快速溶剂萃取–高效液相色谱法测定禽蛋中磺胺嘧啶

建立快速溶剂萃取–高效液相色谱法测定禽蛋中磺胺嘧啶残留的方法。用单因素和正交试验对禽蛋中磺胺嘧啶的萃取条件进行优化,确定了最佳萃取条件:以甲醇为萃取剂,在130℃循环萃取4次,冲洗体积分数为80%,萃取时间为25 min。色谱柱为Hypersil ODS2柱(4.6 mm×250 mm,5μm),流动相为甲醇–0.5%冰乙酸(25∶75),流量为1.0 m L/min,检测波长为265 nm。磺胺嘧啶的质量浓度在0.025~0.500 mg/m L范围内与色谱峰面积呈良好的线性关系,相关系数r=0.999 5,检出限为0.5μg/kg。加标回收率在83.0%~88.2%之间,测定结果的相对标准偏差为2.2%(n=9)。方法的精密度、准确度和基质效应均符合禽蛋样品检测要求,可用于禽蛋中磺胺嘧啶含量的测定。

Determination of Sulfadiazine in Eggs by Accelerated Solvent Extraction and High Performance Liquid Chromatography

A extraction and analytical method with accelerated solvent extraction (ASE) and high performance liquid chromatography was developed to determine sulfadiazine in eggs.Single factor and orthogonal experiment were adopted to optimize the extraction conditions.The results showed that the optimum conditions of extraction were as follows:methanol was as extraction solvent,130 ℃ for four times in 25 min and ring volume fraction of 80％.The separation of samples was carried on Hypersil ODS2 column (4.6 mm × 250 mm,5 μm) with mobile phase of methanol-0.5％ acetic acid(25:75)0and detection wavelength of 265 nm.The mass concentration of sulfadiazine was linear with chromatographic peak area in the range of 0.025-0.500 mg/mL with correlation coefficient of 0.999 5.The detection limit was 0.5 μg/kg.The spiked recoveries were in the range of 83.0％-88.2％ with relative standard deviation of 2.2％(n=9).The precision,accuracy,mean recoveries and the matrix effect were satisfied with the requirements of eggs measurement.The method is suitable for the determination of sulfadiazine in eggs.