Rodríguez J, Berzas J J, Castañeda G, Rodríguez N
Departamento de Quimica Analitica y Tecnologia de Alimentos, Facultad de Quimicas, Universidad de Castilla-La Mancha, Ciudad Real E-13071, Spain.
Talanta. 2004 Feb 6;62(2):427-32. doi: 10.1016/j.talanta.2003.07.017.
The voltammetric behaviour of Sildenafil citrate (SC) and its main metabolite UK-103,320 (UK) was studied by square wave techniques, leading to two methods for its total determination in biological samples (urine and human serum). The application of the square wave (SW), without the adsorptive accumulation, shows a maximum response at -0.950V. The effect of experimental parameters that affect this determination are discussed. The stripping technique, proved to be more sensitive, yielding signals three times larger than those obtained by applying a square wave scan without the previous accumulation. Two calibration graphs to determine total SC and UK concentration were established. Calibration graph in urine sample was linear in the range 4.4x10(-8) to 4.8x10(-7)M by the stripping mode with an accumulation time of 10s. In the same conditions but in serum sample regression line was linear in the range 3.4x10(-8) to 9.7x10(-7)M. The two proposed methods (SW and square-wave adsorptive stripping voltammetry (SWAdSV)) were applied to the total concentration analysis in eight different biological samples by the standard addition method with satisfactory results in the four different serum samples by the SW and in the four urines by SWAdSV.
采用方波技术研究了枸橼酸西地那非(SC)及其主要代谢物 UK - 103,320(UK)的伏安行为,由此建立了两种用于测定生物样品(尿液和人血清)中它们总量的方法。在不进行吸附富集的情况下施加方波(SW),在 - 0.950V 处显示出最大响应。讨论了影响该测定的实验参数的作用。溶出技术被证明更灵敏,产生的信号比在不进行先前富集的情况下施加方波扫描所获得的信号大三倍。建立了两条用于测定 SC 和 UK 总浓度的校准曲线。尿液样品中的校准曲线在溶出模式下,累积时间为 10s 时,在 4.4×10⁻⁸至 4.8×10⁻⁷M 范围内呈线性。在相同条件下但针对血清样品,回归线在 3.4×10⁻⁸至 9.7×10⁻⁷M 范围内呈线性。通过标准加入法将所提出的两种方法(SW 和方波吸附溶出伏安法(SWAdSV))应用于八个不同生物样品中的总浓度分析,SW 法在四个不同血清样品中以及 SWAdSV 法在四个尿液样品中均获得了满意结果。