Kinetic Study of the Degradation of PAC-1 and Identification of a Degradation Product in Alkaline Condition |
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Authors: | Song Zhen Chen Xiaohui Zhang Di Ren Lei Fang Lina Cheng Weiming Gong Ping Bi Kaishun |
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Institution: | 1.School of Pharmacy, Shenyang Pharmaceutical University, 103 Wenhua Road, 110016, Shenyang, China ;2.School of Pharmaceutical Engineering, Shenyang Pharmaceutical University, 103 Wenhua Road, 110016, Shenyang, China ; |
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Abstract: | A selective and validated stability-indicating LC method was developed for the kinetic study of the degradation of PAC-1, which was carried out in aqueous solutions at 37, 60, 80 and 100 °C with pH 1.5–9.0. Separation was performed on a Kromasil C18 column with acetonitrile–water–fomic acid (30:70:0.1, v/v/v) as mobile phase with a flow rate of 1.0 mL min?1 at 281 nm. The degradation rate obtained indicated a first-order reaction law and the activation energy (E
a) was calculated. The results showed that temperature and pH values were significant factors affecting the degradation of PAC-1. An unknown degradation product in alkaline condition was isolated using a reverse-phase semi-preparative LC system. The structure of the degradation product is identified as 2-hydroxy-3-(2-propenyl)-2-hydroxy-3-(2-propenyl)phenyl]methylene]hydrazone utilizing the 1H NMR, 13C NMR, IR and Q-TOF-MS techniques. |
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