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  • Title: Determination of a novel calmodulin antagonist, 3-[2-[4-(3-chloro-2-methylphenyl)-1-piperazinyl]ethyl]-5,6-dimethoxy-1- (4-imidazolylmethyl)-1H-indazole dihydrochloride 3.5 hydrate, DY-9760e, in human plasma using solid-phase extraction and high-performance liquid chromatography with fluorescence detection.
    Author: Tachibana S, Fukano A, Sudo K, Tanaka M.
    Journal: J Chromatogr B Biomed Sci Appl; 1999 Oct 29; 734(1):39-45. PubMed ID: 10574188.
    Abstract:
    A high-performance liquid chromatographic method for the determination of a novel calmodulin antagonist, 3-[2-[4-(3-chloro-2-methylphenyl)-1-piperazinyl]ethyl]-5,6-dimethoxy-1-( 4-imidazolylmethyl)-1H-indazole dihydrochloride 3.5 hydrate, DY-9760e and its major metabolite, 3-[2-[4-(3-chloro-2-methylphenyl)-1-piperazinyl]ethyl]-5,6-dimethoxyi ndazole, DY-9836 in human plasma has been developed. DY-9760e, DY-9836 and the internal standard (I.S.) were extracted from plasma by means of an Isolute C18 (EC) column. The extracts were chromatographed on a reversed-phase TSK-gel ODS-80Ts column using 0.1 M acetate buffer (pH 5)-CH3CN (65:35, v/v) as the mobile phase at a flow-rate of 1.0 ml/min. Fluorescence detection at an excitation wavelength of 303 nm and an emission wavelength of 347 nm resulted in a limit of quantitation of 1.000 ng/ml for plasma. The method showed satisfactory sensitivity, precision, accuracy, recovery and selectivity. Stability studies showed that DY-9760 and DY-9836 were stable in plasma up to at least eight weeks at -80 degrees C.
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