Dispersive Liquid - Liquid Microextraction for the Determination of Sulfonamide Residues in Egg Samples

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Abstract

A dispersive liquid-liquid microextraction combined with high-performance liquid chromatography-diode array detection was developed for the extraction and determination of 15 sulfonamide residues in the egg matrix. The effects of various parameters such as the type, volume, and composition of extraction solvent for sample treatment procedure, the type and volume of disperser solvent, centrifugation time, salting-out effect and solution pH were studied, and optimum conditions were established. Linearity was found in the range of 5.4 – 1 000 μg kg-1 with regression coefficients ranging from 0.9918 - 0.9987. The limit of detection (LOD) and limit of quantification (LOQ) values of the proposed method were in the range of 4.3 - 8.0 μg kg-1 and 12.9 - 24.0 μg kg-1, respectively. Satisfactory intra-day and inter-day precision results in the range of 6.3 - 17.5% and 4.8 - 16.8%, respectively, were achieved. The accuracy of the method was acceptable with percentage recovery in the range of 73 - 108% and %RSD values in the range of 1.1 - 16.5%. The proposed method was applied in chicken egg samples obtained from supermarkets, and findings confirmed that the method is feasible to be used for extraction and determination sulfonamide residues in egg and related complex biological matrices.
分散液-液微萃取法测定鸡蛋样品中磺胺残留
建立了高效液相色谱-二极管阵列检测相结合的分散液液微萃取方法,用于提取和测定鸡蛋基质中15种磺胺残留。考察了样品处理过程中萃取溶剂的种类、体积和组成、分散溶剂的种类和体积、离心时间、盐析效果和溶液pH等参数的影响,确定了最佳工艺条件。在5.4 ~ 1 000 μ kg-1范围内呈线性关系,回归系数为0.9918 ~ 0.9987。方法的检出限和定量限分别为4.3 ~ 8.0 μ kg-1和12.9 ~ 24.0 μ kg-1。在6.3 ~ 17.5%的日内精度和4.8 ~ 16.8%的日间精度范围内取得了满意的结果。回收率在73 ~ 108%之间,RSD值在1.1 ~ 16.5%之间,准确度可接受。将该方法应用于从超市购买的鸡蛋样品中,结果证实该方法可用于鸡蛋及相关复杂生物基质中磺胺残留的提取和测定。
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