An Advanced Double Column-Switching Technique (LC-LC) for Liquid Chromatography/Electrospray Ionisation Tandem Mass Spectrometry for Fully Automated Analysis of Caspofungin
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In: Rapid Communications in Mass Spectrometry , Vol. 18, No. 23, 01.11.2004, p. 2871-2877.
Research output: Journal contributions › Journal articles › Research › peer-review
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TY - JOUR
T1 - An Advanced Double Column-Switching Technique (LC-LC) for Liquid Chromatography/Electrospray Ionisation Tandem Mass Spectrometry for Fully Automated Analysis of Caspofungin
AU - Egle, Hannes
AU - Trittler, Rainer
AU - Kümmerer, Klaus
N1 - 2004 John Wiley & Sons, Ltd.
PY - 2004/11/1
Y1 - 2004/11/1
N2 - Caspofungin (MK-0991; L-743,872) is the first representative of a new important class of antifungal agents, the glucan synthesis inhibitors. To the authors' best knowledge, to date only one high-performance liquid chromatography (HPLC) method has been published for the determination of caspofungin in serum. Severe difficulties with sorption were described. We developed a new method which addresses these difficulties using an advanced column-switching technique for fully automated analysis of caspofungin in serum without any pre-treatment. Extraction was performed automatically inline, using a diol column, followed by chromatography on a CN column. Detection was performed by electrospray ionisation tandem mass spectrometry (ESI-MS/MS) with isolation and fragmentation in the positive ion mode. Total analysis time was 30 min. Detection of caspofungin was achieved by retention time, isolation and fragmentation of the double positively charged caspofungin ion. This LC/MS assay was validated for between-run accuracy (max. 110%) and precision (max. CV 16.1%). The lower limit of quantification was 0.2 μg/mL. The analytical method with fully automated inline extraction of caspofungin described here removes the need for difficult and time-consuming sample pre-treatment. Sorption of caspofungin is not of importance. Additional advantages of the new method are that only a small quantity of serum (5 μL) is needed and that the method is very specific. Copyright © 2004 John Wiley & Sons, Ltd.
AB - Caspofungin (MK-0991; L-743,872) is the first representative of a new important class of antifungal agents, the glucan synthesis inhibitors. To the authors' best knowledge, to date only one high-performance liquid chromatography (HPLC) method has been published for the determination of caspofungin in serum. Severe difficulties with sorption were described. We developed a new method which addresses these difficulties using an advanced column-switching technique for fully automated analysis of caspofungin in serum without any pre-treatment. Extraction was performed automatically inline, using a diol column, followed by chromatography on a CN column. Detection was performed by electrospray ionisation tandem mass spectrometry (ESI-MS/MS) with isolation and fragmentation in the positive ion mode. Total analysis time was 30 min. Detection of caspofungin was achieved by retention time, isolation and fragmentation of the double positively charged caspofungin ion. This LC/MS assay was validated for between-run accuracy (max. 110%) and precision (max. CV 16.1%). The lower limit of quantification was 0.2 μg/mL. The analytical method with fully automated inline extraction of caspofungin described here removes the need for difficult and time-consuming sample pre-treatment. Sorption of caspofungin is not of importance. Additional advantages of the new method are that only a small quantity of serum (5 μL) is needed and that the method is very specific. Copyright © 2004 John Wiley & Sons, Ltd.
KW - accuracy
KW - AGENTS
KW - ANALYSIS
KW - antifungal
KW - ANTIFUNGAL AGENT
KW - ASSAY
KW - Caspofungin
KW - chromatography
KW - COLUMN
KW - column switching
KW - column-switching
KW - detection
KW - determination
KW - Electrospray
KW - EXTRACTION
KW - GERMANY
KW - HIGH PERFORMANCE LIQUID CHROMATOGRAPHY
KW - HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY
KW - HPLC
KW - human plasma
KW - INHIBITOR
KW - INHIBITORS
KW - Ionisation
KW - KNOWLEDGE
KW - LC
KW - MS
KW - liquid
KW - liquid chromatography
KW - LIQUID-CHROMATOGRAPHY
KW - mass spectrometry
KW - MASS-SPECTROMETRY
KW - Method
KW - MK-0991
KW - MODE
KW - pharmacokinetics
KW - PRETREATMENT
KW - QUANTIFICATION
KW - RABBITS
KW - retention
KW - Serum
KW - Sorption
KW - SPECTROMETRY
KW - tandem mass spectrometry
KW - URINE
KW - Chemistry
UR - http://www.scopus.com/inward/record.url?scp=9644266735&partnerID=8YFLogxK
UR - https://www.mendeley.com/catalogue/7166b00d-a772-3009-bb61-a1f761b5658b/
U2 - 10.1002/rcm.1691
DO - 10.1002/rcm.1691
M3 - Journal articles
C2 - 15517540
VL - 18
SP - 2871
EP - 2877
JO - Rapid Communications in Mass Spectrometry
JF - Rapid Communications in Mass Spectrometry
SN - 1097-0231
IS - 23
ER -