【摘要】 以4种磺胺类药物（Sulfonamides,SAs）,即磺胺脒（Sulfaguanidine,SGD）、磺胺嘧啶（sulfadiazine,SDZ）、磺胺噻唑（sulfathiazole,STZ）和磺胺二甲嘧啶（Sulfamethazine,SMZ）为分析物,基于其在碱性介质中对Ag（Ⅲ）配合物-鲁米诺（Luminol）与Ni（Ⅳ）配合物鲁米诺两化学发光体系发光强度均具有抑制作用的性质,建立了高效液相色谱-化学发光法检测牛奶中4种磺胺类药物的方法。将化学发光体系作为高效液相色谱的新型检测器,并对两种化学发光体系的检测器性能进行了比较。4种磺胺药物经高效液相色谱分离后,分别与Ag（Ⅲ）-Luminol及Ni（Ⅳ）-Luminol化学发光体系作用。色谱条件为:反相C₁₈分离柱（250 mm×4.6 mm,5μm）;0.1%甲酸-甲醇为流动相（V/V）;梯度洗脱;流速1 mL/min。化学发光条件:Ag（Ⅲ）、Ni（Ⅳ）-Luminol两体系中,Ag（Ⅲ）配合物浓度1.4×10^-4mol/L（含0.12 mol/L NaOH）;Ni（Ⅳ）配合物浓度1.5×10^-5mol/L（含0.12 mol/L NaOH）;Luminol浓度均为1.2×10⁷mol/L;试剂流速均为1.0 mL/min。在最佳的分离检测条件下,Ag（Ⅲ）-Luminol体系检测4种磺胺类药物的检出限分别为0.15、0.96、1.10和1.50μg/mL,加标回收率为81.0%¹01.5%;Ni（Ⅳ）-Luminol体系检测SGD、SDZ、STZ 3种磺胺类药物的检出限分别为1.5、17.2和16.8μg/mL,加标回收率为83.9%¹10.8%。相比之下,Ag（Ⅲ）-Luminol体系作为高效液相色谱检测器更佳。应用本方法对牛奶中4种磺胺类药物残留量进行检测,结果令人满意。更多还原

【Abstract】 Sulfonamides（ SAs）,such as sulfaguanidine（ SGD）,sulfadiazine（ SDZ）,sulfathiazole（ STZ）and sulfamethazine（ SMZ）,can drastically inhibit the chemiluminescence（ CL） intensities generated in both Ag（Ⅲ）-Luminol and Ni（Ⅳ）-Luminol systems. Based on these observations,a novel method of high performance liquid chromatography（ HPLC） coupled with CL detection was established. Both the Ag（Ⅲ）-Luminol and Ni（Ⅳ）-Luminol CL systems were employed as detectors,and the performances of the two detecting systems were compared. After separated by HPLC,four SAs reacted with Ag（Ⅲ）-Luminol and Ni（Ⅳ）-Luminol CL system,respectively. Chromatographic conditions were as follows: reversed-phase C₁₈ column（ 250 mm × 4. 6 mm,5 μm）,gradient elution,and 0.1%（ V/V） formic acid-methanol as mobile phase with flow rate of 1 mL/min.CL conditions were as follows: [Ag（Ⅲ）]= 1.4×10^-4mol/L（ in 0.12 mol/L NaOH）; [Ni（Ⅳ）]= 1.5×10^-5mol/L（ in 0.12 mol/L NaOH）; [Luminol]= 1.2 × 10^-7mol/L; and flow rate = 1. 0 mL/min. Under the optimal conditions,the detection limits of Ag（Ⅲ）-Luminol CL system were 0. 15,0. 96,1. 10,1.50 μg/mL for SGD,SDZ,STZ,and SMZ,respectively,and the recovery were 81. 0%-101. 5%. Comparatively,the detection limits of Ni（Ⅳ）-Luminol CL system were 1.5,17.2,16.8 μg/mL for SGD,SDZ and STZ,and the recoveries was 83.9%-110.8%. The result showed that the Ag（Ⅲ）-Luminol CL system had a much better performance. The method was applied to the determination of the residues of the above four SAs in milk with satisfactory results.更多还原