Measurement of salicylic acid in human serum using stable isotope dilution and gas chromatography–mass spectrometry

A simple, highly selective, and sensitive method using stable isotope dilution and gas chromatography–mass spectrometry has been developed to quantify salicylic acid (SA) at concentrations naturally occurring in biological fluids, such as in the serum of subjects not taking aspirin. After extraction...

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Published in	Analytical biochemistry Vol. 354; no. 2; pp. 274 - 278
Main Authors	Battezzati, A., Fiorillo, G., Spadafranca, A., Bertoli, S., Testolin, G.
Format	Journal Article
Language	English
Published	United States Elsevier Inc 15.07.2006
Subjects	Blood Chemical Analysis - methods Blood Chemical Analysis - standards Blood Chemical Analysis - statistics & numerical data Deuterium Gas chromatography mass–spectrometry Gas Chromatography-Mass Spectrometry - methods Gas Chromatography-Mass Spectrometry - standards Gas Chromatography-Mass Spectrometry - statistics & numerical data Humans Isotope Labeling - methods Reference Standards Reproducibility of Results Salicylic Acid - blood Salicylic Acid - chemistry Salicylic Acid - standards Salycilic acid Serum Stable isotopes Serum Gas chromatography mass–spectrometry Salycilic acid Stable isotopes
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ISSN	0003-2697 1096-0309
DOI	10.1016/j.ab.2006.05.009

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Abstract	A simple, highly selective, and sensitive method using stable isotope dilution and gas chromatography–mass spectrometry has been developed to quantify salicylic acid (SA) at concentrations naturally occurring in biological fluids, such as in the serum of subjects not taking aspirin. After extraction of liquid–liquid with diethyl ether and ethyl acetate and preparation of the tert-butyldimethylsilyl derivative, SA content was detected using deuterated SA as internal standard. The mean recovery of SA from serum was 85 ± 6%. Intra- and interday precision and % relative error were <15% in all cases.With a detection limit of 0.6 ng and a quantification limit of 2 ng, the method is therefore also adequate for population studies because of the small amount of blood necessary to perform the analyses.
AbstractList	A simple, highly selective, and sensitive method using stable isotope dilution and gas chromatography–mass spectrometry has been developed to quantify salicylic acid (SA) at concentrations naturally occurring in biological fluids, such as in the serum of subjects not taking aspirin. After extraction of liquid–liquid with diethyl ether and ethyl acetate and preparation of the tert-butyldimethylsilyl derivative, SA content was detected using deuterated SA as internal standard. The mean recovery of SA from serum was 85 ± 6%. Intra- and interday precision and % relative error were <15% in all cases.With a detection limit of 0.6 ng and a quantification limit of 2 ng, the method is therefore also adequate for population studies because of the small amount of blood necessary to perform the analyses. A simple, highly selective, and sensitive method using stable isotope dilution and gas chromatography-mass spectrometry has been developed to quantify salicylic acid (SA) at concentrations naturally occurring in biological fluids, such as in the serum of subjects not taking aspirin. After extraction of liquid-liquid with diethyl ether and ethyl acetate and preparation of the tert-butyldimethylsilyl derivative, SA content was detected using deuterated SA as internal standard. The mean recovery of SA from serum was 85 +/- 6%. Intra- and interday precision and % relative error were <15% in all cases. With a detection limit of 0.6 ng and a quantification limit of 2 ng, the method is therefore also adequate for population studies because of the small amount of blood necessary to perform the analyses.A simple, highly selective, and sensitive method using stable isotope dilution and gas chromatography-mass spectrometry has been developed to quantify salicylic acid (SA) at concentrations naturally occurring in biological fluids, such as in the serum of subjects not taking aspirin. After extraction of liquid-liquid with diethyl ether and ethyl acetate and preparation of the tert-butyldimethylsilyl derivative, SA content was detected using deuterated SA as internal standard. The mean recovery of SA from serum was 85 +/- 6%. Intra- and interday precision and % relative error were <15% in all cases. With a detection limit of 0.6 ng and a quantification limit of 2 ng, the method is therefore also adequate for population studies because of the small amount of blood necessary to perform the analyses. A simple, highly selective, and sensitive method using stable isotope dilution and gas chromatography-mass spectrometry has been developed to quantify salicylic acid (SA) at concentrations naturally occurring in biological fluids, such as in the serum of subjects not taking aspirin. After extraction of liquid-liquid with diethyl ether and ethyl acetate and preparation of the tert-butyldimethylsilyl derivative, SA content was detected using deuterated SA as internal standard. The mean recovery of SA from serum was 85 +/- 6%. Intra- and interday precision and % relative error were <15% in all cases. With a detection limit of 0.6 ng and a quantification limit of 2 ng, the method is therefore also adequate for population studies because of the small amount of blood necessary to perform the analyses.
Author	Testolin, G. Bertoli, S. Battezzati, A. Fiorillo, G. Spadafranca, A.
Author_xml	– sequence: 1 givenname: A. surname: Battezzati fullname: Battezzati, A. email: alberto.battezzati@unimi.it – sequence: 2 givenname: G. surname: Fiorillo fullname: Fiorillo, G. – sequence: 3 givenname: A. surname: Spadafranca fullname: Spadafranca, A. – sequence: 4 givenname: S. surname: Bertoli fullname: Bertoli, S. – sequence: 5 givenname: G. surname: Testolin fullname: Testolin, G.
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Cites_doi	10.1016/0378-4347(95)00464-5 10.1016/j.ab.2004.09.034 10.1056/NEJM199509073331011 10.1002/jsfa.2740320813 10.1001/archinte.160.20.3123 10.1136/heart.85.3.265 10.1021/jf035073r 10.1111/j.1365-2036.2004.02045.x 10.1016/S0002-8223(21)03743-3 10.1136/jcp.54.7.553 10.1038/28958 10.1016/S0009-9120(96)00137-3 10.1016/0962-8924(94)90235-6 10.1073/pnas.84.5.1417 10.1136/jcp.51.7.502
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Pathol. doi: 10.1136/jcp.51.7.502
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SubjectTerms	Blood Chemical Analysis - methods Blood Chemical Analysis - standards Blood Chemical Analysis - statistics & numerical data Deuterium Gas chromatography mass–spectrometry Gas Chromatography-Mass Spectrometry - methods Gas Chromatography-Mass Spectrometry - standards Gas Chromatography-Mass Spectrometry - statistics & numerical data Humans Isotope Labeling - methods Reference Standards Reproducibility of Results Salicylic Acid - blood Salicylic Acid - chemistry Salicylic Acid - standards Salycilic acid Serum Stable isotopes
Title	Measurement of salicylic acid in human serum using stable isotope dilution and gas chromatography–mass spectrometry
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