首页> 外文期刊>Journal of Chromatographic Science >Determination of Suifamethazine Residue in Chicken Serum and Egg by High-Performance Liquid Chromatography with Chemiluminescence Detection
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Determination of Suifamethazine Residue in Chicken Serum and Egg by High-Performance Liquid Chromatography with Chemiluminescence Detection

机译:高效液相色谱-化学发光法测定鸡肉和鸡蛋中的磺胺二甲嘧啶残留

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摘要

A sensitive method that involves high-performance liquid chromatography with cliemiluminescence detection is developed for the determination of sulfamethazine residue in samples of chicken serum and egg. Sulfamethazine is extracted from the samples and derivatized with fluorescamine. The derivatized samples are eluted by reversed-phase chromatography using a mixture of 10 mM potassium phosphate and 30% acetonitrih- on a Nova-Pak C_(18) column. The post-column reagents in the chemiluminescence systemare 1mM bis[2-(3,6,9-trioxadecanyloxycarbonyl)-4-nitrophenyl] oxalate and 0.3M hydrogen peroxide in aceionilrile. The detection limit in the standard solution is 1 ng/mL, and the calibration curve is linear between 1 and 100 ng/mL. The recoveries of spiked samples (50 ppb) are 95.8 ± 9.7% in chicken serum samples and 84.9 ± 10.7% in egg samples. In actual sample analysis, the lowest detectable concentration of sulfamethazine (0.073 mu g/mL) was found at 48 h in serum and on day 9 (0.017 mu g/g) in egg after oral administration of a dose of 100 mg/kg body weight to hens.
机译:建立了一种灵敏的方法,该方法涉及具有荧光发光检测的高效液相色谱法,用于测定鸡血清和鸡蛋样品中的磺胺二甲基嘧啶残留量。从样品中提取出磺胺二甲嘧啶,并用荧光胺衍生。在Nova-Pak C_(18)色谱柱上,使用10 mM磷酸钾和30%乙腈的混合物,通过反相色谱洗脱衍生化的样品。化学发光系统中的柱后试剂为1mM草酸双[2-(3,6,9-三氧十二烷氧羰基)-4-硝基苯基]草酸酯和0.3M过氧化氢。标准溶液中的检出限为1 ng / mL,校准曲线在1至100 ng / mL之间呈线性关系。加标样品(50 ppb)的回收率在鸡血清样品中为95.8±9.7%,在鸡蛋样品中为84.9±10.7%。在实际样品分析中,口服剂量为100 mg / kg的人体后,血清48小时和鸡蛋第9天的最低检测浓度为磺胺二嗪(0.073μg / mL),0.09μg/ g。母鸡体重。

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