Zacharis Constantinos K, Tzanavaras Paraskevas D, Themelis Demetrius G, Theodoridis Georgios A, Economou Anastasios, Rigas Pantelis G
Laboratory of Analytical Chemistry, Department of Chemistry, Aristotle University Thessaloniki, 54124 Thessaloniki, Greece.
Anal Bioanal Chem. 2004 Jul;379(5-6):759-63. doi: 10.1007/s00216-004-2530-4. Epub 2004 Feb 19.
The present work reports for the first time a simple and rapid method for the spectrofluorimetric determination of lisinopril (LSP) in pharmaceutical formulations using sequential injection analysis (SIA). The method is based on reaction of LSP with o-phthalaldehyde (OPA) in the presence of 2-mercaptoethanol (borate buffer medium, pH=10.6). The emission of the derivative is monitored at 455 nm upon excitation at 346 nm. The various chemical and physical conditions that affected the reaction were studied. The calibration curve was linear in the range 0.3-10.0 mg L(-1) LSP, at a sampling rate of 60 injections h(-1). Consumption of OPA reagent was significantly reduced compared with conventional flow injection (FI) systems, because only 50 microL of OPA was consumed per run. The method was found to be adequately precise ( s(r)=2% at 5 mg L(-1) LSP, n=10) and the 3 sigma detection limit was 0.1 mg L(-1). The method was successfully applied to the analysis of two pharmaceutical formulations containing LSP. The results obtained were in good agreement with those obtained by use of high-performance liquid chromatography (HPLC), because the mean relative error, e(r), was <1.8%.
本研究首次报道了一种使用顺序注射分析（SIA）分光荧光法快速简便地测定药物制剂中赖诺普利（LSP）的方法。该方法基于LSP与邻苯二甲醛（OPA）在2-巯基乙醇（硼酸盐缓冲介质，pH = 10.6）存在下的反应。在346 nm激发下，于455 nm处监测衍生物的发射。研究了影响该反应的各种化学和物理条件。校准曲线在0.3 - 10.0 mg L⁻¹ LSP范围内呈线性，进样速率为60次/小时。与传统流动注射（FI）系统相比，OPA试剂的消耗量显著降低，因为每次运行仅消耗50 μL OPA。该方法具有足够的精密度（在5 mg L⁻¹ LSP时，s(r) = 2%，n = 10），3σ检测限为0.1 mg L⁻¹。该方法成功应用于两种含LSP药物制剂的分析。所得结果与使用高效液相色谱（HPLC）获得的结果高度一致，因为平均相对误差e(r) < 1.8%。
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