Determination of some sulphonamides by sequential injection analysis with chemiluminescence detection
Determination of some sulphonamides by sequential injection analysis with chemiluminescence detection
复制标题
通过化学发光检测序贯进样分析测定某些磺胺类药物
DOI：
10.1016/s0003-2670(00)01310-6
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发表时间：
2001
期刊：
影响因子：
--
通讯作者：
J. Dolejšová
中科院分区：
文献类型：
--
作者：
H. Paseková;M. Polášek;Joaquim Filipe Cigarro;J. Dolejšová
建立了磺胺类药物(磺胺、磺乙酰胺、磺胺噻唑、磺胺类)的顺序注射化学发光(CL)检测方法。在硫酸介质中，高锰酸钾氧化磺胺产生化学发光信号。实验室制造的SIA系统包括一个2.5ml的Cavro注射器泵，八端口Vici Valco选择阀和一个实验室改装的光谱物理FS970荧光检测器。它由一台PC控制，使用最初编译的LabVIEW®支持的软件。用单纯形法对浓度、试剂用量和流速进行了优化。一些增强剂被测试以增加CL信号。磺胺的最佳进样条件和进样顺序为：0.1M戊二醛45μL，样品50μL，0.5M H_2SO_445μL，1 mM KMnO_446μL，100μls−1流速。在单次倒流后记录了瞬时CL信号(λ≥390 nm)。CL强度(峰高)与分析物浓度之间的校准曲线为曲线(二次多项式)，直线段通常在≈0.01-0.5 mm磺胺范围内。进样量为120h−1。该方法已用于药物制剂中磺胺类和磺胺类药物的含量测定。SIA结果与根据USP XXIV滴定获得的结果没有任何统计上的显著差异。
Determination of a group of sulphonamides (sulphanilamide, sulphacetamide, sulphathiazole, sulphadimidine, sulphafurazole, sulphamethoxypyridazine, sulphaguanidine) using sequential injection analysis (SIA) technique with chemiluminescence (CL) detection has been devised. The CL signal was emitted during the oxidation of sulphonamides by potassium permanganate in sulphuric acid medium. The lab-made SIA system consisted of a 2.5ml Cavro syringe pump, eight-port Vici Valco selection valve and a lab-modified Spectra-Physics FS 970 fluorescence detector. It was controlled by a PC with use of originally compiled LabVIEW®-supported software. Concentration, volume of reagents and flow rate were optimised by a simplex method. A number of enhancers was tested to increase the CL signal. The optimum conditions and sequence of injected zones for sulphanilamide (model substance) were: 0.1M glutaraldehyde 45μl, sample 50μl; 0.5M H2SO445μl; 1mM KMnO446μl and 100μls−1flow rate. The transient CL signal (λ≥390nm) was recorded after a single reversal of the flow. Calibration curves relating the intensity of CL (peak heights) to the concentration of the analytes were curvilinear (of the second polynomial order) with rectilinear sections typically in the range ≈0.01–0.5mM sulphonamide. The sample throughput was 120h−1. The proposed method has been applied for the assay of sulphacetamide and sulphafurazole in pharmaceutical dosage forms. The SIA results did not show any statistically significant difference from those obtained by titrimetry according to USP XXIV.