杀菌剂苯噻菌胺在马铃薯中的残留检测方法研究

Determination of Benthiavalicarb-isopropyl Residues in Potato by Gas Chromatography

[目的]评价苯噻菌胺在马铃薯中的归趋和安全性,研究和建立了马铃薯中苯噻菌胺残留的气相色谱检测方法。[方法]选用乙腈对马铃薯样品中残留的苯噻菌胺进行振荡提取,再用二氯甲烷进行液-液分配,净化后用带NPD检测器的气相色谱仪对苯噻菌胺进行检测,分析检测所使用的色谱柱型号为DB-17(30 m×0.32 mm,0.25μm)。[结果]结果表明:在0.05~12.50 mg/L质量浓度范围内苯噻菌胺峰面积与浓度呈现出良好的线性关系;在添加质量分数为0.02~2.00 mg/kg时,马铃薯中苯噻菌胺的添加回收率和相对标准偏差分别为80.3%~105.0%和1.3%~4.1%;该方法的最小检出量(LOD)为0.15 ng,苯噻菌胺在马铃薯中的最低检测浓度(LOQ)为0.02 mg/kg。[结论]该方法具有灵敏度、精密度和准确度良好,杂质干扰少等特点,符合农药残留检测分析的基本要求。

[Aims] An analytical method was established for determining benthiavalicarb-isopropyl residues in potato by gas chromatography with nitorgen-phosphus detector （GC-NPD） to evaluate the trend and safety of benzothiamine in potato. [Methods] The benthiavalicarb-isopropyl residue in potatoes was extracted with acetonitrile, and cleaned-up through liquid-liquid partition with dichloromethane. The analysis was performed on DB-17 steel column （30 mx0.32 ram, i.d. 0.25 Ixm）. [Results] The calibration curve ofbenthiavalicarb-isopropyl was in good linearity within the concentration of 0.05-12.50 mg/L. When the spiked level ranged from 0.02 to 2.00 mg/kg, the average spiked recoveries of benthiavalicarb-isopropyl in potato were in the range of 80.3-105.0% with the relative stardand deviation （RSD） of 1.3-4.1%. The limit of detection （LOD） of benthiavalicarb-isopropyl was 0.15 ng, and the limit of quantification（LOQ） of benthiavalicarb-isopropyl in potato samples was 0.02 mg/kg. [Conclusions] The method was proved to meet the basic requirements of pesticide residue analysis on sensitivity, accuracy and precision, and to be suitable for analysis of benthiavalicarb-isopropyl residues in the environmental matrix such as potato and soil.