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A novel, simple and robust method for the analysis of sulfonamides in fish farming water samples using column switching liquid chromatography

机译:一种使用柱切换液相色谱法分析鱼类养殖水样中磺胺类药物的新颖,简单,耐用的方法

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摘要

A novel method for the online extraction and preconcentration of four sulfonamides was developed using column switching liquid chromatography. Sulfadiazine, sulfathiazole, sulfamethoxypyridazine and sulfamethoxazole were analysed in water samples and preconcentrated in a C18 guard column. Suitable validation parameters were obtained, such as precision, accuracy and relative recovery, in accordance with the validation guidelines of the Food and Drug Administration. Low limits of detection (0.05-0.09 mu g L-1) and quantification (0.30 mu g L-1, for all of them) were obtained. The quadratic polynomial model was used to adjust the calibration data, and the coefficients of determination were higher than 0.999 for all the analytes. The method was shown to be robust to the assayed parameters according to Youden's test. The proposed method was successfully used to determine sulfonamides in 11 different fish farming water samples, in which sulfadiazine (0.732 mu g L-1), sulfamethoxazole (0.531 mu g L-1), sulfathiazole (0.546-1.856 mu g L-1) and sulfamethoxypyridazine (0.369-1.509 mu g L-1) were found.
机译:利用柱切换液相色谱法开发了一种在线提取和预浓缩四种磺酰胺的新方法。在水样中对磺胺嘧啶,磺胺噻唑,磺胺甲氧基哒嗪和磺胺甲恶唑进行了分析,并在C18保护柱中进行了预浓缩。根据美国食品药品管理局的验证指南,获得了合适的验证参数,例如精度,准确性和相对回收率。获得了低检测限(0.05-0.09μg L-1)和定量分析(全部均为0.30μgL-1)。使用二次多项式模型调整校准数据,所有分析物的测定系数均高于0.999。根据Youden的测试,该方法显示出对测定参数的鲁棒性。该方法成功用于11种鱼类养殖水样中磺胺类的测定,其中磺胺嘧啶(0.732μg L-1),磺胺甲恶唑(0.531μgL-1),磺胺噻唑(0.546-1.856μgL-1)发现了磺胺甲氧哒嗪(0.369-1.509μgL-1)。

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