RP-SPE-HPLC分析蔬菜中灭多威、2，4-D和噻嗪酮的残留量

Analysis of Methomyl,2,4-D and Buprofezin in Vegetables by RP-SPE-HPLC

建立了反相固相萃取(RP-SPE)配合高效液相色谱(HPLC)测定蔬菜中灭多威、2,4-D和噻嗪酮3种农药残留量的方法。采用超声波辅助提取样品,提取液经固相萃取柱富集后,在XDB-C18柱上分离,以甲醇:水:磷酸(V:V:V)=70:30:0.1的混合液为流动相.流速为0.8 ml/min,用紫外检测器在波长240 nm下,测定了灭多威、2.4-d和噻嗪酮在芹菜和韭菜中的残留量。以保留时间定性确证,峰面积外标法进行定量。结果表明:3种农药的浓度与其峰面积在30～360μg/L的范围内呈良好的线性关系,检出限为0.003～0.06μg/g,样品的加标平均回收率为96.52%～102.91%,相对标准偏差1.82%～3.58%。此方法简便、快速、灵敏,适用于蔬菜中这3种农药的同时分析。

A reversed phase solid phase extraction equipped with high performance liquid chromatography method for the determination of methomyl, 2,4-D and buprofezin in vegetables had been developed. The samples were extracted by using ultrasound assistant, enriched and cleaned up by ODS - C18 solid phase extraction column. Chromatographic separation was performed on a XDB - C18 column using methanol：water：phosphoric acid （V：V：V）=70：30：0.1 intermixture as flow phage. The results demonstrated that the linear ranges ranged from 30 μg/L to 360 μg/L, with detection limits ranged from 0.0031μg/g to 0.06 μg/g. The average recoveries for all three analytical pesticides ranged from 90.3% to 106% with elative standard deviation from 1.82% to 3.58%. The method was simple, rapid, accurate and suitable for simultaneous determination of these three kinds of pesticides in vegetables.