1. 福建农林大学生命科学学院
2. 福州大学化学化工学院食品安全分析与检测教育部重点实验室
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孔德贤, 李清禄, 池毓务, 等. 流动注射电化学发光测定动物饲料中6-丙基-2-硫脲嘧啶含量的研究[J]. 分析测试学报, 2013,32(11):1283-1388.
Determination of 6-Propy-2-thiouracile in Animal Feeds by Flow-injection Electrochemiluminescence Method[J]. 2013,32(11):1283-1388.
基于6-丙基-2-硫脲嘧啶(PTU)对三联吡啶钌( Ru(bpy)2+3) 电化学发光(ECL)有强烈的增敏作用,建立了流动注射电化学发光(FI-ECL)检测PTU的新方法。通过考察影响体系电化学发光的因素(如电压信号类型及电位、缓冲溶液pH值、载液流速及Ru(bpy)2+3浓度等),得到FI-ECL测定PTU的最佳条件,并提出了可能的反应机理。研究结果表明,在0.1 mol/L pH 12.0的H3PO4-NaOH缓冲介质中,控制恒电位为+1.50 V,Ru(bpy)2+3浓度为1.0×10-4 mol/L,载液流速为1.5 mL/min,PTU对Ru(bpy)2+3的电化学发光具有最大的增敏作用。在此条件下,测得PTU的线性范围为2.0×10-7~1.0×10-4 mol/L(r2=0.998 6),检出限(S/N=3)为1.3×10-8 mol/L,对7份浓度均为1.0×10-6 mol/L的PTU标准溶液进行测定,所得结果的相对标准偏差为1.2%。该方法简便、快速、灵敏,用于模拟动物饲料中PTU含量的检测,结果满意。
Based on the fact that 6-propy-2-thiouracile(PTU) could strongly enhance the electrochemiluminescence(ECL) of tris(2,2’-bipyridine) ruthenium(Ⅱ)(Ru(bpy)2+3),a new flow injection analysis method with a homemade electrochemiluminescence(FI-ECL) detector was proposed for the first time.The experimental parameters those may influence the ECL intensity of the Ru(bpy)2+3/PTU system(such as voltage signal mode and applied potential,pH of buffer solution,flow rate of the carrier solution,and concentration of Ru(bpy)2+3solution ) were investigated.The optimum conditions for the FI-ECL detection of PTU were obtained and the possible mechanism of the ECL system was suggested.The results showed that in 0.1 mol?L-1 pH 12.0 H3PO4-NaOH buffer solution,when the carrier solution’s flow rate was setted at 1.5 mL?min-1,the strongest ECL intensity enhancement could be realized at potential of +1.50 V in the present of 1.0×10-4 mol/L Ru(bpy)2+3.Under this optimal condition,the linear range of PTU was 2.0×10-7-1.0×10-4 mol/L with a correlation coefficient of 0.998 6 and a detection limit(S/N=3) of 1.3×10-8 mol/L.The relative standard deviation(RSD,n=3) for 1.0×10-6 mol/L PTU standard solution was 1.2%.The method was simple,rapid and sensitive,and was successfully applied in the determination of PTU in spiked animal feeds.
流动注射电化学发光6-丙基-2-硫脲嘧啶三联吡啶钌
flow-injectionelectrochemiluminescence6-propy-2-thiouraciletris(22’-bipyridine) ruthenium(Ⅱ)
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