Development of a sensitive liquid chromatography–electrospray ionization tandem mass spectrometry method for the measurement of 7-cyanoquinocarcinol in human plasma |
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Authors: | Kazuo Yamaguchi Eiichi Fuse Michio Takashima Tohru Yasuzawa Takashi Kuwabara Satoshi Kobayashi |
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Affiliation: | Drug Development Research Laboratories, Pharmaceutical Research Institute, Kyowa Hakko Kogyo Co., Ltd, 1188 Shimotogari Nagaizumi-cho, Shizuoka-ken 411, Japan |
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Abstract: | A sensitive method for the determination of an anti-cancer agent, DX-52-1 (7-cyanoquinocarcinol, I) and quinocarmycin (II) which is formed from I either by metabolism or degradation, in human plasma has been developed utilising liquid chromatography electrospray–ionization tandem mass spectrometry (LC–ESI-MS–MS). The procedure involves solid-phase extraction at pH 2 and low temperature (4–6°C) to prevent the decomposition of I to II, the separation by reversed-phase HPLC and the multiple reaction monitoring (MRM) by ESI-MS–MS. The mean precision and accuracy at the lower limit of quantitation (LLOQ) of I, 0.25 ng ml−1, were 8.7% and −10.8%, respectively. Since an interfering peak eluting slightly earlier than II was observed on the HPLC of blank plasma, the LLOQ of II was set at 5 ng ml−1 where the mean precision and accuracy were 15.6% and −9.8%. The results suggested that the method is useful for the simultaneous monitoring of Iand II in the clinical trials of I. |
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Keywords: | 7-Cyanoquinocarcinol |
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