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.
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.
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DOI：
10.1016/j.chroma.2005.07.123
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发表时间：
2005-11
期刊：
影响因子：
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通讯作者：
J. Soto-Chinchilla;L. Gámiz-Gracia;A. García-Campaña;K. Imai;L. E. García-Ayuso
中科院分区：
文献类型：
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作者：
J. Soto-Chinchilla;L. Gámiz-Gracia;A. García-Campaña;K. Imai;L. E. García-Ayuso
首次提出采用高效液相色谱-化学发光检测法同时测定七种磺胺类药物。分析物与荧光胺衍生化，分离，随后他们参与柱后化学发光（CL）过氧草酸盐体系使用咪唑作为催化剂。在所测试的不同过氧草酸盐中，双[4-硝基-2-（3，6，9-三氧代癸氧基羰基）苯基]草酸盐提供更高的灵敏度和稳定性，避免了沉淀问题。通过实验设计的显着变量的严格优化已经开发，以调和的色谱条件与CL反应。该方法的检测限在低μgl− 1范围内，并已令人满意地应用于加标原料奶样品的分析。
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 μgl−1range and has been satisfactorily applied to the analysis of spiked raw milk samples.