Svagrová I, Stulík K, Pacáková V, Caliceti P, Veronese F M
Department of Analytical Chemistry, Charles University, Prague, Czechoslovakia.
J Chromatogr. 1991 Jan 18;563(1):95-102. doi: 10.1016/0378-4347(91)80280-p.
Narciclasine was determined in the blood of mice by reversed-phase high-performance liquid chromatography, using a C18 stationary phase and a mobile phase of methanol-0.025 M potassium dihydrogen phosphate (50:50, v/v) of pH 5.5. Amperometric detection at a carbon fibre array working electrode held at +1.8 V (Ag/AgCl) permitted determination down to concentrations of 10 and 15.4 ng ml-1 (at a signal-to-noise ratio of 2) in aqueous solution and in serum, respectively. Fluorescence detection (excitation and emission wavelengths of 360 and 480 nm, respectively) exhibited somewhat poorer sensitivities for aqueous and serum samples: the respective limits of detection were 25 and 32 ng ml-1 at a signal-to-noise ratio of 2. Both the amperometric and the fluorescence detection were free from interference from blood components, but the fluorescence measurement required a post-column pH adjustment. UV photometric detection at 254 nm exhibited detection limits of 15 and 65 ng ml-1 in aqueous samples and in serum, respectively, and suffered from interferences from blood components that strongly absorbed in the ultraviolet region. All three detection techniques exhibited good linearity and precision.
采用反相高效液相色谱法，以C18固定相和pH 5.5的甲醇-0.025 M磷酸二氢钾（50:50，v/v）流动相，测定小鼠血液中的水仙环素。在+1.8 V（Ag/AgCl）的碳纤维阵列工作电极上进行安培检测，在水溶液和血清中分别可测定低至10和15.4 ng ml-1的浓度（信噪比为2）。荧光检测（激发和发射波长分别为360和480 nm）对水溶液和血清样品的灵敏度稍差：在信噪比为2时，检测限分别为25和32 ng ml-1。安培检测和荧光检测均不受血液成分干扰，但荧光测量需要柱后进行pH调节。254 nm处的紫外光度检测在水溶液样品和血清中的检测限分别为15和65 ng ml-1，且受到在紫外区域有强烈吸收的血液成分的干扰。这三种检测技术均表现出良好的线性和精密度。
