$Tsyndetics_thumb_exl</thumbnail><link.rule.ids>314,780,784,27924,27925,79364</link.rule.ids><backlink>$$Uhttps://www.ncbi.nlm.nih.gov/pubmed/20150214$$D View this record in MEDLINE/PubMed$$Hfree_for_read</backlink></links><search><creatorcontrib>Owen, L J</creatorcontrib><creatorcontrib>Haslam, S</creatorcontrib><creatorcontrib>Adaway, J E</creatorcontrib><creatorcontrib>Wood, P</creatorcontrib><creatorcontrib>Glenn, C</creatorcontrib><creatorcontrib>Keevil, B G</creatorcontrib><title>A simplified liquid chromatography tandem mass spectrometry assay, using on-line solid-phase extraction, for the quantitation of cortisol in saliva and comparison with a routine DELFIA method</title><title>Annals of clinical biochemistry</title><addtitle>Ann Clin Biochem</addtitle><description>Background We have developed a liquid chromatography tandem mass spectrometry (LC-MS/MS) method for measuring salivary cortisol, which requires only 200 μL sample and no extraction. Methods Sample (200 μL) and 25 μL internal standard were added directly to a 96-deep-well plate. Of this, 50 μL was loaded onto a guard cartridge, the cartridge was then washed and the eluate was diverted to waste. The compounds were eluted from the guard cartridge onto the C18 analytical column. Cortisol and deuterated cortisol were monitored using transitions m/z 363.2 &gt; 121.1 and 365.1 &gt; 122.2, respectively. Results The method had a lower limit of quantitation of 2 nmol/L. Intra-assay and inter-assay imprecision were better than 9.5%. Comparison with an established dissociation enhanced lanthanide fluorescent immunoassay (DELFIA) gave good agreement for the majority of samples; LC-MS/MS = 1.0065 × DELFIA − 3.7 (n = 130). The reference range was determined to be 5.8–45.7 nmol/L at 08:00 h and &lt;6.4 nmol/L at 23:00 h (n = 44). 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Conclusions We have developed a simple, robust assay to measure salivary cortisol using on-line solid-phase extraction to reduce sample clean-up requirements.</abstract><cop>London, England</cop><pub>SAGE Publications</pub><pmid>20150214</pmid><doi>10.1258/acb.2009.009053</doi><tpages>6</tpages></addata></record>
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subjects Adult
Biological Assay - methods
Chromatography, Liquid - methods
Clinical Laboratory Techniques
Female
Fluorescent Antibody Technique - methods
Humans
Hydrocortisone - analysis
Immunoassay - methods
Lanthanoid Series Elements - analysis
Male
Middle Aged
Reference Values
Saliva - chemistry
Solid Phase Extraction - methods
Tandem Mass Spectrometry - methods
title A simplified liquid chromatography tandem mass spectrometry assay, using on-line solid-phase extraction, for the quantitation of cortisol in saliva and comparison with a routine DELFIA method
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