周艳明，忻 雪，胡 睿

(沈阳农业大学分析测试中心，辽宁 沈阳 110161)

气相色谱法测定蔬菜水果中三氯杀螨醇残留量

周艳明，忻 雪，胡 睿

(沈阳农业大学分析测试中心，辽宁 沈阳 110161)

建立测定蔬菜和水果中三氯杀螨醇农药残留的气相色谱方法。选择10种蔬菜、水果样品，经丙酮正己烷混合试剂提取后，过弗罗里固相萃取柱净化、碱解，用带有电子捕获检测器的气相色谱仪测定，外标法定量。通过对该方法的灵敏度、准确度和精密度进行实验，三氯杀螨醇的最低检出限为0.005mg/kg，各水平的添加回收率范围为70.23%～98.10%，变异系数为3.21%～10.12%，所建立的蔬菜、水果中三氯杀螨醇残留量的测定方法满足国家标准对食品中农药残留测定的要求。

气相色谱法；蔬菜；水果；三氯杀螨醇；碱解反应

Abstract ：A method using gas chromatography (GC) was established for the determination of dicofol residue in vegetables and fruits. Samples were extracted with a mixture of acetone and n-hexane. The resulting extract was then cleaned up on a Florisil column and treated with a mixture of absolute ethanol and aqueous potassium hydroxide solution. The n-hexane (upper layer) was harvested and washed with 20 g/L aqueous sodium sulfate solution twice prior to the injection into a GC system equipped with an electron capture detector. The external standard method was adopted for dicofol quantification. The figures of merit of the developed method such as sensitivity, accuracy and precision were evaluated. The limit of detection for dicofol was 0.005 mg/kg. Average recoveries for dicofol in 10 species of real samples separately spiked at 3 levels in 10 replicates each were ranged from 70.23%to 98.10%, with a RSD range between 3.21% and 10.12%. This method may satisfy the requirements of the national standards for pesticide residue determination.

Key words：gas chromatography；fruits and vegetables；dicofol；alkaline hydrolysis

三氯杀螨醇又称开乐散，是一种有机氯杀螨剂。工业品为褐色透明油状液体，微溶于水，能溶于多种有机溶剂。化学性质稳定，在碱性条件下能水解成二氯苯酮和氯仿[1]。该药为神经毒剂，对害螨具有较强的触杀作用，无内吸附性，对成螨、若螨和卵均有效，是我国目前常用的杀螨剂农药，可防治棉花、果树、蔬菜等作物上的螨类[2]。

三氯杀螨醇日容许摄入量为0.025mg/kg，过多的摄入有致畸作用。其分解慢，施药一年后在蔬菜、水果中仍有残留，严重影响蔬菜水果等作物的质量[3-5]。目前我国国家标准中尚无蔬菜水果中三氯杀螨醇残留量的检测方法。本实验拟建立测定蔬菜、水果中三氯杀螨醇残留量的气相色谱方法。……