[Methyl-D3]2hypericin as internal standard for quantification in human plasma.
The multistep synthesis and negative ion-ESI fragmentation pattern of [methyl-D(3)](2)hypericin (1-D(6)) is described. The application of 1-d(6) as internal standard for the quantification of hypericin (1) in the ng mL(-1) range in human plasma by isotope-dilution LC-MS is demonstrated. The hypericin-containing plasma samples are spiked with 1-D(6), deproteinized and extracted with ethyl acetate. The extracts are injected into a HPLC-ESI-ion-trap system and the mass-separated negative ions from 1 and 1-D(6) are analysed. From their intensities linear standard curves over the concentration range from 1 to 10 ng mL(-1) are obtained. Accuracy, precision and recovery are discussed.
Piperopoulos
Georgios
G
Institut für Organische Chemie, Eberhard-Karls Universität Tübingen, Auf der Morgenstelle 18, 72076 Tübingen, Germany.
Kiehne
Andrea
A
Ingendoh
Arnd
A
Zeller
Klaus-Peter
KP
D000873:Anthracenes; D003903:Deuterium; D006801:Humans; D015394:Molecular Structure; D010569:Perylene / Q000031:analogs & derivatives* / Q000097:blood* / Q000737:chemistry; D012015:Reference Standards; D012680:Sensitivity and Specificity; D021241:Spectrometry, Mass, Electrospray Ionization / Q000379:methods* / Q000592:standards
C479278:(methyl-D3)2hypericin; D000873:Anthracenes; D010569:Perylene; C004965:hypericin; D003903:Deuterium