固相萃取-高效液相法测定蔬菜中6种磺胺类药物

Determination of Six Sulfonamide Residues in Vegetables by Solid Phase Extraction Combined with High Performance Liquid Chromatography

以石墨烯为吸附剂制备固相萃取柱,建立固相萃取-高效液相色谱法检测6种磺胺类药物的方法。采用紫外检测器进行定性和定量分析,检测波长为270nm。对包括吸附剂的种类、洗脱剂的种类和用量、样品溶液的pH值和样品体积等参数进行详细优化。在优化条件下,6种磺胺类药物在0.1～100μg/L范围内与峰面积呈良好的线性关系,相关系数为0.990～0.997。检出限(R_(SN)=3)为6.3～21.1ng/L。方法的精密度为2.12%～4.75%。将该方法用于蔬菜样品分析,回收率为79.3%～104.2%。

A method for determination of six sulfonamide residues in vegetables was developed using solid-phase extraction （SPE） on a column filled with grapheme as an adsorbent combined with HPLC. The qualification and quantification of six sulfonamides were performed using an ultraviolet detector at 270 nm. Experimental parameters such as SPE adsorbent type, eluent type and volume, and sample solution pH and volume were optimized. Under the optimized conditions, six sulfonamides showed good linear relationship between peak area and concentration in the range of 0.1-100 μg/L with correlation coefficients of 0.990-0.997. The limits of detection （LOD） of the developed method were in the range of 6.3-21.1 ng/L （RsN = 3）. The precision （RSD） for replicate determinations varied from 2.12% to 4.75%. The average recovery rates of this method when used to analyze different vegetables were between 79.3% and 104.2%.