Determination of enantiomeric purity of the new D-2 dopamine agonist 2-(N-propyl-N-2-thienylethylamino)-5-hydroxytetralin (N-0437) by reversed-phase high-performance liquid chromatography after pre-column derivatization with D(+)-glucuronic acid.
This paper describes an enzymic derivatization procedure that allows accurate determination of very small amounts of enantiomeric impurities in the D-2 dopamine agonist 2-(N-propyl-N-2-thienylethylamino)-5-hydroxytetralin (N-0437). After pre-column glucuronidation of the individual enantiomers, two diastereoisomers were formed which were separated by reversed-phase high-performance liquid chromatography. An enantiomeric purity of 99.84% was calculated for the (-)-enantiomer, against 99.89% for the (+)-enantiomer. The assay was validated by spiking 1% of the (-)-enantiomer in the (+)-enantiomer. A high accuracy (error 4.5%) and precision (coefficient of variation 2.9%, n = 5) of the method were established.
Gerding
T K
TK
Department of Toxicology, State University, Groningen, The Netherlands.
Drenth
B F
BF
Van de Grampel
V J
VJ
Niemeijer
N R
NR
De Zeeuw
R A
RA
Tepper
P G
PG
Horn
A S
AS
D000818:Animals; D002417:Cattle; D002851:Chromatography, High Pressure Liquid; D005965:Glucuronates; D020723:Glucuronic Acid; D007202:Indicators and Reagents; D008862:Microsomes, Liver / Q000378:metabolism; D009281:Naphthalenes / Q000032:analysis*; D013237:Stereoisomerism; D013764:Tetrahydronaphthalenes / Q000032:analysis*; D013876:Thiophenes / Q000032:analysis*
D005965:Glucuronates; D007202:Indicators and Reagents; D009281:Naphthalenes; D013764:Tetrahydronaphthalenes; D013876:Thiophenes; C047508:rotigotine; D020723:Glucuronic Acid