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建立基于非水胶束电动毛细管色谱在线富集技术测定蔬果中克百威和甲萘威残留的新方法。对影响分离和富集效果的缓冲液参数、分离电压和进样时间进行优化。运行缓冲溶液为含100mmol/L十二烷基硫酸钠、30mmol/L乙酸钠的甲酰胺-乙腈(85:15,V/V)溶液,表观pH值为9.4;分离电压20kV;进样时间150s。在此优化条件下,克百威和甲萘威的富集倍数分别为678和758倍;检出限分别为31μg/L和7.9μg/L;6次重复测定的峰面积相对标准偏差为2.47%、1.76%;平均加标回收率为80.4%～96.2%和92.5%～104.1%。以上结果表明该方法具有良好的灵敏度和重现性,可用于果蔬中该两种农药残留的检测。
A new method for determination of carbofuran and carbaryl residues in fruits and vegetables based on non-aqueous micellar electrokinetic capillary chromatography on-line enrichment was established. Buffer parameters affecting separation and enrichment efficiency, voltage separation, and injection time were optimized. The running buffer solution was a formamide-acetonitrile (85:15, V / V) solution containing 100 mmol / L sodium dodecyl sulfate and 30 mmol / L sodium acetate at an apparent pH of 9.4; separation voltage of 20 kV; injection time 150s. Under these optimal conditions, the enrichment fold of carbofuran and carbaryl were 678 and 758 times, respectively; the detection limits were 31μg / L and 7.9μg / L, respectively. The relative standard deviation (RSD) of peak area of 6 replicates was 2.47 % And 1.76% respectively. The average recoveries were 80.4% ~ 96.2% and 92.5% ~ 104.1%. The above results show that the method has good sensitivity and reproducibility and can be used for the detection of the two pesticide residues in fruits and vegetables.