超高效液相色谱法测定啶酰菌胺和咯菌腈在番茄与土壤中的残留

Determination of Boscalid and Fludioxonil in Tomato and Soil by Ultra Performance Liquid Chromatography

应用超高效液相色谱仪建立一种同时检测番茄和土壤中啶酰菌胺和咯菌腈残留的分析方法。样品经乙腈提取,乙二胺-N-丙基硅烷(PSA)吸附净化,以乙腈和水为流动相等度洗脱,采用可变波长紫外检测器检测,外标法定量分析。结果表明,啶酰菌胺和咯菌腈在0.05～1μg/mL范围内呈现良好的线性关系,相关系数R2均为0.999,方法的检出限均为0.01 mg/kg,定量限为0.1 mg/kg;在0.1～1 mg/kg范围内,添加回收率在82.8%～102.8%和86.5%～115.3%之间,相对标准偏差(RSD)在4.1%～8.7%和4.9%～9.1%之间。该方法简单可靠、重现性好,适用于番茄和土壤中啶酰菌胺和咯菌腈的残留检测。

The study aims to establish an analytical method for simultaneous determination the residues of boscalid and fludioxonil in tomato and soil by ultra performance liquid chromatography(UPLC). The tomato and soil samples were extracted with acetonitrile, and cleaned up with PSA, then analyzed by gradient elution using acetonitrile-water as the mobile phase. The residues were determined by wavelength ultraviolet detector and quantified by an external standard method. The residues showed good linear relationship in the range of 0.05–1 μg/mL with correlation coefficient of 0.999, the limit of detection(LOD) and the limit of quantitation(LOQ) were 0.01 mg/kg and 0.1 mg/kg, respectively. And the recoveries for boscalid and fludioxonil in 3 samples at spiked levels of 0.1–1 mg/kg were between 82.8%–102.8% and 86.5%–115.3% with RSD of 4.1%–8.7% and 4.9%–9.1%. This method is simple, reliable with a good reproducibility, which is applicable for analysis of boscalid and fludioxonil residues in tomato and soil.