Chen Ning, Li Weixia, Wu Shuchao, Zhu Yan
Department of Chemistry, Zhejiang University, Xixi Campus, Hangzhou 310028, People's Republic of China.
Zhejiang Institute of Geology and Mineral Resources, Hangzhou 310007, People's Republic of China.
R Soc Open Sci. 2018 Aug 15;5(8):171948. doi: 10.1098/rsos.171948. eCollection 2018 Aug.
A novel method combining high-performance liquid chromatography with online post-column electrochemical derivatization and fluorescence detection was established for the detection of reserpine in mouse serum. Reserpine separation was conducted using a C18 column with 5 mM HPO and acetonitrile (55/45, v/v) as eluent. Reserpine was then electro-oxidized into a strongly fluorescent compound using an electrolytic cell device. Detection parameters, such as potential and fluorescence wavelength, were optimized. The linearity of the proposed method ranged from 0.01 to 5.0 mg l with a correlation coefficient of 0.9997. The limit of qualification (/ = 10) and limit of detection (/ = 3) were 9.7 and 2.9 µg l, respectively. Resperine recoveries from spiked blank and drug-treated mouse serum samples ranged from 92.0 to 115%.
建立了一种将高效液相色谱与在线柱后电化学衍生化及荧光检测相结合的新方法，用于检测小鼠血清中的利血平。利血平的分离采用C18柱，以5 mM HPO和乙腈（55/45，v/v）作为洗脱液。然后使用电解池装置将利血平电氧化为强荧光化合物。对检测参数，如电位和荧光波长进行了优化。该方法的线性范围为0.01至5.0 mg·l，相关系数为0.9997。定量限（/ = 10）和检测限（/ = 3）分别为9.7和2.9 μg·l。加标空白和药物处理小鼠血清样品中利血平的回收率为92.0%至115%。
