论文部分内容阅读
建立了采用气相色谱-电子捕获检测器(GC-ECD)测定柑桔和土壤中苯丁锡残留量的分析方法。样品经乙腈提取,浓盐酸衍生化,中性氧化铝柱净化。结果表明:在0.5～5.0 mg/kg添加水平范围内,苯丁锡的平均添加回收率为92%～98%,相对标准偏差(RSD)为5.8%～8.7%(n=5)。方法的最小检出量(MDL)为1×10-10g,苯丁锡在桔肉、桔皮、全果和土壤4种基质中的定量限(LOQ)均为0.5 mg/kg。该方法杂质干扰少,准确性及灵敏度满足农药残留检测要求,对检测硬件要求低,适用于柑桔和土壤中苯丁锡残留的分析。消解动态试验结果表明,苯丁锡在柑桔和土壤中的消解半衰期分别为9～14 d和9～11 d,属易降解农药。
An analytical method was established for the determination of benzin-tin residues in citrus and soil by gas chromatography-electron capture detector (GC-ECD). Samples were extracted with acetonitrile, concentrated hydrochloric acid derivatization, neutral alumina column purification. The results showed that the average recoveries of dibenzyl tin were 92% -98% and the relative standard deviations (RSDs) were 5.8% -8.7% (n = 5) within the range of 0.5-5.0 mg / kg. The minimum detection limit (MDL) of the method was 1 × 10-10 g. The limit of quantification (LOQ) of all the four substrates in citrus, orange peel, whole fruit and soils was 0.5 mg / kg. The method has less impurity interference, the accuracy and the sensitivity meet the requirements of pesticide residue detection, the detection hardware has low requirements and is suitable for the analysis of residues of benzidine in citrus and soil. The dynamic test results of digestion showed that the digestion half-lives of butyltin in citrus and soil were 9-14 d and 9-11 d, respectively, which were easily biodegradable pesticides.