固相萃取-高效液相色谱法同时检测红小豆中咪唑啉酮类除草剂

Simultaneous Determination of Six Imidazolinone Herbicides Residues in Adzuki Beans by Solid Phase Extraction and High Performance Liquid Chromatography

为建立一种同时测定红小豆中6种咪唑啉酮类除草剂残留的反相高效液相色谱分析方法,将样品粉碎过筛后,用二氯甲烷超声提取,经OASISMCX固相萃取柱净化,采用AgilentTC-C18(250mm×4.6mm,i.d5μm)色谱柱,磷酸水溶液(pH3.5)-乙腈为流动相梯度分离,流速1mL/min,紫外检测波长252nm,以外标法定量。结果表明:咪唑啉酮类除草剂在质量浓度0.01～1.00μg/mL(灭草喹0.004～0.5μg/mL)范围内,标准曲线的线性相关系数范围0.9998～0.9999;方法检出限(LOD)0.0016～0.004mg/kg;红小豆中的平均加标回收率72.2%～98.8%,相对标准偏差(RSD)1.02%～4.86%。该分析方法操作简便,灵敏度高,重现性好,适用于红小豆中咪唑啉酮类农药的多残留检测。

A method for simultaneous determination of six pesticides in Adzuki Bean samples by solid phase extraction （SPE） and high performance liquid chromatographic （HPLC） was developed. The analytical procedure involved ultrasonic extraction with dichloromethane and purification using a OASIS MCX SPE column （3 mL, 60 mg）. The eluate was blown to dryness under a stream of nitrogen and the residue was dissolved in mobile phase, followed by separation and quantitative analysis by using reversed phase HPLC with gradient elution for the base line separation of the 6 pesticides and uhraviolet wave detection. The experimental results showed a good linear relationship between the peak area and the concentration（r=0.9998-0.9999）, and the average recoveries ranged from 72.2% to 98.8% with the relative standard deviation（RSD） range of 1.02% to 4.86%. The results showed that the method was easy to operate, high sensitivity and good repeatability for determining multi residual pesticides in Adzuki Bean sample.