Satínský Dalibor, Sklenárová Hana, Huclová Jitka, Karlícek Rolf
The Research Centre LN00B125, Charles University, Heyrovského 1203, 500 05 Hradec Králové, Czech Republic.
Farmaco. 2003 Oct;58(10):1057-62. doi: 10.1016/S0014-827X(03)00179-4.
In the proposed procedure, the determination of bopindolol using a sequential injection technique (SIA) with spectrophotometric detection at 560 nm is described. The new method of determination is based on the color reaction of the indole group in the molecule of bopindolol with 4-dimethylaminobenzaldehyde (Ehrlich's reagent) in acidic medium with production of a violet water-soluble complex. Due to the kinetic standpoint of reaction, the "stopped flow" technique with mixing coil between the valve and detector was tested and optimized. The proposed SIA system was used for the direct determination of bopindolol in tablets, negative effects of interfering substances (excipients of tablets) were not observed. The selectivity of the proposed method of determination was tested in the presence of seven interfering substances from the group of beta-blockers with good results. The interference effect was observed only in the presence of pindolol. The sample throughput with stopped flow technique was 40 samples per hour. Bopindolol was determined in the linear range from 1 to 10 microg ml(-1), RSD was less than 1% (n=10), with limit of detection (3sigma) 0.1 microg ml(-1) and limit of quantification 0.5 microg ml(-1). Obtained results were compared with conventional HPLC method, both analytical techniques were in good agreement.
在本方法中,描述了采用顺序注射技术(SIA)结合560nm分光光度检测法测定波吲洛尔。该新测定方法基于波吲洛尔分子中吲哚基团在酸性介质中与4-二甲基氨基苯甲醛(埃利希试剂)发生显色反应,生成紫色水溶性络合物。从反应动力学角度出发,对阀与检测器之间带有混合盘管的“停流”技术进行了测试和优化。所提出的SIA系统用于直接测定片剂中的波吲洛尔,未观察到干扰物质(片剂辅料)的负面影响。在存在七种β受体阻滞剂干扰物质的情况下测试了所提出测定方法的选择性,结果良好。仅在吲哚洛尔存在时观察到干扰效应。停流技术的样品通量为每小时40个样品。波吲洛尔的测定线性范围为1至10μg ml⁻¹,相对标准偏差小于1%(n = 10),检测限(3σ)为0.1μg ml⁻¹,定量限为0.5μg ml⁻¹。将所得结果与传统高效液相色谱法进行比较,两种分析技术结果吻合良好。