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通过亚硝化伏安法测定剂型和生物流体中的苯那普利和雷米普利。

Voltammetric determination of benazepril and ramipril in dosage forms and biological fluids through nitrosation.

作者信息

Belal F, Al-Zaagi I A, Abounassif M A

机构信息

King Saud University, College of Pharmacy, Department of Pharmaceutical Chemistry, Riyadh, Saudi Arabia.

出版信息

J AOAC Int. 2001 Jan-Feb;84(1):1-8.

Abstract

A simple and highly sensitive voltammetric method was developed for the determination of benazepril (I) and ramipril (II). The compounds were treated with nitrous acid, and the cathodic current produced by the resulting nitroso derivatives was measured. The voltammetric behavior was studied by adopting direct current (DCt), differential pulse (DPP), and alternating current (ACt) polarography. Both compounds produced well-defined, diffusion-controlled cathodic waves over the whole pH range in Britton-Robinson buffers (BRb). At pH 3 and 5, the values of diffusion-current constants (Id), were 5.90 +/- 0.40 and 6.66 +/- 0.61 for I and II, respectively. The current concentration plots for I were rectilinear over the range of 1.5-40 and 0.1-30 microg/mL in the DCt and DPP modes, respectively; for II, the range was 2-30 and 0.1-20 microg/mL in the DCt and DPP modes, respectively. The minimum detectabilities (S/N = 2) were 0.015 microg/mL (about 3.25 x 10(-8)M) and 0.012 microg/mL (about 2.88 x 10(-8)M) for I and II, respectively, adopting the DPP mode. Results obtained for the proposed method when applied to the determination of both compounds in dosage forms were in good agreement with those obtained using reference methods. Hydrochlorthiazide, which is frequently co-formulated with these drugs, did not interfere with the assay. The method was also applied to the determination of benazepril in spiked human urine and plasma. The percentage recoveries adopting the DPP mode were 96.2 +/- 1.21 and 95.7 +/- 1.61, respectively.

摘要

开发了一种简单且高度灵敏的伏安法用于测定苯那普利(I)和雷米普利(II)。将这些化合物用亚硝酸处理,并测量所得亚硝基衍生物产生的阴极电流。采用直流(DCt)、差分脉冲(DPP)和交流(ACt)极谱法研究了伏安行为。在 Britton-Robinson 缓冲液(BRb)中,两种化合物在整个 pH 范围内均产生了明确的、受扩散控制的阴极波。在 pH 3 和 5 时,I 和 II 的扩散电流常数(Id)值分别为 5.90±0.40 和 6.66±0.61。在 DCt 和 DPP 模式下,I 的电流浓度曲线在 1.5 - 40 和 0.1 - 30 μg/mL 范围内分别呈直线;对于 II,在 DCt 和 DPP 模式下,范围分别为 2 - 30 和 0.1 - 20 μg/mL。采用 DPP 模式时,I 和 II 的最低检测限(S/N = 2)分别为 0.015 μg/mL(约 3.25×10⁻⁸ M)和 0.012 μg/mL(约 2.88×10⁻⁸ M)。将所提出的方法应用于剂型中两种化合物的测定时,所得结果与使用参考方法获得的结果高度一致。经常与这些药物共同配制的氢氯噻嗪不干扰测定。该方法还应用于加标的人尿液和血浆中苯那普利的测定。采用 DPP 模式时的回收率分别为 96.2±1.21 和 95.7±1.61。

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