Fernández-Sánchez J F, Carretero A Segura, Cruces-Blanco C, Fernández-Gutiérrez A
Department of Analytical Chemistry, Faculty of Sciences, University of Granada, C/Fuentenueva s/n, E-18071 Granada, Spain.
J Pharm Biomed Anal. 2003 Apr 1;31(5):859-65. doi: 10.1016/s0731-7085(02)00692-1.
We describe a simple and selective method for analysing propranolol and a sensitive test for its control in urine. A flow-through fluorescence optosensor based on on-line immobilization in a non-ionic-exchanger (Amberlite XAD-7) solid support in a continuous flow was used in both cases. Determination was made in 5 mM H(2)PO(4)(-)/HPO(4)(2-) buffer solution at pH 6 at a working temperature of 20 degrees C. Fluorescence intensities were measured at lambda(ex/em) = 300/338 nm with a response time of 80 s, thus obtaining a linear concentration range of between 0 and 250.0 ng ml(-1) with a detection limit of 1.3 ng ml(-1), an analytical sensitivity of 6.0 ng ml(-1) and a standard deviation of 2.40% at a 150 ng ml(-1) concentration level for propranolol. We also propose a test to detect propranolol in urine with a linear concentration range between 0 and 100.0 ng ml(-1), a detection limit of 0.2 ng ml(-1), an analytical sensitivity of 1.0 ng ml(-1), and a standard deviation of 0.84% at a 75 ng ml(-1) concentration level. The effect of proteins presents in urine samples were evaluated. The two proposed methods were satisfactorily applied to commercial formulations and urine samples respectively.
我们描述了一种分析普萘洛尔的简单且选择性的方法以及一种用于尿液中普萘洛尔检测的灵敏测试。两种情况均使用了基于在连续流动的非离子交换剂(Amberlite XAD - 7)固体支持物上进行在线固定的流通式荧光光传感器。在20℃的工作温度下,于pH 6的5 mM H₂PO₄⁻/HPO₄²⁻缓冲溶液中进行测定。在λ(ex/em) = 300/338 nm处测量荧光强度,响应时间为80 s,从而获得普萘洛尔在0至250.0 ng ml⁻¹之间的线性浓度范围,检测限为1.3 ng ml⁻¹,分析灵敏度为6.0 ng ml⁻¹,在150 ng ml⁻¹浓度水平下的标准偏差为2.40%。我们还提出了一种用于检测尿液中普萘洛尔的测试,其线性浓度范围在0至100.0 ng ml⁻¹之间,检测限为0.2 ng ml⁻¹,分析灵敏度为1.0 ng ml⁻¹,在75 ng ml⁻¹浓度水平下的标准偏差为0.84%。评估了尿液样品中蛋白质的影响。所提出的两种方法分别令人满意地应用于市售制剂和尿液样品。