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High performance liquid chromatography post-column chemiluminescence determination of sulfonamide residues in milk at low concentration levels using bis[4-nitro-2-(3,6,9-trioxadecyloxycarbonyl)phenyl] oxalate as chemiluminescent reagent.
Journal of Chromatography A ( IF 3.8 ) Pub Date : 2005 Nov 18 , DOI: 10.1016/j.chroma.2005.07.123
Jorge J. Soto-Chinchilla , Laura Gámiz-Gracia , Ana M. García-Campaña , Kazuhiro Imai , Luis E. García-Ayuso

The determination of seven sulfonamides by means of HPLC with chemiluminescence detection is proposed for the first time. The analytes are derivatized with fluorescamine, separated and subsequently they participate in the post-column chemiluminescence (CL) peroxyoxalate system using imidazole as a catalyst. Among the different peroxyoxalates tested, bis[4-nitro-2-(3,6,9-trioxadecyloxycarbonyl)phenyl] oxalate provides higher sensitivities and stabilities, avoiding precipitation problems. A rigorous optimization of the significant variables by means of experimental designs has been developed in order to reconcile the chromatographic conditions with the CL reaction. The method provides detection limits in the low microgl(-1) range and has been satisfactorily applied to the analysis of spiked raw milk samples.

中文翻译:

高效液相色谱柱后化学发光法测定草酸双[4-硝基-2-(3,6,9-三氧代癸氧基羰基)苯基]草酸酯为化学发光试剂以低浓度测定牛奶中的磺酰胺残留量。

首次提出了采用化学发光检测方法通过HPLC测定7种磺酰胺类药物的方法。使用荧光胺将分析物衍生化,分离,然后使用咪唑作为催化剂参与柱后化学发光(CL)过氧草酸酯系统。在所测试的不同过氧草酸酯中,双[4-硝基-2-(3,6,9-三氧代十六烷基氧羰基)苯基]草酸酯提供更高的灵敏度和稳定性,避免了沉淀问题。已经开发出通过实验设计对显着变量进行严格优化的方法,以使色谱条件与CL反应协调一致。该方法提供了低microgl(-1)范围内的检测限,并已令人满意地应用于加标原料奶样品的分析。
更新日期:2017-01-31
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