Mervartová Katerina, Polásek Miroslav, Calatayud José Martínez
Department of Analytical Chemistry, Faculty of Pharmacy, Charles University, Heyrovského 1203, CZ-500 05 Hradec Králové, Czech Republic.
Anal Chim Acta. 2007 Sep 26;600(1-2):114-21. doi: 10.1016/j.aca.2007.01.057. Epub 2007 Jan 26.
Automated sequential injection (SIA) method for chemiluminescence (CL) determination of nonsteroidal anti-inflammatory drug indomethacin (I) was devised. The CL radiation was emitted in the reaction of I (dissolved in aqueous 50% v/v ethanol) with intermediate reagent tris(2,2'-bipyridyl)ruthenium(III) (Ru(bipy)(3)(3+)) in the presence of acetate. The Ru(bipy)(3)(3+) was generated on-line in the SIA system by the oxidation of 0.5mM tris(2,2'-bipyridyl)ruthenium(II) (Ru(bipy)(3)(2+)) with Ce(IV) ammonium sulphate in diluted sulphuric acid. The optimum sequence, concentrations, and aspirated volumes of reactant zones were: 15 mM Ce(IV) in 50mM sulphuric acid 41 microL, 0.5 mM Ru(bipy)(3)(2+) 30 microL, 0.4M Na acetate 16 microL and I sample 15 microL; the flow rates were 60 microLs(-1) for the aspiration into the holding coil and 100 microLs(-1) for detection. Calibration curve relating the intensity of CL (peak height of the transient CL signal) to concentration of I was curvilinear (second order polynomial) for 0.1-50 microM I (r=0.9997; n=9) with rectilinear section in the range 0.1-10 microM I (r=0.9995; n=5). The limit of detection (3sigma) was 0.05 microM I. Repeatability of peak heights (R.S.D., n=10) ranged between 2.4% (0.5 microM I) and 2.0% (7 microM I). Sample throughput was 180 h(-1). The method was applied to determination of 1 to 5% of I in semisolid dosage forms (gels and ointments). The results compared well with those of UV spectrophotometric method.
设计了用于化学发光(CL)法自动顺序注射(SIA)测定非甾体抗炎药吲哚美辛(I)的方法。在乙酸盐存在下,I(溶解于50% v/v乙醇水溶液中)与中间试剂三(2,2'-联吡啶)钌(III)(Ru(bipy)₃³⁺)反应时发出CL辐射。在SIA系统中,通过在稀硫酸中用硫酸铈(IV)铵氧化0.5 mM三(2,2'-联吡啶)钌(II)(Ru(bipy)₃²⁺)在线生成Ru(bipy)₃³⁺。反应物区的最佳顺序、浓度和吸入体积为:50 mM硫酸中15 mM Ce(IV) 41 μL、0.5 mM Ru(bipy)₃²⁺ 30 μL、0.4 M乙酸钠16 μL和I样品15 μL;吸入到保持盘管的流速为60 μL s⁻¹,检测流速为100 μL s⁻¹。对于0.1 - 50 μM的I,将CL强度(瞬态CL信号的峰高)与I浓度相关的校准曲线为曲线(二阶多项式)(r = 0.9997;n = 9),在0.1 - 10 μM的I范围内为直线段(r = 0.9995;n = 5)。检测限(3σ)为0.05 μM I。峰高的重复性(相对标准偏差,n = 10)在2.4%(0.5 μM I)至2.0%(7 μM I)之间。样品通量为180 h⁻¹。该方法用于测定半固体剂型(凝胶和软膏)中1%至5%的I。结果与紫外分光光度法的结果比较良好。