蔬菜中灭蝇胺残留的强阳离子交换固相萃取柱净化-液相色谱分析

建立了简单、快速测定蔬菜中灭蝇胺残留量的方法。蔬菜样品经乙酸胺-乙腈(1∶ 4,体积比)混合溶液提取,强阳离子交换固相萃取(SCX-SPE)柱净化后,采用高效液相色谱仪在波长215 nm处测定,所用色谱柱为Agilent NH2,流动相为乙腈-水溶液(97∶ 3,体积比),以1.0 mL/min的流速等梯度洗脱。结果表明,在浓度为0.02~2 mg/L范围内,线性相关系数为0.999 9。灭蝇 胺的添加浓度在0.05~0.4 mg/kg范围内,平均回收率为83.4%~104%,相对标准偏差为1.7%~8. 4%,均在农药残留测定所允许的范围内。该方法的最低检出限(LOD)为0.02 mg/kg,最低检测浓度(LOQ)为0.05 mg/kg。

Determination of Cyromazine Residue in Vegetables by Strong Cation Exchange-Solid Phase Extraction and High Performance Liquid Chromatography

A simple and rapid method was developed for the residue determination of cyromazine.Cyromazine in vegetable samples was extracted by the mixed solution of ammonium acetate and acetonitrile,followed by cleanup with strong cation exchange-solid phase extraction (SCX-SPE).The elution was determined by HPLC in 215 nm.In the method,cyromazine was analyzed on an Agilent NH2 column,using a mixture of acetonitrile-water(97∶ 3,V/V)as the mobile phase with a flow rate of 1.0 mL/min.The correlation coefficient in the concentration range 0.02~2 mg/L was 0.999 9.The average recoveries of cyromazine in vegetables at 0.05,0.2,0.4 mg/kg fortification level were 83.4%~104%,and the relative standard deviations (RSD) were 1.7%~8.4%.The limit of detection (LOD) of this method is 0.02 mg/kg,and the limit of quantitation (LOQ) reaches 0.05 mg/kg.