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Simultaneous simple and fast quantification of three major immunosuppressants by liquid chromatography—tandem mass-spectrometry

Objectives: The aim of the current study was to develop a simple, fast and universal method for quantification of any combination of the three major immunosuppressants sirolimus, tacrolimus and cyclosporin in whole blood, using a LC-tandem mass spectrometer (API-2000, SCIEX, Toronto, Canada). Method...

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Published in:Clinical biochemistry 2001-06, Vol.34 (4), p.285-290
Main Authors: Volosov, Andrew, Napoli, Kimberly L., Soldin, Steven J.
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Soldin, Steven J.
description Objectives: The aim of the current study was to develop a simple, fast and universal method for quantification of any combination of the three major immunosuppressants sirolimus, tacrolimus and cyclosporin in whole blood, using a LC-tandem mass spectrometer (API-2000, SCIEX, Toronto, Canada). Methods: 250 μL whole blood was spiked with internal standard (ritonavir), and protein precipitated with 350 μL acetonitrile. The sample was centrifuged and 30 μL aliquot was injected onto the HPLC column, where it underwent an online extraction with ammonium acetate. After that the automatic switching valve was activated, changing the mobile phase to methanol and thereby eluting the analytes into the tandem mass spectrometer. The high selectivity of a tandem mass analyzer allows determination of any combination of the three drugs within a 5 min run. Results: Between-day precision was between 2.4% and 9.7% for all analytes at the concentrations tested. Accuracy ranged between 98.8% and 103.2% ( n = 20). The method was linear over the measuring ranges of all analytes. Within-run precision was below %CV = 6% for all analytes. Good correlation with other analytical methods was observed. Conclusions: The simplicity, universality and high throughput of the method make it suitable for application in a clinical laboratory. The method has been implemented in our laboratory for a routine use.
doi_str_mv 10.1016/S0009-9120(01)00235-1
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Methods: 250 μL whole blood was spiked with internal standard (ritonavir), and protein precipitated with 350 μL acetonitrile. The sample was centrifuged and 30 μL aliquot was injected onto the HPLC column, where it underwent an online extraction with ammonium acetate. After that the automatic switching valve was activated, changing the mobile phase to methanol and thereby eluting the analytes into the tandem mass spectrometer. The high selectivity of a tandem mass analyzer allows determination of any combination of the three drugs within a 5 min run. Results: Between-day precision was between 2.4% and 9.7% for all analytes at the concentrations tested. Accuracy ranged between 98.8% and 103.2% ( n = 20). The method was linear over the measuring ranges of all analytes. Within-run precision was below %CV = 6% for all analytes. Good correlation with other analytical methods was observed. 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Methods: 250 μL whole blood was spiked with internal standard (ritonavir), and protein precipitated with 350 μL acetonitrile. The sample was centrifuged and 30 μL aliquot was injected onto the HPLC column, where it underwent an online extraction with ammonium acetate. After that the automatic switching valve was activated, changing the mobile phase to methanol and thereby eluting the analytes into the tandem mass spectrometer. The high selectivity of a tandem mass analyzer allows determination of any combination of the three drugs within a 5 min run. Results: Between-day precision was between 2.4% and 9.7% for all analytes at the concentrations tested. Accuracy ranged between 98.8% and 103.2% ( n = 20). The method was linear over the measuring ranges of all analytes. Within-run precision was below %CV = 6% for all analytes. Good correlation with other analytical methods was observed. 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purification</topic><topic>Tacrolimus</topic><topic>Tacrolimus - blood</topic><topic>Tacrolimus - isolation &amp; purification</topic><topic>Tandem mass-spectrometry</topic><topic>Transplantations</topic><toplevel>peer_reviewed</toplevel><toplevel>online_resources</toplevel><creatorcontrib>Volosov, Andrew</creatorcontrib><creatorcontrib>Napoli, Kimberly L.</creatorcontrib><creatorcontrib>Soldin, Steven J.</creatorcontrib><collection>Medline</collection><collection>MEDLINE</collection><collection>MEDLINE (Ovid)</collection><collection>MEDLINE</collection><collection>MEDLINE</collection><collection>PubMed</collection><collection>CrossRef</collection><collection>MEDLINE - Academic</collection><jtitle>Clinical biochemistry</jtitle></facets><delivery><delcategory>Remote Search Resource</delcategory><fulltext>fulltext</fulltext></delivery><addata><au>Volosov, Andrew</au><au>Napoli, Kimberly L.</au><au>Soldin, Steven J.</au><format>journal</format><genre>article</genre><ristype>JOUR</ristype><atitle>Simultaneous simple and fast quantification of three major immunosuppressants by liquid chromatography—tandem mass-spectrometry</atitle><jtitle>Clinical biochemistry</jtitle><addtitle>Clin Biochem</addtitle><date>2001-06-01</date><risdate>2001</risdate><volume>34</volume><issue>4</issue><spage>285</spage><epage>290</epage><pages>285-290</pages><issn>0009-9120</issn><eissn>1873-2933</eissn><abstract>Objectives: The aim of the current study was to develop a simple, fast and universal method for quantification of any combination of the three major immunosuppressants sirolimus, tacrolimus and cyclosporin in whole blood, using a LC-tandem mass spectrometer (API-2000, SCIEX, Toronto, Canada). 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subjects Calibration
Chemistry, Clinical - methods
Chromatography
Chromatography, High Pressure Liquid - methods
Cyclosporin
Cyclosporine - blood
Cyclosporine - isolation & purification
Gas Chromatography-Mass Spectrometry - methods
Humans
Immunosuppressants
Immunosuppressive Agents - blood
Immunosuppressive Agents - chemistry
Immunosuppressive Agents - isolation & purification
Linear Models
Reproducibility of Results
Sensitivity and Specificity
Sirolimus
Sirolimus - blood
Sirolimus - isolation & purification
Tacrolimus
Tacrolimus - blood
Tacrolimus - isolation & purification
Tandem mass-spectrometry
Transplantations
title Simultaneous simple and fast quantification of three major immunosuppressants by liquid chromatography—tandem mass-spectrometry
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